improved methods for forensic toxicology...
TRANSCRIPT
Improved Methods for
ForensicToxicologyAnalysis
We at Phenomenex understand your needs and have therefore developed products that allow you to get your work done with confidence. Phenomenex SPE, GC/MS, HPLC, and LC/MS products have the phases and formats you need in order to detect drugs of abuse from various matrices. We use the latest technology to ensure our products will give you the highest sensitivity and fastest analysis time every time.
The screening and confirmation for drugs of abuse and their metabolites present many challenges in toxicological analysis. Searching for illegal drugs in complex matrices, such as urine and blood, can prove to be difficult because if present, they may be found at very low concentration levels. Direct analysis of these samples is often hampered by endogenous compounds in the biomatrix. These interferences are often in higher concentrations than that of the target analytes and thus may mask their presence.
Specialized Products for Forensic Toxicology
Table of Contents
Specialized Products for Forensic Toxicology ----pp. 2-6
Sample Preparation/SPE ------------------------------------------ 2-3
GC/MS -------------------------------------------------------------- 4-5
LC/MS ------------------------------------------------------------------6
Applications --------------------------------------- pp. 8-25
PCP ---------------------------------------------------------------------8
Methadone -------------------------------------------------------------9
THC ----------------------------------------------------------------10-11
Cocaine -----------------------------------------------------------12-13
Amphetamines ---------------------------------------------------14-15
Opiates ------------------------------------------------------------16-17
Steroids ------------------------------------------------------------18-19
Benzodiazepines ------------------------------------------------ 20-21
Barbiturates ------------------------------------------------------ 22-23
6-MAM --------------------------------------------------------------- 24
Blood Alcohols ------------------------------------------------------- 25
Ordering Information -----------------------------pp. 28-33
Sample Preparation/SPE Sorbents ------------------------------- 28
GC Columns --------------------------------------------------------- 29
General GC Accessories --------------------------------------- 30-31
HPLC Columns -------------------------------------------------- 32-33
KeyPremier Solutions: Products providing the optimal results for the analysisStandard Solutions: Products for general routine workLow Cost Solutions: Alternative products for labs interested in cost savings
© 2009 Phenomenex, Inc. All rights reserved.
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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Mixed-mode Cation Exchange
Strata® Silica-Based SPE Sorbents
Effective Extraction and High Recovery
Extraction of hydrophobic and basic drugs from •biological matrices such as blood, serum, and urine
Removes anionic and neutral interferences without •seriously affecting the recovery of the basic analyte
Consistent manufacturing for accurate and reproducible results•
Inert material provides clean extracts•
Standing orders available•
Large particle for clog-free, superior flow in absence •of a vacuum
Good for viscous samples such as horse urine and •plasma, or gravity flow applications
High extraction efficiency compared to traditional •mixed-mode sorbents of smaller particle size
Alternative for:
Low Cost Solutions
Strata Screen-C Strata Screen-C GFImproved Gravity Flow
Alternative for:Varian Bond Elut Certify® I, UCT Clean Screen® DAU, JT BAKER Bakerbond Narc™-2, IST ISOLUTE® HCX,Macherey-Nagel Chromabond Drug
Varian Bond Elut Certify® HF, UCT XtrackT® DAU
Contact Phenomenex or your local Phenomenex distributor for Strata Screen-C GF ordering information.
SamPLe PreParaTion/SPe
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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Lot-to-lot reproducibility provides consistent recoveries •from extraction-to-extraction
pH stability from 1-14 for safe and stable basic elution •of many drug compounds
High analyte capacity for loading up to 66 % more in •comparison to silica-based sorbents per gram
Strata™-X Polymer-Based SPE Sorbents
Withstands high organic washes to more completely •remove matrix contaminants
Attain better LODs/LOQs for increased sensitivity, •accuracy, and precision of data
pH limit 1-14 offers more controlled selectivity and •higher recoveries of analytes
Eliminate the need for harsh halogenated solvents •
Large particle size provides excellent flow for viscous •biological fluids such as horse urine and plasma
High recovery of drugs using the same selectivity as •Strata-X-C
Consistent tube-to-tube flow•
Controlled selectivity for target analytes for removal of •contaminants and better elimination of matrix effects
High analyte capacity for loading up to 66 % more in •comparison to silica-based sorbents per gram
Withstands aggressive organic washes ( 57 - 60 % •organic)* without breakthrough of analyte
Reproducible recoveries from extraction-to-extraction •and superior lot-to-lot reproducibility
Large particle size provides excellent flow for viscous •biological fluids such as horse urine and plasma
High recovery of drugs using the same selectivity as •Strata-X
Consistent tube-to-tube flow•
Strata-X is de-condition resistant for higher recovery, precision, & ruggedness
Strata-X-CImproved Gravity FlowStrata-XL-C
Strata-X Reversed Phase
Premier Solutions
Strong Cation Exchange and Reversed Phase
Strata-XL
For Strata-X on-line extraction cartridges, see p. 28.
Improved Gravity Flow
SamPLe PreParaTion/SPe
An alternative for:Waters Oasis® MCX, UCT’s StyreScreen® DBX
An alternative for:Waters Oasis® HLB, Varian NEXUS, FOCUS and PLEXA, UCT’s StyreScreen® DVB, JT Baker H20-pilic DVB, IST ENV+, Macherey-Nagel’s Easy and HR-X
*Please see TN-0017, "Testosterone on Strata-X vs. C18-E"
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GC Column Dimensions for Fast Drug Analysis
Reduce analysis time!
Standard SolutionNEW Zebron™ GC Columns Developed for Forensic Testing
New Optimized Column Dimensions Available in These Popular Phases:Zebron ZB-5MSi - Specially deactivated for analysis of derivatized and un-derivatized drug compounds.
Alternative for: DB-5, HP-5msi, Rtx-5ms, Rtx-5Amine, HP-5ms
ZB-1ms - Good low polarity phase for general drug screening.
Alternative for: DB-1ms, HP-1ms, Rtx-1ms, VF-1ms, MDN-1, Equity-1, AT-1ms
ZB-5ms - Provides improved resolution for aromatic compounds
Alternative for: DB-5ms, DB-5ms EVDX, VF-5ms, CP-Sil 8 CB MS, DB-5.625
ZB-XLB - unique phase that can be used to improve resolution of structurally similar compounds
Alternative for:DB-XLB, Rtx-XLB, MDN-12, VF-Xms
NEWGc/mS
Traditional Dimension Optimized DimensionColumn: Zebron ZB-5MSi
Dimensions: 15 meter x 0.25 mm x 0.25 μmPart No.: 7EG-G018-11Injection: Split 10:1 @ 260 °C, 1 μL
Carrier Gas: Helium @ 1.5 mL/min (constant flow )Oven Program: 150 °C to 320 °C @ 25 °C/min
Detector: MSD @ 320 °CSample: Analytes @ 1.2 ppm BSTFA
1. Carboxy-THC-d32. Carboxy-THC
Column: Zebron ZB-5MSiDimensions: 10 meter x 0.18 mm x 0.18 μm
Part No.: 7CD-G018-08Injection: Split 10:1 @ 280 °C, 1 μL
Carrier Gas: Helium @ 0.7 mL/min (constant flow )Oven Program: 200 °C to 300 °C @ 20 °C/min
Detector: MSD @ 320 °CSample: Analytes @ 1.2 ppm BSTFA
1. Carboxy-THC-d32. Carboxy-THC
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Phenomenex now offers new optimized column dimensions (10 meter x 0.18 mm x 0.18 µm) in our award winning Zebron GC column phases. This special dimension allows for a major improvement in sample throughput, while still providing great peak shapes and resolution. In addition, the extended temperature stability range and the low column bleed levels allow for high temperature removal of matrix contamination and fast elution of target analytes.
Decrease run time by at least 30 %•
Symmetrical peak shapes and great resolution for drugs of abuse•
Better limits of detection (LOD) and quantitation (LOQ)•
30 %Faster
Run Time
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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GC Columns Designed for Drugs of Abuse
Zebron ZB-Drug-1: Faster Results, Better Peak Shape, Great Separation
Premier SolutionNEW Zebron™ ZB-Drug-1 is a Specialized Solution Developed for Forensic Testing
Specially deactivated to improve quantitation for drug compounds•
New 10 meter x 0.18 mm x 0.18 µm dimensions significantly •reduces run time
Temperature Limits (-60 to 320/340 °C)•
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Zebron ZB-Drug-1 is a new mid polarity phase designed to provide fast analysis for compounds in drugs of abuse. The unique stationary phase improves separation of target analytes from common matrix interferences present in biological samples. The special deactivation procedure improves peak shape for acidic and basic drugs, allowing for more accurate quantitation. MS certified bleed levels allow for low level detection.
Gc/mS
Opiates on a ZB-5ms Opiates on a ZB-Drug-1Column: Zebron ZB-5ms
Dimensions: 10 meter x 0.18 mm x 0.18 μmPart No.: 7CD-G018-08-CInjection: Split 10:1 @ 240 °C, 1 μL
Carrier Gas: Helium @ 1.2 mL/min (constant flow )Oven Program: 140 °C to 320 °C @ 20 °C/min for 1 min
Detector: MSD @ 230 °CSample: Analytes @ 10 ppm BSTFA/Pyridine
1. Codeine-d62. Codeine3. Morphine-d34. Morphine
Column: Zebron ZB-Drug-1Dimensions: 10 meter x 0.18 mm x 0.18 μm
Part No.: 7CD-G023-08Injection: Split 10:1 @ 280 °C, 1 μL
Carrier Gas: Helium @ 55 cm/sec (constant flow )Oven Program: 180 °C to 340 °C @ 20 °C/min
Detector: MSD @ 230 °CSample: Analytes @ 10 ppm BSTFA/Pyridine
1. Codeine-d62. Codeine3. Morphine-d34. Morphine
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Unique Selectivity for
Drugs
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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HPLC Columns for LC/MS Analysis
Premier SolutionsPhenomenex HPLC Columns
Achieve high sensitivity, optimal retention, and great separation of basic drugs•
Positively impact laboratory productivity with longer column lifetime•
Extended pH stability 1-12•
Gemini®
Luna®
Synergi
High quality phases good for all types of forensic samples•
Low MS bleed improves sensitivity for LC/MS/MS methods•
Extensive batch traceability and reproducibility data supplied with every column•
Unique phases that provide enhanced selectivity across the polarity scale•
Often resolves compounds that co-elute on traditional column chemistries•
Synergi Hydro-RP (C18 with Polar Endcapping) has maximum hydrophobic •selectivity with added polar retention. Also compatible with 100 % aqueous conditions
MercuryMS™ Ultra-fast, low-cost analysis for high-throughput LC/MS laboratories•
Packed with Luna, Synergi, and Gemini material•
Short 10 and 20 mm cartridge formats use a new proprietary slurry packing process•
Lc/mS
Phenomenex’s LC/MS columns are designed to give high sensitivity, optimal retention, and a full range of selectivities for drugs of abuse. Our columns have low MS bleed, which results in less background noise. This is important when quantitating samples in low concentration.
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Cocaine and Metabolites
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14 Column: Luna 3 µm HILICDimensions: 100 x 2.0 mm
Part No.: 00D-4449-B0 Mobile Phase: A: Acetonitrile/ 100 mM Ammonium
formate, pH 3.2 (50:45:5) B: Acetonitrile/ Water/ 100 mM Ammonium formate pH 3.2 (50:45:5)
Gradient: A/B (100:0) for 1.7 min, to A/B (45:55) in 3.1 min, hold for 1.7 min, then to A/B (100:0) for 6 min
Flow Rate: 0.4 mL/minDetection: Mass Spectrometer (MS)
Sample: 1. Cocaine2. Norcocaine3. Ecgonin Methyl Ester4. Benzoylecgonine5. Ecgonine
™
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
Applications
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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Premier Solution: Strata™-X-CLow Cost Solution: Strata® Screen-CPCP is a weakly basic compound with a pKa of about 8.5, but a relatively high LogP of 5.32. The pKa and high LogP allow it to be effectively retained through hydrophobic and ionic interactions on mixed-mode cation-exchange sorbent such as Screen-C or Strata-X-C. The high hydrophobic retention of PCP can reduce recoveries if strong organic elution is not used.
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiDerivatization of this compound is not necessary as the amine functionality does not display adverse secondary interactions in the GC system. The single peak is easily analyzed with good sensitivity.
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
PCP 200 243 186
PCP - d5 (IS) 205 248
GC/MS Cut off 25 ng/mLDerivatization n/a
Extraction of Phencyclidine from Urine and Analysis by GC/MS
Recovery of PCP by SPE
Phencyclidine on a Zebron™ ZB-5MSi
Phencyclidine on a Zebron™ ZB-Drug-1
Phencyclidine (PCP) induces hallucinogenic and neurotoxic effects. Since a vast majority of the parent drug and its metabolite are excreted in urine, abuse is determined by detecting the parent drug.
SPE Method Sorbent: Strata-X-C, 60 mg/3 mLPart No.: 8B-S029-UBJ
Condition: 2 mL methanol followed by 2 mL water Load: 4 mL (1 mL of analyte and IS spiked human urine acidi-
fied with 2 % H3PO4; diluted with 3 mL 100 mM KH2PO4, pH 6.0) sample
Wash 1: 2 mL 0.1 N HCI Wash 2: 2 mL methanol
Dry: 1 min under 10 in. HgElute: 2 mL 5 % NH4OH/Methanol (2 x 1 mL)
Evaporate: Under nitrogen Reconstitute: 300 µL Ethyl acetate
Column: Zebron ZB-5MSi Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G018-08Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 0.6 mL/min (constant flow) Oven Program: 150 °C to 320 °C @ 20 °C/min
Detection: MSD @ 230 °C Sample: Analytes at 2 ppm in Ethyl acetate
1. Phencyclidine-d5 2. Phencyclidine
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 280 °C, 0.5 µL
Carrier Gas: Helium @ 55 cm/sec (constant flow) Oven Program: 160 °C to 340 °C @ 20 °C/min
Detection: MSD @ 230 °CSample: Analytes at 2 ppm in Ethyl acetate
1. Phencyclidine-d5 2. Phencyclidine
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Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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Methadone
Solutions
SPE
Premier Solution: Strata™-X-C Low Cost Solution: Strata® Screen-CMethadone is a non-polar basic compound that is well retained on cation-exchangers, such as Strata® Screen-C and Strata X-C, or on neutral sorbents such as Strata-X.
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiMethadone can be analyzed by GC/MS, similar to other drugs. Derivatization improves peak shape by decreasing reactivity with system components.
GC/MS Cut off 300 ng/mLDerivatization n/a
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
Methadone-d9 (IS) 78 303
Methadone 72 294 223
SPE MethodSorbent: Strata-X-C, 60 mg/3 mLPart No.: 8B-S029-UBJ
Condition: 2 mL methanol followed by 2 mL water Load: 3 mL urine spiked with analytes and IS (0.5 µg/mL);
dilute 1:1 with 100 mM KH2PO4 (pH 6); acidified with 2 % phosphoric acid
Wash 1: 2 mL 0.1 N HCI Wash 2: 2 mL methanol
Elute: 2 mL 5 % NH4OH/Methanol (2 x 1 mL)Evaporate: Under nitrogen
Reconstitute: 200 µL Ethyl acetate
Extraction of Methadone from Urine and Analysis by GC/MS
Recovery of Methadone by SPE
Methadone on a Zebron™ ZB-Drug-1
Methadone binds with opiate receptors and displays many of the same physiological affects as heroin. However, it is not structurally related to heroin or other opiate compounds. To determine abuse, a separate screening method must be performed.
Methadone on a Zebron™ ZB-5MSi Column: Zebron ZB-5MSi
Dimensions: 10 meter x 0.18 mm x 0.18 µm Part No.: 7CD-G018-08Injection: Split 10:1@ 280 °C, 1 µL
Carrier Gas: Helium @ 0.7 mL/min (constant flow) Oven Program: 200 °C to 300 °C @ 20 °C/min
Detection: MSD @ 320 °C Sample: 24 ppm in Ethyl acetate
1. Methadone-d9 2. Methadone
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 55 cm/sec (constant flow) Oven Program: 200 °C to 300 °C @ 25 °C/min
Detection: MSD @ 230 °C Sample: 24 ppm in Ethyl acetate
1. Methadone-d9 2. Methadone
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OMethadone
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Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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THC
O
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Solutions
SPE
Premier Solution: Strata™-X-CLow Cost Solution: Strata® Screen-A or -CThough THC is best extracted using mixed-mode anion-exchange sorbents, such as Strata Screen-A, for convenience many labs will use a mixed-mode cation-exchange sorbent since they are already using this type of sorbent for the majority of their other methods. THC-COOH and THC are effectively extracted from Strata-X-C and Screen-C through disruption of hydrophobicity and hydrogen bonding mechanisms. Removal of more polar matrix interferences can still be effectively done by washing with an organic solution acidified at or below pH 3.
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiIn many countries, THC is the most commonly screened drug. Due to the high volume of samples, system stability and fast run time are critical. Starting the GC oven at >200 oC did not affect peak shape or quantitation of THC-COOH, but allowed for much faster cycle times significantly improving sample throughput.
LC/MS
Premier Solution: Gemini® C18Acidic compounds, such as THC-COOH are often run under mildly basic conditions in negative ion mode. Gemini allows the user an extended pH range to increase basic conditions much further, and create more favorable mass spec ionization for acids and neutrals in a mixture together. In this application, at pH 10, both the THC neutral parent and the THC-COOH metabolite are successfully de-protonated for optimum MS sensitivity in negative ion mode..
Recovery of THC by SPE
SPE MethodSorbent: Strata Screen-C, 150 mg/3 mLPart No.: 8B-S016-SBJ
Condition: 2 mL methanol followed by 2 mL 50 mM phosphoric acidLoad: Hydrolyzed urine sample
Base hydrolysis: 2 mL urine spiked with analyte and IS, add 300 µL 10 N KOH. Mix, vortex and hydrolyze for 20 min at 60 ºC. Cool and adjust pH to 4-5 (by add-ing 165 µL glacial acetic acid followed by addition of 2 mL 0.1 M sodium acetate (pH 7)/methanol (95:5)
Wash 1: 3 mL 50 mM phosphoric acidWash 2: 3 mL 50 mM phosphoric acid/methanol (80:20, v:v)
Dry: 3 min under vacuum; add 0.5 mL hexane followed by additional drying for 1 min Elute: 2 mL hexane/ethyl acetate (80:20, v:v)
Evaporate: Nitrogen @ 40 ºCReconstitute: Add 25 µL ethyl acetate and 25 µL BSTFA (1 % TMCS). React @ 70 ºC for 20 min.
SPE MethodSorbent: Strata-X-C, 60 mg/3 mLPart No.: 8B-S029-UBJ
Condition: 2 mL methanol followed by 2 mL 0.1 N HClLoad: Hydrolyzed urine sample
Base hydrolysis: 2 mL urine spiked with analyte and IS, add 100 µL 10 N KOH. Mix, vortex and hydrolyze for 20 min at 60 °C. Cool and adjust pH to 3.5-4.0 (by adding 200 µL glacial acetic acid)
Wash 1: 2 mL 0.1 N HClWash 2: 2 mL 0.1 N HCl/acetonitrile (70:30)
Dry: 4 min under vacuum. To further remove water: add 200 µL glacial acetic acid, letting it percolate under gravity for 30-40 sec. Dry sorbent for 1 min under vacuum.
Elute: 2 mL 2 % glacial acetic acid/acetonitrile (2 x 1 mL)Dry: Blow down to dryness under N
2 @ 40 °CReconstitute: Add 30 µL 10 mM imidazole/ethylacetate + 30 µL BSTFA (1 % TMCS). React at
70 °C for 20 min.
Extraction of ∆9–Carboxy-THC from Urine and Analysis by LC/MS or GC/MSTetrahydrocannabinol (THC), the main active chemical in marijuana, is mainly metabolized to 9-carboxy-11-Nor-∆9-carboxy-THC (THC-COOH). This compound is then conjugated with glucuronic acid and excreted in urine.
THC-COOH
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p. 11
Please inquire about other applications.
GC/MS Cut off 15 ng/mLDerivatization BSTFA (with 1 % TMCS)
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
Carboxy-∆9-THC 371 473 474
D3-Carboxy-∆9-THC (IS) 374 476 477
Thc
Carboxy-THC on a Zebron™ ZB-5MSi
THC and Metabolite on Gemini® C18
Carboxy-THC on a Zebron™ ZB-Drug-1
Column: Zebron ZB-5MSi Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G018-08Injection: Split 10:1 @ 280 °C, 1 µL
Carrier Gas: Helium @ 0.7 mL/min (constant flow)Oven Program: 200 °C to 300 °C @ 20 °C/min
Detection: MSD @ 320 °C Sample: Analytes at 1.2 ppm in BSTFA
1. Carboxy-THC-d3 2. Carboxy-THC
Column: Gemini 3 µm C18 Dimensions: 50 x 3.0 mm
Part No.: 00B-4439-Y0 Mobile Phase: A: 10 mM NH
4HCO3 (pH 10) B: Acetonitrile
Gradient: A/B (85:15) to A/B (5:95) in 2.9 min, hold 30 sec, then to A/B (85:15) hold for 30 sec
Flow Rate: 0.8 mL/minDetection: MS @ 450 °C
Sample: 1. 11-nor-9-Carboxy-THC (THC-COOH) 2. ∆-9-tetrahydrocannabinol (THC)-d3 3. ∆-9-tetrahydrocannabinol (THC)
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 280 °C, 0.1 µL
Carrier Gas: Helium @ 55 cm/sec (constant flow) Oven Program: 220 °C to 340 °C @ 20 °C/min
Detection: MSD @ 320 °CSample: Analytes at 1.5 ppm in BSTFA
1. Carboxy-THC-d3 2. Carboxy-THC
Ap
p ID
179
01
Ap
p ID
178
01
Ap
p ID
1779
1
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
aP
PLi
ca
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nS cocaine
N
O
O
O
O
0
10
20
30
40
50
60
70
80
90
100
Strata-X Strata-X-C Strata Screen-C
Ben
zoyl
ecg
oni
ne
Co
caet
hyle
ne
Co
cain
e
Ben
zoyl
ecg
oni
ne
Co
caet
hyle
ne
Co
cain
e
Ben
zoyl
ecg
oni
ne
Co
caet
hyle
ne
Co
cain
e
% R
ecov
ery
82
88 8994
9192
9910197
p. 12
Cocaine
Solutions
SPE
Premier Solution: Strata™-X or Strata-X-CLow Cost Solution: Strata® or Strata Screen-CBenzoylecgonine contains both an amine and carboxylic acid functionality allowing it to be retained through multiple mecha-nisms. Typically, benzoylecgonine is extracted using a mixed-mode cation-exchanger such as Strata Screen-C or Strata X-C. However, the ammonium hydroxide used for elution on cation-exchangers causes hydrolysis of the methyl ester in cocaine and cocaethylene converting them into carboxylic acid containing benzoylecgonine metabolite. Using a neutral sorbent such as Strata-X does not require high pH elution, allowing for independent analysis of all three cocaine compounds.
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiThe single compound of benzoylecgonine eluted in just over 3 minutes by using a fast temperature ramp. To ensure all matrix contamination is removed, a final oven temperature of 320 oC was used. Overall cycle time is kept to a minimum due to the higher starting oven conditions, which reduce the need for GC cool down time.
LC/MSPremier Solution: Luna® HILICUsing a HILIC (Hydrophilic-Interaction-Liquid-Chromatography) LC/MS column, cocaine and its metabolites will elute in less than 7 minutes. Adequate separation is achieved for the key metabolites for further detection by MS.
SPE MethodSorbent: Strata-X, 30 mg/1 mLPart No.: 8B-S100-TAK
Condition: 1 mL methanol / 1 mL waterLoad: 1 mL spiked Porcine plasma acidified with 2 % H
3PO4 (Diluted 1:2 with water)
Wash: 1 mL 20 % methanol in waterDry: 1 min at 10 in. of Hg
Elute: 1 mL methanolEvaporate: Under nitrogen @ 40 oC
Reconstitute: Depends on analysis technique
SPE MethodSorbent: Strata Screen-C, 150 mg/3 mLPart No.: 8B-S016-SBJ
Condition: 2 mL methanol followed by 2 mL waterLoad: 2 mL porcine plasma spiked with analytes
diluted 1:2 with waterWash 1: 2 mL 0.1 N HClWash 2: 2 mL methanol
Dry: 1 min under vacuumElution: 5 % ammonium hydroxide in methanol
Evaporate: Under nitrogen @ 40 ºCReconstitute: Depends on analysis technique
Extraction of Benzoylecgonine from Urine and Analysis by LC or GC/MS
Recovery of Cocaine by SPE
Cocaine is extensively metabolized by the liver, with only 1 % being excreted in the urine unchanged. Abuse is thus detected by monitoring its main metabolite, benzoylecgonine.
1
1
0
17914
2
2
3
3
4
4
5
5
6 7 8 9 10 11 12 min
Cocaine and Metabolites
Ap
p ID
179
14 Column: Luna 3 µm HILICDimensions: 100 x 2.0 mm
Part No.: 00D-4449-B0 Mobile Phase: A: Acetonitrile/ 100 mM Ammonium
formate, pH 3.2 (50:45:5) B: Acetonitrile/ Water/ 100 mM Ammonium formate pH 3.2 (50:45:5)
Gradient: A/B (100:0) for 1.7 min, to A/B (45:55) in 3.1 min, hold for 1.7 min, then to A/B (100:0) for 6 min
Flow Rate: 0.4 mL/minDetection: Mass Spectrometer (MS)
Sample: 1. Cocaine2. Norcocaine3. Ecgonin Methyl Ester4. Benzoylecgonine5. Ecgonine
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aP
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nScocaine
N
O
O
O
O
2.8 3.0 3.2 3.4 3.6
1,2
3.8 4.0 4.2 4.4 4.6 4.8 5.0 5.2 5.4 min
17792
2.5
17805
1,2
2.6 2.7 2.8 2.9 3.0 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 4.0 min
p. 13
Please inquire about other applications.
N
O
OH
O
O
O
NO
O
O
N
O
O
O
O
GC/MS Cut off 150 ng/mLDerivatization BSTFA (with 1 % TMCS)
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
D3-Benzoylecgonine (IS) 243 259 364
Benzoylecgonine 240 256 361
Benzoylecgonine on a Zebron™ ZB-5MSi
Benzoylecgonine on a Zebron™ ZB-Drug-1
Column: Zebron ZB-5MSi Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G018-08Injection: Split 10:1 @ 250 °C, 1 µL
Carrier Gas: Helium @ 0.7 mL/min (constant flow)Oven Program: 160 °C to 320 °C @ 20 °C/min
Detection: MSD @ 320 °C Sample: Analytes at 24 ppm in BSTFA
1. Benzoylecgonine-d3 2. Benzoylecgonine
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 55 cm/sec (constant flow)Oven Program: 235 °C to 320 °C @ 25 °C/min
Detection: MSD @ 230 °C Sample: Analytes at 24 ppm in BSTFA
1. Benzoylecgonine-d3 2. Benzoylecgonine
Ap
p ID
178
05
Ap
p ID
1779
2
Benzoylecgonine
Cocaethylene
Cocaine
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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0
10
20
30
40
50
60
70
80
90
100
Strata-X-C
HM
MA
MD
A
MD
MA
MD
MA
-DS
Am
ph
eta
min
es
MD
A-D
S
Me
tha
mp
he
tam
ine
s
% R
ecov
ery 65
83
70
86
76
6668
p. 14
Amphetamines
Solutions
SPE
Premier Solution: Strata™-X-CLow Cost Solution: Strata® Screen-CAmphetamines are polar aromatic compounds that are basic in nature. This polarity makes them difficult to retain through hydrophobic interactions, but they are well-suited for cation-exchange sorbents such as Strata Screen-C or Strata-X-C. High organic washes remove a majority of hydrophobic matrix interferences that can build up on the GC columns.
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiWhen compared to other drug classes, these compounds are more volatile and require a lower starting oven condition to achieve proper peak shape. However, by ramping quickly up to 320 oC matrix interferences can still be efficiently removed preventing system stability problems. It is also worth noting that separation is achieved between the analyte and its deuterated analog. This separation does not affect quantitation in any way.
LC/MSPremier Solution: Gemini® C18At high pH, basic compounds, such as amphetamines and methamphetamines, are neutralized. Gemini is pH stable from 1-12, providing longer column lifetime when running at high pH.
Absolute Recovery of Amphetamines by SPE
Before Blowing down samples, Be sure to make them into the salt
form By acidifying your solution.failure to do so can result in
sample loss due to evaporation and resulting proBlems with
sample detection.
Extraction of Amphetamine from Urine and Analysis by LC/MS or GC/MS
NH2
NH
Amphetamines are very addictive stimulant drugs that affect the central nervous system. Methamphetamines are metabolized to amphetamines so abuse is typically detected by monitoring both compounds initially by immunoassay. A positive result is then confirmed by LC/MS or GC/MS.
SPE MethodSorbent: Strata-X-C, 30 mg/1 mLPart No.: 8B-S029-TAK
Condition: 1 mL methanol followed by 1 mL waterLoad: 2 mL porcine plasma spiked with analytes diluted
1:2 with waterWash 1: 1 mL waterWash 2: 1 mL 0.1 M acetic acid Wash 3: 1 mL methanolElution: 1 mL 2 % of ammonium hydroxide (28-30 %)* in
methanol (2 x 500 µL)Evaporate: To dryness under gentle nitrogen flow
Reconstitute: Add 200 µL mobile phaseNote: To prevent the loss of amphetamine and
methamphetamine during solvent evaporation, add two drops of concencentrated HCl before the evaporation step
sample preparation
tip
amPheTamineS
Amphetamine Methamphetamine
*Most commercially available NH4OH is 28-30 % stock concentration
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
aP
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NH
2
2.6
17807
1 2
3
4
2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6 min
3
1
2
3
4
5
6
7
8
9
10
4 5 6 min
17809
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 min0.0
17900
1
2
3
6
7
5
4
p. 15
Please inquire about other applications.
GC/MS Cut off 500 ng/mLDerivatization HFBA
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
D11-Amphetamine (IS) 244 128
Amphetamine 240 118 117
D14-Methamphetamine (IS) 261 213
Methamphetamine 254 210 118
D5-MDA (IS) 167 380 244
MDA 162 375 240
D5-MDMA (IS) 258 213 164
MDMA 254 210 389
D5-MDEA (IS) 273 241 408
MDEA 268 240 403
Amphetamines in Urine on a Gemini® C18Column: Gemini 5 µm C18
Dimensions: 150 x 3.0 mm Part No.: 00F-4435-Y0
Mobile Phase: 10 mM Ammonium Formate, 0.1 % formic acid / Acetonitrile (90:10)Flow Rate: 0.6 mL/min Detection: MS @ 450 °C Sample:
1. 4-Hydroxy-3-methoxymethamphetmine (HMMA) 2. Amphetamine (AMPH) 3. Methamphetamine (M-AMPH) 4. 3,4-Methylenedioxy-amphetamine (MDA)-d55. 3,4-Methylenedioxy-amphetamine (MDA)6. 3,4-Methylendiox-methamphetamine (MDMA)-d57. 3,4-Methylendiox-methamphetamine (MDMA) Amphetamines on a Zebron™ ZB-Drug-1
Expanded Amphetamines on a Zebron™ ZB-Drug-1
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 55 cm/sec (constant flow)Oven Program: 110 °C to 320 °C @ 25 °C/min
Detection: MSD @ 320 °C Sample: Analytes are 10 ppm derivatized with HFBA
1. Amphetamine-d11 2. Amphetamine 3. Methamphetamine-d144. Methamphetamine
Ap
p ID
179
00
Ap
p ID
178
09
Ap
p ID
178
07
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 280 °C, 0.1 µL
Carrier Gas: Helium @ 55 cm/sec (constant flow)Oven Program: 70 °C to 130 °C @ 20 °C/min to 270 ºC @ 30 ºC
Detection: MSD @ 230 °C Sample: Analytes are 40 ppm derivatized with HFBA
1. Amphetamine-d11 2. Amphetamine 3. Methamphetamine-d14 4. Methamphetamine 5. MDA-d5 6. MDA 7. MDMA-d5 8. MDMA 9. MDEA-d510. MDEA
amPheTamineS
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aP
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H
N
O
O
OH 1
1
0 2
2
3
3
4 5 6 7 8 9 min
16445
4.0
17806
3,4
1
2
4.1 4.2 4.3 4.4 4.5 4.6 4.7 4.8 min
p. 16
Opiates
Solutions
SPE
Premier Solution: Strata™-X-CLow Cost Solution: Strata® or Strata Screen-CThe nitrogen containing ring system give opiates their basic property and allows them to be extracted using mixed-mode cation exchange sorbents. The ion-exchange retention mechanism allows for much more aggressive wash conditions (up to 100 % organic) for more effective removal of other co-extracted urine components.
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiIf the patient has been using other opiate related compounds such as heroin or norcodeine, these compounds will also be co-extracted and can interfere with the analysis. In such cases, alternative GC/MS conditions should be developed to allow for accurate quantitation of these compounds.
LC/MS
Premier Solution: Luna® HILICA typical SPE method elutes opiates in a high concentration of organic solvent. This concentration is stronger than what is typically used to begin a reversed phase LC method, thus requiring an additional dry-down step followed by reconstitution in the proper mobile phase concentrations before injection. Employing HILIC (Hydrophilic-Interaction-Liquid-Chromatography) is an excellent complement to this extraction process, since this technique uses a starting mobile phase which employs a high concentration of organic solvent. Luna HILIC columns are ideally suited for the direct injection of eluted samples following SPE.Standard Solution: Synergi Hydro-RPSynergi Hyrdro-RP (C18) has an enhanced hydrophobic selectivity that provides extra retention for polar drugs. This results in baseline separation for all opiates. The column is also compatible with 100 % aqueous conditions.
Recovery of Opiates by SPE GC/MS Cut off 300 ng/mLDerivatization BSTFA (with 1 % TMCS)
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
D6 Codeine (IS) 377 349
Codeine 371 343 234
D3 Morphine (IS) 432 417
Morphine 429 414 401
SPE MethodSorbent: Strata-X-C, 30 mg/1mLPart No.: 8B-S029-TAK
Condition: 1 mL methanol followed by 1 mL water Load: 1 mL urine spiked with analytes and IS (0.8 µg/mL) Dilute
1:1 with phosphate buffer solution (pH 7) Acidified with 2 % phosphoric acid
Wash 1: 1 mL 0.1 N HCI Wash 2: 1 mL methanol
Elute: 1 mL 5 % NH4OH/Methanol (2 x 500 µL)
Evaporate: Dry down under nitrogen Reconstitute: Add 200 µL water
Extraction of Opiates from Biological Matrices with High Recovery and Analysis by LC/MS or GC/MS
Strata-X-C0
10
20
30
40
50
60
70
80
90
100
% R
ecov
ery
101
There are a number of opiate related compounds known to have addictive properties. The standard structure contains five ring systems and is substituted at various positions with hydroxyls, ketones, or other groups that contribute to both its pain reducing and its addictive properties.
Morphine and Metabolites on a Luna HILIC
Opiates on a Zebron™ ZB-Drug-1
Column: Luna 3 µm HILIC Dimensions: 100 x 2.0 mm
Part No.: 00D-4449-B0 Mobile Phase: A: Acetonitrile / 100 mM Ammonium
formate, pH 3.2 (90:10) B: Acetonitrile / 100 mM Ammonium formate, pH 3.2 (50:50)
Gradient: A/B (100:0) for 1 min to A/B (0:100) in 2 min, hold for 1.5 min
Flow Rate: 0.4 mL/minDetection: MS
Note: Direct injection following Acetonitrile/ Water (5:1) protein precipitation (PPT)
Sample:1. Morphine 2. Normorphine 3. Morphine-3-ß-glucuronide
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 280 °C, 1 µL
Carrier Gas: Helium @ 55 cm/sec (constant flow)Oven Program: 180 °C to 340 °C @ 20 °C/min
Detection: MSD @ 230 °C Sample: Analytes are 24 ppm derivatized
with BSTFA1. Codeine-d6 2. Codeine 3. Morphine-d3 4. Morphine
looking to run opiates on a standard C18 Column? please inquire with your loCal phenomenex representative.
Ap
p ID
178
06
Ap
p ID
16
44
5
™
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
aP
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nSheaLThcare oPiaTeS
H
N
O
O
OH
H
N
O
O
OH 3.9 4.0 4.1 4.2 4.3 4.4 4.5 4.6 4.7 4.8 4.9 5.0 5.1 5.2 5.3 5.4 min
1,2
3
4
5
6
7
8
9
10
17899
p. 17
Please inquire about other applications.
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 0.7 mL/min (constant flow)Oven Program: 180 °C to 340 °C @ 20 °C/min
Detection: MSD @ 320 °C Sample: Analytes are 24 ppm derivatized with
1. Hydroxylamine 2. BSTFA 1. Morphine-d3 2. Morphine 3. Codeine-d6 4. Codeine 5. Oxymorphone 6. Hydromorphone-d6 7. Hydromorphone 8. Oxycodone-d6 9. Oxycodone10. Hydrocodone
Healthcare Opiates
Solutions
SPEPremier Solution: Strata™-X-CWLow Cost Solution: Strata® Screen-C
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiTo improve peak shape, opiates are often derivatized using BSTFA with 1 % TMCS. When analyzing one or two opiates, this approach works well. However, some opiate structures form multiple products when single step derivatization is done. To ensure a single reaction product for hydromorphone or oxycodone, an oxime derivative is formed prior to reaction with BSTFA. The oxime reaction eliminates the multiple points of interaction resulting in a single derivative product. Once derivatization has been completed, GC/MS analysis can be performed. Separation of all closely related isomers can be somewhat challenging, requiring special attention to those compounds that share the same mass ions such as Norcodeine and Morphine.
7.0 7.2 7.4 7.6 7.8 8.0 min
16555
1
2
3
4
5
6
7
GC/MS Cut off 300 ng/mLDerivatization BSTFA (with 1 % TMCS)
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
D3-Morphine (IS) 432 417
Morphine 429 414 401
D6-Codeine (IS) 377 349
Codeine 371 343 234
Oxymorphone 532 517 287
D6-Hydromorphone (IS) 361 450
Hydromorphone 355 444 429
D6-Oxycodone (IS) 480 465
Oxycodone 474 459 460
Hydrocodone 386 297 371
H
N
O
O
OH
Extraction of Various Prescribed Opiates from Urine and Analysis by GC/MSEven though opiate related compounds pose the risk of addiction, their therapeutic benefit is important for pain management. Opiates such as hydrocodone (Vicodin), oxycodone (OxyContin), and meperidine (Demerol) are routinely prescribed for pain control, but due to their addictive qualities, they often become the subject of abuse.
Column: Zebron ZB-5MSi Dimensions: 30 meter x 0.25 mm x 0.25 µm
Part No.: 7HG-G018-11 Injection: Splitless 20:1 @ 250 °C, 1 µL
Carrier Gas: Helium @ 1.5 mL/min (constant flow)Oven Program: 170 °C for 0.5 min to 360 °C @ 18 °C/min
Detection: MSD @ 180 °C Sample: Analytes at 1 ppm in Methanol
1. Codeine 2. Norcodeine 3. Morphine 4. Hydrocodone 5. Hydromorphone6. Oxycodone7. Oxymorphone
Healthcare Opiates on a Zebron™ ZB-5MSi
Expanded Opiates on a Zebron™ ZB-Drug-1
Ap
p ID
16
55
5
Ap
p ID
178
99
Codeine
Underivatized
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O
O
OH
HO
H
H H
STeroidS
p. 18
Steroids
Solutions
SPE
Premier Solution: Strata™-XWhile standards can be directly analyzed on HPLC without any difficulty, interferences due to proteins, lipids, and salts require cleanup by SPE prior to injection for plasma and urine samples. SPE using Strata-X removes most matrix contaminants from the sample that would interfere with UV and MS detection, as well as allows for concentration of dilute samples. When compared to the commonly used neutral phase SPE sorbents, such as C18, Strata-X retention allows for stronger organic washes for more optimal cleanliness and longer column lifetime.
LC/MS
Premier Solution: Gemini® C18Most steroids are very similar in structure, as well as in molecular weight. Therefore, the need for an HPLC column that can achieve baseline resolution of steroids is critical for accurate quantitation by HPLC-UV. Gemini C18 columns can provide the hydrophobic selectivity needed for most major corticosteroids down to levels around 50 ng/mL with good linearity (r2 > 0.995) and accuracy (98 % - 105 %). While UV detection may be sensitive enough to detect current steroid usage and monitor steroid levels for therapeutic treatments, detection of past steroid usage may require the more sensitive detection offered by a tandem mass spectrometry. The sensitivity of using MS/MS detection allows quantification of background endogenous steroids (cortisone and hydrocortisone) found in blank urine. With MS detection, such low level endogenous amounts must be taken into account with any testing method for illicit steroid use. Linear quantification data using MS detection with Gemini columns deliver excellent linearity and reproducibility for such methods, and are powerful tools for quantitation of steroid levels in plasma and urine. Gemini C18 columns excel in volatile MS-friendly buffers making them the ideal choice for these methods.
SPE MethodSorbent: Strata-X, 30 mg/1 mLPart No.: 8B-S100-TAK
Condition: 1 mL methanol followed by 1 mL waterLoad: 1 mL spiked human serum or urine (diluted 1:1 with water)
Wash: 1 mL water followed by 1 mL 40 % methanol in water (up to 50-60 %)*
Elute: 1 mL methanol (2 x 500 µL)Evaporate: Under nitrogen stream (ambient)
Reconstitute: Add 100 μL acetonitrile/water 40:60
Extraction Steroids from Urine and/or Plasma and Analysis by LC, LC/MS or GC/MS
O
O
OH
OHHOH
H H
O
O
O
OH
HO
H
H H
Corticosteroids are an important class of compounds that have uses as therapeutic agents as well as some illicit uses. However, testing for them has become more challenging due to the use of drug-masking agents by athletes in an attempt to cover their steroid use. Such interferences make chemical and ELISA-based tests sometimes impractical for
accurate detection. The combination of mass spectroscopy, improved chromatography separations and efficient sample preparation by SPE allows for a specific, sensitive and accurate method for detection of steroid usage.
Prednisolone Cortisone
*Please see TN-0017, "Testosterone on Strata-X vs. Strata-X C18-E"
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O
O
O
OH
HO
H
H H
STeroidS
0
1
2
3
4
5
6
7
8
9
0 50 100 150 200 250 300 350 400 450
Steroids in Urine - Standard Calibration Curves LC\MS\MS (1)
Conc.(ng/mL)
Inte
nsity
11α-Hydroxyprogesterone R2 = 0.9999 Deoxycorticosterone R2 = 1.000011-Ketoprogesterone R2 = 0.9999Corticosterone R2 = 0.9999 Hydrocortisone R2 = 0.9999Prednisone R2 = 0.9993
0
2
4
6
8
10
12
14
16
0 50 100 150 200 250 300 350 400 450
Steroids in Urine - Standard Calibration Curves LC\MS\MS
Conc.(ng/mL)
Inte
nsity
Prednisolone R2 = 0.9998 Cortisone R2 = 0.9999 Cortisone acetate R2 = 0.9999 Triamcinolone acetate R2 = 0.9993 Betamethasone-17-valerate R2 = 0.9997 Triamcinolone R2 = 0.9997
2.9e4
2.0e4
0.0
5 10 15 min
Inte
nsity
. cp
s
20.0
2000.0
4000.0
6000.0
8000.0
1.0e4
1.2e4
1.4e4
1.6e4
1.8e4
4 6 108 12 14 16 18 min
Inte
nsity
. cp
s
Extracted ion chromatogram of different MS/MS steroids from urine blank
Cortisone (endogenous)
Hydrocortisone
0
100
200
300
400
500
600
700
800
900
1000
0 200 400 600 800 1000 1200
Steroids in Plasma - LC-UV
Conc.(ng/mL)
Inte
nsity
11α-Hydroxyprogesterone R2 = 0.9991
Prednisolone R2 = 0.9988
Corticosterone R2 = 0.9992
Triamcinolone R2 = 0.9994
Triamcinolone acetonide R2 = 0.9991
p. 19
Please inquire about other applications.
Conditions for All LC Steroid Methods:Column: Gemini® 5 µm C18
Dimensions: 150 x 3.0 mm Part No.: 00F-4435-Y0
Mobile Phase: A: 0.1 % Formic Acid in waterB: 0.1 % Formic Acid in 95 % Acetonitrile / water
Gradient: A/B (60:40) for 4 min to A/B (25:75) in 11 minFlow Rate: 0.6 mL/minDetection: LC-UV @ 254 nm or MS/MS
Temperature: Ambient
LC/MS/MS Chromatogram of Steroid Standard in Urine
LC/MS/MS Chromatogram of a Blank Urine Sample
Steroids in Urine - Standard Calibration Curves LC\MS\MS
Steroids in Plasma-LC-UV
Steroids in Urine - Standard Calibration CurvesLC\MS\MS
Ap
p ID
179
71
Ap
p ID
179
72
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
aP
PLi
ca
Tio
nS
N
N
CI
O
N
N
CI
O
1 20 min0.00
1.00e5
2.00e5
3.00e5
4.00e5
5.00e5
6.00e5
7.00e5
8.00e5
9.00e5
1.00e6
12
3
6
2
16042
0.5 1.0 1.5 2.0 min0.00
1.00e5
2.00e5
3.00e5
4.00e5
5.00e5
6.00e5
7.00e5
8.00e5
9.00e5
1.00e6
1.10e6
1
2 3
6
7
16040
p. 20
benzodiazePineS
Benzodiazepines
Solutions
SPE
Premier Solution: Strata™-X and Strata™-X-CWLow Cost Solution: Strata® Screen-CThere are a number of benzodiazepine related compounds and extraction efficiency depends on the set of compounds being analyzed. General methods can rely primarily on hydrophobic interactions using polymeric sorbents such as Strata-X. This sorbent is suitable for several different classes of compounds with recoveries between 70-130 %. Mixed-mode weak ion-exchangers such as Strata-X-CW can also be used to achieve high recoveries for certain benzo’s with high pKa values.
LC/MS
Improved Solution: Luna® C8(2) and Synergi Fusion-RPBenzo’s are well-suited to analysis by reversed phase HPLC analysis without derivatization. Eliminating this time consuming step can significantly improve sample throughput. High speed LC/MS analysis can be done using the Luna C8(2) or Synergi Fusion car-tridges. These 2.5 µm materials provide high column efficiency allowing for complete analysis of eight benzo’s in under 2 minutes.
GC/MSPremier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSi
Extraction of Benzodiazepines from Urine or Plasma and Analysis by LC/MS or GC/MS
Recovery of Benzodiazepines by SPE
0
3040
50
1020
607080
90100
110
Nor
daz
epam
Dia
zep
am
Oxa
zep
am
Lora
zep
am
Tem
azep
am
Bro
maz
epam
Flur
azep
am
Dia
zap
am
Flun
itraz
epam
Strata-X-CW Strata-X-C
% R
ecov
ery
102 105
93 96
94
98100969794
SPE Method:Sorbent: Strata-X-CW, 30 mg/1 mLPart No.: 8B-S035-TAK
Condition: 1 mL methanol followed by 1 mL D.I. waterLoad: 1 mL analyte spiked human urine (dilute 500 µL urine with 25 mM
sodium acetate, pH 4.5 (1:1)Wash 1: 1 mL 25 mM sodium acetate, pH 4.5Wash 2: 1 mL methanol/acetonitrile/ 2 % acetic acid (1:1:8)
Dry: 2 min at 10 inches of HgElute: 1 mL Ethylacetate. Add 50 µL of Flurazepam (20.0 μg/mL) (2 x 500 µL)
Evaporate: Under slow stream of nitrogen to dryness (no heat) Reconstitute: Add 100 µL 15 % acetonitrile in water
SPE Method:Sorbent: Strata-X-C, 60 mg/3 mLPart No.: 8B-S029-UBJ
Condition: 2 mL methanol followed by 2 mL waterLoad: 2 mL spiked with analytes and IS (0.8 µg/mL); dilute 1:1 with 100 mM
KH2PO4 (pH 6); sample acidified with 2 % H3PO4
Wash 1: 2 mL 0.1 N HClWash 2: 2 mL methanol
Dry: 10 min under vacuumElute: 2 mL 5 % NH4OH/methanol (2 x 1 mL)
Evaporate: Dry down under slow stream of nitrogenReconstitute: Add 200 µL mobile phase
Benzodiazepines on a Synergi Fusion-RP Column: Synergi 2.5 µm Fusion-RP MercuryMS™ Cartridge
Dimensions: 10 x 2.0 mm Part No.: 00N-4423-B0-CE
Mobile Phase: A: 0.1 % Formic Acid in Water B: 0.1 % Formic Acid in Acetonitrile
Gradient: 85:15 (A/B) to 5:95 in 1 min, re-equilibrate to 85:15 in 1 min
Flow Rate: 0.6 mL/min Detection: MS Injection: 10 µL of 100 ng/mL Benzodiazepines in urine
after SPE cleanupSample: 1. 7-Aminoflunitrazepam
2. Chlordiazepoxide 3. Oxazepam4. Nordazepam5. Clonazepam (IS)6. Temazepam7. Flunitrazepam8. Diazepam
Benzodiazepines on a Luna® C8(2)
Column: Luna 3 µm C8(2) MercuryMS™ CartridgeDimensions: 20 x 2.0 mm
Part No.: 00M-4248-B0-CE Mobile Phase: A: 0.1 % Formic Acid in Water
B: 0.1 % Formic Acid in Acetonitrile Gradient: A/B (85:15) to A/B (5:95) in 1 min to (85:15)
hold for 1 minFlow Rate: 0.6 mL/minDetection: MS
Sample: 1. 7-Aminoflunitrazepam 2. Chlordiazepoxide 3. Oxazepam 4. Nordazepam5. Clonazepam (IS)6. Temazepam7. Flunitrazepam8. Diazepam
Benzodiazepines (benzo’s) are psychoactive drugs that are prescribed for anti-anxiety. Due to their addictive nature, benzo’s are highly regulated in most countries. Their possession can be a criminal offense if proper prescriptive information is not demonstrated.
Note: Holder required. See page 32 for ordering information.
Note: Holder required. See page 32 for ordering information.
Ap
p ID
16
042
Ap
p ID
16
04
0
™
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
aP
PLi
ca
Tio
nS
N
N
CI
O
N
N
CI
O
2.2 2.4 2.6 2.8 3 3.2 3.4 3.6 3.8 4 4.2 4.4 4.6 4.8 5 min
17808
2,3 4,51
9
6,7
8
11,12
10
min2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4 4.6
1
3
10
4, 56, 7
11 122
8
9
17894
p. 21
Please inquire about other applications.
GC/MS Cut off 100 ng/mLDerivatization MTBSTFA* (with 1 % MTBDMCS)
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
D5-Nordiazepam-TBDMS (IS) 332 334
Nordiazepam-TBDMS 327 328 383
D5-Oxazepam-TBDMS (IS) 462 519
Oxazepam-TBDMS Serax® 457 513 459
D5-Temazepam-TBDMS (IS) 362 288 390
Temazepam-TBDMS Restoril® 357 359 385
Lorazepam-TBDMS Ativan® 491 513 493
Clonazepam Clonopin® 372 374 326
Diazepam Valium® 256 283 221
Alprazolam Xanax® 279 308 204
D5-α-Hydroxyalprazolam-TBDMS (IS) 386 388
α-Hydroxyalprazolam-TBDMS 381 383 384
benzodiazePineS
N
N
NH
Br
O
N
N
CI
O
N
N
CI
O
F
N
N
N
N+F
O
O
O-
Benzodiazepines on a Zebron™ ZB-Drug-1
Benzodiazepines on a Zebron™ ZB-5MSi Sample:Analytes are 24 ppm derivatized with MBSTFA 1. Diazepam 7. Temazepam2. Nordiazepam-d5 8. Clonazepam3. Nordiazepam 9. Lorazepam4. Oxazepam-d5 10. Alprazolam5. Oxazepam 11. α-Hydroxyalprazolam-d56. Temazepam-d5 12. α-Hydroxyalprazolam
Sample:Analytes are 24 ppm derivatized with MTBSTFA 1. Diazepam 2. Nordiazepam-d5 3. Nordiazepam 4. Oxazepam-d5 5. Oxazepam 6. Temazepam-d5 7. Temazepam 8. Clonazepam 9. Lorazepam10. Alprazolam11. α-Hydroxyalprazolam-d512. α-Hydroxyalprazolam
Ap
p ID
178
08
Ap
p ID
178
94
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 20:1 @ 280 °C, 0.1 µL
Carrier Gas: Helium @ 55 cm/sec (constant flow)Oven Program: 200 °C to 210 °C @ 20 °C/min to 320 ºC
@ 30 ºC for 1 min Detection: MSD @ 320 °C
Column: Zebron ZB-5MSi Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G018-08 Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 1 mL/min (constant flow)
Oven Program: 200 °C to 340 °C @ 25 °C/min for 1 min
Detection: MSD @ 320 °C
Diazepam
Flunitrazepam
Bromazepam
Flurazepam
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
aP
PLi
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Tio
nS
0
20
10
40
30
60
50
80
70
100
90
120
110
Phe
noba
rbita
l
But
albi
tal
Am
obar
bita
l
Phe
noba
rbita
l
But
albi
tal
Am
obar
bita
l
Strata Screen-C Strata-X-C
% R
ecov
ery
100103101102107100
p. 22
SPE Method:Sorbent: Strata-X-C, 60 mg/1 mLPart No.: 8B-S029-UBJ
Condition: 2 mL methanol followed by 2 mL waterLoad: 2 mL analyte and IS spiked human urine (dilute 1:1 with water)
Wash 1: 2 mL 5 % methanol in waterWash 2: 2 mL 10 % methanol / 2 % acetic acid
Dry: 1 min @ 10 in. of HgElute: 2 mL 35 % methanol / 2 % ammonium hydroxide
Evaporate: At 40 ºC under slow stream of N2
Reconstitute: Add 300 µL mobile phase
SPE MethodSorbent: Strata Screen-C, 150 mg/6 mLPart No.: 8B-S016-SCH
Condition: 2 mL methanol followed by 2 mL waterLoad: 2 mL human urine spiked with analytes and IS (0.5 µg/mL); dilute 1:1 with water
Wash 1: 2 mL 5 % methanol in waterWash 2: 2 mL 10 % methanol / 2 % acetic acid, Dry 1 min under vacuum
Elute: 2 mL methanolEvaporate: Dry down @ 40 ºC under slow stream of nitrogen
Reconstitute: Add 300 µL mobile phase buffer
Barbiturates
Solutions
SPEPremier Solution: Strata™-X-CLow Cost Solution: Strata® Screen-CBarbiturates are weakly acidic in nature but can be retained through hydrophobic and hydrogen bonding interactions in SPE. Washing with acidified organic allows for removal of matrix contamination.
HPLC/MS
Premier Solution: Synergi Max-RPBarbiturates can be analyzed by HPLC without derivatization using reversed phase LC, such as with the Synergi Max-RP C12 col-umn. The Synergi Max-RP C12 column is also available in the 2.5 μm HST (High Speed Technology) format. These highly efficient columns allow for rapid LC/MS analysis.
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiAnalysis by GC/MS requires derivatization to improve quantitation. Derivatization with trimethylanilinium hydroxide (TMPAH) allowed five controlled barbiturates to be separated in less than 5 minutes.
Recovery of Barbiturates by SPE
barbiTuraTeS
Extraction of Barbiturates from Urine or Plasma and Analysis by LC, LC/MS or GC/MS
NH
O
NHO O
NHO
NH
O
O
NHO
NH
O
O
Barbiturates are depressants that are typically classified into ultrashort-, short-, intermediate-, and long-acting varieties. When abused, they cause feelings similar to intoxication and induce a “mellow” or relaxed state.
Butalbital
Amobarbital
Phenobarbital
™
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aP
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NHO
NH
O
O
14 min
14622
102 864
5
432
1
12
17810
min1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2
1, 2
3
5
4
6
7
3.2
1
2
3
4
5
6
7
3.0 3.6 3.8 4.0 4.2 4.4 4.6 4.8 5.0 min
17738
p. 23
Please inquire about other applications.
GC/MS Cut off 200 ng/mLDerivatization TMPAH (optional)
Mass Ion(s) Quant Ion Secondary Ion Tertiary Ion
D5-Butalbital (IS) 201 184 214
Butalbital 196 181 138
Amobarbital 169 184 225
Pentobarbital 169 184 225
Secobarbital 196 181 138
D5-Phenobarbital (IS) 122 151 233
Phenobarbital 232 146 117
barbiTuraTeS
Barbiturates on a Zebron™ ZB-Drug-1 Barbiturates on a Zebron™ ZB-5MSi
Barbiturates on a Synergi Max-RP
Column: Zebron ZB-5MSi Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G018-08 Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 0.6 mL/min (constant flow) Oven Program: 100 °C to 320 °C @ 20 °C/min for 5 min
Detection: MSD @ 230 °CSample: Analytes are 12 ppm derivatized with TMPAH
1. Butalbital-d5 2. Butalbital 3. Amobarbital 4. Pentobarbital 5. Secobarbital 6. Phenobarbital-d5 7. Phenobarbital
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 0.7 mL/min (constant flow)Oven Program: 145 °C to 300 °C @ 25 °C/min
Detection: MSD @ 230 °CSample: Analytes are 12 ppm derivatized with TMPAH
1. Butalbital-d5 2. Butalbital 3. Amobarbital 4. Pentobarbital 5. Secobarbital 6. Phenobarbital-d5 7. Phenobarbital
Ap
p ID
1773
8A
pp
ID
14
62
2
Ap
p ID
178
10
Column: Synergi 4 µm Max-RPDimensions: 150 x 4.6 mm
Part No.: 00F-4337-E0 Mobile Phase: A: 20 mM KH2PO4, pH 7.0
B: Acetonitrile Gradient: A/B (80:20) hold 3 min to A/B
(50:50) in 12 min to A/B (80:20) in 1 min
Flow Rate: 1 mL/minDetection: UV @ 210 nm
Sample: 1. Phenobarbital 2. Butabarbital 3. Butalbital 4. Amobarbital 5. Secobarbital
™
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aP
PLi
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Tio
nS
2.0
17802
1,2
2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 min
3.6 3.8 4.0 4.2 4.4
1,2
4.6 4.8 5.0 5.2 5.4 min
17789
p. 24
6-MAM
Solutions
SPE
Premier Solution: Strata™ -X or X-CWLow Cost Solution: Strata® Screen-CExtraction of 6-MAM is similar to other opiate related species. A mixed-mode cation-exchange sorbent such as Screen-C or Strata-X-C ionically retains 6-MAM, and wash solutions with up to 100 % methanol are used to remove weakly bound matrix interferences. However, the use of ammonium hydroxide for elution can make the acetate group in 6-MAM unstable, converting it into morphine. To avoid any potential problems, use a weak cation exchanger such as Strata-X-CW or a neutral sorbent such as Strata-X. Strata-X-CW sorbent can be neutralized by eluting with 2 % formic acid in methanol or any other oganic solvent.
GC/MS
Premier Solution: Zebron™ ZB-Drug-1Standard Solution: Zebron™ ZB-5MSiHeroin can be metabolized into 6-Monoacetylmorphine (6-MAM) and 3-Monoacetylmorphine. 6-MAM can be further metabolized into morphine, so is often found in samples as well. By scanning simply for the 6-MAM ions, high sensitivity confirmation of heroin abuse can be determined. If you wish to detect other opiates as well, simply adjust the SIM ion program to include ions for those analytes. Analysis of all three analytes is possible using the same GC/MS column.
GC/MS Cut off 10 ng/mLDerivatization BSTFA (with 1 % TMCS)
Mass Ion(s) Quant Ion Secondary IonTertiary
Ion
6-Monoacetylmorphine (6-MAM) 399 400 340
D5-6-Monoacetylmorphine (6-MAM d5) (IS) 402 403
6-mam
Extraction of 6-Monoacetylmorphine (6-MAM) from Urine and Analysis by GC/MS
Recovery of 6-MAM by SPE
0
20
40
60
80
100
120
Strata-X-CW Strata-X
% R
eco
very
10299
N O
O
OH
OHO
HO
HO
N
6-Monoacetylmorphine is a unique metabolite of heroin and can be used to differentiate between users of heroin and other legal and illegal opiate drugs.
SPE Method:Sorbent: Strata-X, 60 mg/ 3 mLPart No.: 8B-S100-UBJ
Condition: 2 mL methanol followed by 2 mL waterLoad: 2 mL spiked human urine (diluted 1:2 with water)
Wash: 2 mL water followed by 2 mL 10 % methanol/waterElute: 2 mL methanol
Dry: 2 min at 10 in. HgEvaporate: Blow down to dryness under nitrogen at 40 °C
Reconstitute: Add 0.50 µL ethylacetate and 50 µL BSTFA (1 % TMCS). React at 70 °C for 20 min.
Column: Zebron ZB-5MSi Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G018-08 Injection: Split 10:1 @ 280 °C, 1 µL
Carrier Gas: Helium @ 0.7 mL/min (constant flow) Oven Program: 170 °C to 300 °C @ 20 °C/min
Detection: MSD @ 320 °CSample: Analytes are 1 ppm derivatized with
BSTFA1. 6-MAM-d3 2. 6-MAM
Column: Zebron ZB-Drug-1 Dimensions: 10 meter x 0.18 mm x 0.18 µm
Part No.: 7CD-G023-08 Injection: Split 10:1 @ 260 °C, 1 µL
Carrier Gas: Helium @ 0.7 mL/min (constant flow)Oven Program: 245 °C to 300 °C @ 25 °C/min
Detection: MSD @ 300 °CSample: Analytes are 1 ppm derivatized with
BSTFA1. 6-MAM-d3 2. 6-MAM
6-MAM on Zebron™ ZB-Drug-1
6-MAM on a Zebron™ ZB-5MSi
Ap
p ID
1778
9A
pp
ID
178
02
6-MAM
Morphine
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aP
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Tio
nS
1
1
0
17898
2
2
3
3
4
5
6
7
min1
1
17897
0 2
2
3
3
4
5
6
7
min
p. 25
Please inquire about other applications
Solutions
GC/MS
Premier Solution: Zebron™ ZB-BAC1 and 2The new Zebron ZB-BAC1 and 2 column pair is optimized for fast ethanol separation. These columns resolve both t-Butanol and n-Propanol from other volatile solvents, enabling the use of either compound as the internal standard. This is advantageous because n-Propanol, which may be present in blood samples as a result of bacterial growth, is not a reliable standard in some cases. Zebron ZB-BAC1 and 2 are ideal for law enforcement applications where breathalyzer tests are not feasible as well as with post mortem samples.
bLood aLcohoLS
Blood AlcoholsBlood alcohol analysis is typically used by law enforcement to determine if a driver was unlawfully operating a vehicle. The results will be used in a court of law, therefore it is important to minimize systematic and operator errors.
Confirmation of Blood Alcohols on a Zebron™ ZB-BAC2Blood Alcohols on a Zebron™ ZB-BAC1
Column: Zebron ZB-BAC1 Dimensions: 30 meter x 0.32 mm x 1.80 µm
Part No.: 7HM-G021-31 Injection: Split 5:1 @ 140 °C, 0.5 mL
Carrier Gas: Helium @ 80 cm/sec (constant flow)Oven Program: 40 °C (Isothermal)
Detection: FID @ 220 °CSample: 1. Methanol
2. Acetaldehyde 3. Ethanol4. Isopropanol5. Acetone6. t-Butanol (IS)7. 2-Butanol (IS)
Column: Zebron ZB-BAC2 Dimensions: 30 meter x 0.32 mm x 1.20 µm
Part No.: 7HM-G022-25 Injection: Split 5:1 @ 140 °C, 0.5 mL
Carrier Gas: Helium @ 80 cm/sec (constant flow)Oven Program: 40 °C (Isothermal)
Detection: FID @ 220 °CSample: 1. Methanol
2. Acetaldehyde 3. Ethanol4. Isopropanol5. Acetone6. t-Butanol (IS)7. 2-Butanol (IS)
Ap
p ID
178
97
Ap
p ID
178
98
Fast and Accurate Blood Alcohol Analysis by GC/FID
when working with post mortem samples, it is often safer to
use t-Butanol as your internal standard. n-propanol, a
common internal standard, might Be present as a result of Bacterial growth and can give
you misleading results. since the ZeBron ZB-Bac1 and 2
gc columns completely resolve t-Butanol, you can use it as an
internal standard and attain more accurate results.
gc tip
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Complete SupportTechnical specialists available to help with your troubleshooting •and method optimization
Full range of method development guides and reference tools•
Complete technical solutions for sample preparation and •HPLC/GC analysis
Comprehensive guides and technical notes are available to meet all your SPE, GC or LC needs.
FREE application and troubleshoot-ing services are available to help you create optimized SPE methods for your analysis.
Phenomenex technical specialists are available to provide technical and product support worldwide.
gloBal assistance
method development reference tools
Please ask your Phenomenex technical consultant for complimentary methods on
Extraction of Amphetamines from Urine using Strata• ® Screen-C (ER-0001)
Simplified Method Development for the Extraction of Acidic, •Basic, and Neutral Drugs with a Single SPE Sorbent Strata™-X (TN-0004)
Sample Preparation of Tricyclic Antidepressants for Drug •Screens: The Advantages of Strata-X over Mixed-Mode Sorbents (TN-0006)
LC/MS/MS Analysis of Basic Drugs with Positive Ion •Electrospray in High pH Mobile Phase (TN-1031)
Please inquire about other applications from our Application and Technote Library.
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Ordering Information
or
de
rin
G in
Fo
rm
aT
ion
If Strata SPE products do not perform as well or better than your current SPE product of similar phase, mass and size, send in your comparative data within 45 days and keep the Strata SPE product for FREE!
p. 28
SamPLe PreP./SPe
Strata® and Strata™-X SPE Sorbents
Strata™-XFormat
Sorbent Mass Part. No. Unit Price
Tube30 mg 8B-S100-TAK 1 mL (100/box)* $ 17530 mg 8B-S100-TBJ 3 mL (50/box) 100
60 mg 8B-S100-UBJ 3 mL (50/box)** 135200 mg 8B-S100-FBJ 3 mL (50/box) 155100 mg 8B-S100-ECH 6 mL (30/box) 125200 mg 8B-S100-FCH 6 mL (30/box) 135500 mg 8B-S100-HCH 6 mL (30/box) 160
96-Well Plate 10 mg 8E-S100-AGB 2 Plates/Box 540
30 mg 8E-S100-TGB 2 Plates/Box 54060 mg 8E-S100-UGB 2 Plates/Box 540
*ASPEC capped tubes available in 500/bag (8B-S100-TAM-A)**Tab-less tubes available (8L-S100-UBJ)
Strata™-X-CFormat
Sorbent Mass Part. No. Unit Price
Tube 30 mg 8B-S029-TAK 1 mL (100/box) $ 225
30 mg 8B-S029-TBJ 3 mL (50/box) 12060 mg 8B-S029-UBJ 3 mL (50/box) 135200 mg 8B-S029-FBJ 3 mL (50/box) 185100 mg 8B-S029-ECH 6 mL (30/box) 155200 mg 8B-S029-FCH 6 mL (30/box) 170500 mg 8B-S029-HCH 6 mL (30/box) 230
96-Well Plate 10 mg 8E-S029-AGB 2 Plates/Box 580
30 mg 8E-S029-TGB 2 Plates/Box 58060 mg 8E-S029-UGB 2 Plates/Box 580
Strata® Screen-CFormat
Sorbent Mass Part. No. Unit Price
Tube100 mg 8B-S016-EAK 1 mL (100/box) $ 165100 mg 8B-S016-EBJ 3 mL (50/box) 105150 mg 8B-S016-SBJ 3 mL (50/box) 105200 mg 8B-S016-FBJ 3 mL (50/box) 105300 mg 8B-S016-RBJ 3 mL (50/box) 110150 mg 8B-S016-SCH 6 mL (30/box) 85
*200/box available (8B-S016-5BL)
Strata™-XL-CFormat
Sorbent Mass Part. No. Unit Price
Tube30 mg 8B-S044-TAK 1 mL (100/box) $ 22560 mg 8B-S044-UBJ 3 mL (50/box) 135
200 mg 8B-S044-FBJ 3 mL (50/box) 175100 mg 8B-S044-ECH 6 mL (30/box) 175200 mg 8B-S044-FCH 6 mL (30/box) 205500 mg 8B-S044-HCH 6 mL (30/box) 225
96-Well Plate30 mg 8E-S044-TGB 2 Plates/Box 550
Strata™-XLFormat
Sorbent Mass Part. No. Unit Price
Tube60 mg 8B-S043-UBJ 3 mL (50/box) $ 135
200 mg 8B-S043-FBJ 3 mL (50/box) 150100 mg 8B-S043-EBJ 3 mL (50/box) 140200 mg 8B-S043-FCH 6 mL (30/box) 155500 mg 8B-S043-HCH 6 mL (30/box) 135
96-Well Plate30 mg 8E-S043-TGB 2 Plates/Box 550
Strata® Screen-C GFFormat Sorbent Mass Part. No. Unit PriceTube
200 mg 8B-S026-FBJ 3 mL (50/box) $ 110200 mg 8B-S026-FCH 6 mL (30/box) 90500 mg 8B-S026-HBJ 3 mL (50/box) 125500 mg 8B-S026-HCH 6 mL (30/box) 951000 mg 8B-S026-JCH 6 mL (30/box) 115
SPE Vacuum ManifoldsPart No. Description Unit Price24 – Position Vacuum ManifoldAH0-6024 SPE 24-Position Vacuum Manifold Set, complete
assemblyea $ 840
24 – Position Vacuum Manifold Replacement PartsAH0-6026 SPE Glass Chamber ea 190AH0-6028 SPE Cover, Gasket and 24 Stopcocks ea 360AH0-6030 SPE Gaskets 2/pk 35AH0-6038 SPE Collection Rack, including shelves, legs,
clips and postsea 160
AH0-6049 SPE Luer Stopcocks 24/pk 8512 – Position Vacuum Manifold AH0-6023 SPE 12-Position Vacuum Manifold Set, complete
assemblyea 605
12 – Position Vacuum Manifold Replacement Parts AH0-6025 SPE 12-Position Glass Chamber ea 145AH0-6027 SPE Cover, Gasket and 12 Stopcocks ea 215AH0-6029 SPE Gaskets 2/pk 30AH0-6037 SPE Collection Rack, including shelves, legs,
clips and postsea 140
AH0-6052 SPE 12-Position Vacuum Waste Container, polypropylene
10/pk 95
AH0-6049 SPE Luer Stopcocks 24/pk 85
Strata On-Line Extraction CartridgesPart No. Description Unit/Box Price00M-S033-B0-CB Strata-X on-line extraction cartridge,
20 x 2.0 mmea $ 320
00M-S036-B0-CB Strata-X-CW on-line extraction cartridge, 20 x 2.0 mm
ea 320
00M-S039-B0-CB Strata C18 on-line extraction cartridge, 20 x 2.0 mm
ea 340
00M-S101-B0-CB Strata C8 on-line extraction cartridge, 20 x 2.0 mm
ea 340
CH0-5845 Cartridge holder, 20 mm ea 109
Strata™-X-CWFormat Sorbent Mass Part Number Unit PriceTube 30 mg 8B-S035-TAK 1 mL (100/box) $ 225
60 mg 8B-S035-UBJ 3 mL (50/box) 135200 mg 8B-S035-FBJ 3 mL (50/box) 185200 mg 8B-S035-FCH 6 mL (30/box) 170
Strata® Screen-AFormat Sorbent Mass Part. No. Unit PriceTube
200 mg 8B-S019-FBJ 3 mL (50/box) $ 105500 mg 8B-S019-HCH 6 mL (30/box) 90
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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If Zebron columns do not provide you with equivalent separations as compared to any other GC column of the same phase, and comparable dimensions, send in your comparative data within 45 days and keep the Zebron column for FREE.
p. 29
Gc coLumnS
Zebron™-High Performance GC Columns
ZB-1msID(mm) df(µm) Temp. Limits °C Part No. Price10-Meter0.10 0.10 -60 to 360/370 7CB-G011-02 $ 3850.18 0.18 -60 to 360/370 7CD-G011-08 22512-Meter0.20 0.33 -60 to 360/370 7DE-G011-14 28515-Meter0.25 0.25 -60 to 360/370 7EG-G011-11 3250.32 0.25 -60 to 360/370 7EM-G011-11 35020-Meter0.18 0.18 -60 to 360/370 7FD-G011-08 46025-Meter0.20 0.33 -60 to 360/370 7GE-G011-14 45030-Meter0.25 0.10 -60 to 360/370 7HG-G011-02 5350.25 0.25 -60 to 360/370 7HG-G011-11 5350.25 0.50 -60 to 360/370 7HG-G011-17 5350.25 1.00 -60 to 360/370 7HG-G011-22 5350.32 0.25 -60 to 360/370 7HM-G011-11 5750.32 1.00 -60 to 360/370 7HM-G011-22 57560-Meter0.25 0.25 -60 to 360/370 7KG-G011-11 9000.25 1.00 -60 to 360/370 7KG-G011-22 9000.32 1.00 -60 to 360/370 7KM-G011-22 980
ZB-5MSiID(mm) df(µm) Temp. Limits °C Part No. Price10-Meter0.18 0.18 -60 to 360/370 7CD-G018-08 $ 22515-Meter0.25 0.25 -60 to 360/370 7EG-G018-11 32530-Meter0.25 0.25 -60 to 360/370 7HG-G018-11 5300.25 0.50 -60 to 360/370 7HG-G018-17 5900.32 0.25 -60 to 360/370 7HM-G018-11 5700.32 0.50 -60 to 360/370 7HM-G018-17 57060-Meter0.25 0.25 -60 to 360/370 7KG-G018-11 895
ZB-5msID(mm) df(µm) Temp. Limits °C Part No. Price10-Meter0.10 0.10 -60 to 325/350 7CB-G010-02 $ 3850.18 0.18 -60 to 325/350 7CD-G010-08 22915-Meter0.25 0.25 -60 to 325/350 7EG-G010-11 32520-Meter0.18 0.18 -60 to 325/350 7FD-G010-08 4600.18 0.32 -60 to 325/350 7FD-G010-51 4600.18 0.36 -60 to 325/350 7FD-G010-53 46030-Meter0.25 0.25 -60 to 325/350 7HG-G010-11 5350.25 0.50 -60 to 325/350 7HG-G010-17 5350.25 1.00 -60 to 325/350 7HG-G010-22 5350.32 0.25 -60 to 325/350 7HM-G010-11 5750.32 0.50 -60 to 325/350 7HM-G010-17 5750.32 1.00 -60 to 325/350 7HM-G010-22 57560-Meter0.25 0.25 -60 to 325/350 7KG-G010-11 9000.32 0.25 -60 to 325/350 7KM-G010-11 980
ZB-XLBID(mm) df(µm) Temp. Limits °C Part No. Price10-Meter0.18 0.18 30 to 340/360 7CD-G019-08 $ 22515-Meter0.25 0.25 30 to 340/360 7EG-G019-11 32520-Meter0.18 0.18 30 to 340/360 7FD-G019-08 45530-Meter0.25 0.25 30 to 340/360 7HG-G019-11 5300.25 0.50 30 to 340/360 7HG-G019-17 5300.32 0.25 30 to 340/360 7HM-G019-11 5700.32 0.50 30 to 340/360 7HM-G019-17 5700.53 1.50 30 to 320/340 7HK-G019-28 62060-Meter0.25 0.25 30 to 340/360 7KG-G019-11 895
ZB-Drug-1ID(mm) df(µm) Temp. Limits °C Part No. Price10-Meter0.18 0.18 -60 to 320/340 °C 7CD-G023-08 $ 22515-Meter0.25 0.25 -60 to 320/340 °C 7EG-G023-11 32530-Meter0.25 0.25 -60 to 320/340 °C 7HG-G023-11 535
ZB-BAC1ID(mm) df(µm) Temp. Limits °C Part No. Price30-Meter0.32 1.80 -20 to 260/280 °C 7HM-G021-31 $ 4950.53 3.00 -20 to 260/280 °C 7HK-G021-36 520
ZB-BAC2ID(mm) df(µm) Temp. Limits °C Part No. Price30-Meter0.32 1.20 -20 to 260/280 °C 7HM-G022-25 $ 4950.53 2.00 -20 to 260/280 °C 7HK-G022-32 520
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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p. 30
GeneraL Gc acceSSorieS
SeptaSilicone Rubber Inlet Septa
Advanced silicone formulations reduce coring •and increase septum lifetimeEnhanced durability and re-sealing capabilities•
PhenoGrey™-250This general purpose silicone rubber septum is designed for use up to 250 °C for extended periods of time. With a durometer reading of 40-45, septum puncture is easy (fewer bent needles) for up to 100 injections.
PhenoBlue™-300This low-bleed septum is designed from a recent technology advance in the silicone field. The high durometer rating of 50-60 guarantees over 100 injections at 300 °C, but is actually heat-stable to 350 °C to give you even greater confidence when the oven heats up!
PhenoRed™-400Temperature-rated to 400 °C, even continuous injection port temperatures of 350 °C rarely change this septum's physical properties. Typical injection life is 150 punctures. Available with or without needle GuideRight™ Hole.
PhenoGreen™-400Long life, high-temperature green septum, rated to 400 °C. GuideRight™ through-hole to guide the needle during injection.
General GC Accessories
Septa Sizes by GC InstrumentManufacturer Instrument Model Septa DiameterAgilent (HP) 5850, 5880, 5890, 6850, 6890 7/16 in. (11 mm)
5700 series, 5880A 3/8 in. (9.5 mm)
FerrulesGraphite Ferrules
High-purity graphite significantly reduces ferrule bleed•Special construction minimizes "flaking"•
*Similar to but not always an exact equivalent to the original manufacturer's product.
All Vespel containing ferrules should be pre-shrunk in an oven at 250 ˚C for at least 4 hours prior to use.
Silicone Rubber SeptaPart No. Description Unit Price PhenoGrey 3/8 in. (9.5 mm) Diameter AG0-4686 PhenoGrey-250 Injector Septa 50/pk $ 43AG0-4687 PhenoGrey-250 Injector Septa 100/pk 70PhenoBlueAG0-4688 PhenoBlue-300 Injector Septa 50/pk 70AG0-4689 PhenoBlue-300 Injector Septa 100/pk 115PhenoRedAG0-4690 PhenoRed-400 Injector Septa 50/pk 70AG0-4691 PhenoRed-400 Injector Septa 100/pk 130PhenoGrey 7/16 in. (11 mm) DiameterAG0-4692 PhenoGrey-250 Injector Septa 50/pk 49AG0-4693 PhenoGrey-250 Injector Septa 100/pk 70PhenoBlueAG0-4694 PhenoBlue-300 Injector Septa 50/pk 70AG0-4695 PhenoBlue-300 Injector Septa 100/pk 115PhenoRedAG0-4696 PhenoRed-400 Injector Septa 50/pk 70AG0-4697 PhenoRed-400 Injector Septa 100/pk 130
Graphite Ferrules, Rated to 450 °CPart No. Description Unit Price0.4 mm Ferrule IDAG0-4698 Graphite Ferrule 1/16 in. to 0.4 mm 10/pk $ 39AG0-4699 Graphite Ferrule 1/16 in. to 0.4 mm 50/pk 1350.5 mm Ferrule IDAG0-4701 Graphite Ferrule 1/16 in. to 0.5 mm 10/pk 39AG0-4702 Graphite Ferrule 1/16 in. to 0.5 mm 50/pk 1350.8 mm Ferrule IDAG0-4704 Graphite Ferrule 1/16 in. to 0.8 mm 10/pk 39AG0-4705 Graphite Ferrule 1/16 in. to 0.8 mm 50/pk 135
Short FerrulesVespel/Graphite (85/15 %) Short Ferrules (not for GC/MS), Rated to 350 °CPart No. Description Similar to Mfr. No.* Unit PriceAG0-7318 Vespel/Graphite (85/15 %)
Short Ferrules, 1/16 in. to 0.4 mm (for 0.10 to 0.25 mm ID columns)
5181-3323 10/pk $ 60
AG0-7319 Vespel/Graphite (85/15 %)Short Ferrules, 1/16 in. to 0.5 mm (for 0.32 ID columns)
5062-3514 10/pk 60
AG0-7320 Vespel/Graphite (85/15 %) Short Ferrules, 1/16 in. to 0.8 mm (for 0.45 to 0.53 mm ID columns)
5062-3512 10/pk 60
Graphite (100 %) Short Ferrules (not for GC/MS), Rated to 450 °C
Part No. Description Similar to Mfr. No.* Unit PriceAG0-7513 Graphite (100 %)
Short Ferrules, 1/16 in. to 0.5 mm072635 10/pk 36
Vespel/Graphite (85/15 %) Short Ferrules GC/MS Compatible, Rated to 350 °CPart No. Description Similar to Mfr. No.* Unit PriceAG0-7321 Vespel/Graphite (85/15 %) GC/MS
Short Ferrules, 1/16 in. to 0.4 mm (for 0.10 to 0.25 mm ID columns)
5181-3322 10/pk 60
AG0-7322 Vespel/Graphite (85/15 %) GC/MSShort Ferrules, 1/16 in. to 0.5 mm (for 0.32 ID columns)
5062-3513 10/pk 60
AG0-7323 Vespel/Graphite (85/15 %) GC/MSShort Ferrules, 1/16 in. to 0.8 mm (for 0.45 to 0.53 mm ID columns)
5062-3511 10/pk 60
Vespel / Graphite FerrulesVespel/Graphite Ferrules (60/40 %), Rated to 400 °CPart No. Description Unit Price0.4 mm Ferrule ID AG0-4707 Vespel/Graphite Ferrule 1/16 in. to 0.4 mm 10/pk $ 42AG0-4708 Vespel/Graphite Ferrule 1/16 in. to 0.4 mm 50/pk 1550.5 mm Ferrule ID AG0-4710 Vespel/Graphite Ferrule 1/16 in. to 0.5 mm 10/pk 42AG0-4711 Vespel/Graphite Ferrule 1/16 in. to 0.5 mm 50/pk 1550.8 mm Ferrule ID AG0-4713 Vespel/Graphite Ferrule 1/16 in. to 0.8 mm 10/pk 42AG0-4714 Vespel/Graphite Ferrule 1/16 in. to 0.8 mm 50/pk 155
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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GeneraL Gc acceSSorieSCo
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General GC Accessories
Contact Phenomenex or your local Phenomenex distributor for additional GC accessories. Other manufacturer GC accessories are available.
Injection Port Inlet LinersLiners Agilent Technologies (HP)
Description GC Model No.
DimensionsID x L x OD
(mm)Material*
(deactivated)
Quartz Wool
(Y / N)
Notes
Similar to Mfr. No.**
Part No.
Unit PriceSplitless Straight Liner 5880/5890/6890 4 x 78.5 x
6.45B (n) N ea
5/pk25/pk
210-3003 210-3003-5
–2077320774
–AG0-4651AG0-4652
5/pk25/pk
$ 80309
Split / Splitless with Single Taper 5880/5890/6890 4 x 78.5 x 6.45
B (y) N ea5/pk25/pk
5181-33165183-46955183-4696
–2079920800
–AG0-7516AG0-7640
5/pk25/pk
105370
Splitless, Double Taper/Gooseneck Liner 5880/5890/6890 4 x 78.5 x 6.45
B (y) N ea5/pk25/pk
5181-33155183-47055183-4706
–2078520786
–AG0-8173
– 5/pk 150
Split / Splitless with wool 5880/5890/6890 4 x 78.5 x 6.3 B (y) Y ea 210-4004 – AG0-8174 5/pk 85
Split / Splitless, Single Taper with wool
5880/5980/6890 4 x 78.5 x 6.3 B (y) Y ea5/pk25/pk
5183-4711 210-40225183-47125183-4713
–2240622407
AG0-8175 5/pk 125
* B= Borosilicate; Deactivated = Yes (y) or No (n). ** Similar to but not always an exact equivalent to the original manufacturer’s product.
Cool-Lock™ for Shimadzu GC System Part No. Description Unit PriceAG0-8419 Cool-Lock GC Capillary Nut For Use With Short-
Style Ferrulesea $ 75
AG0-8420 Cool-Lock Nut Installation Gauge ea 69
Gold Inlet Base SealsPart No. Description Similar to Mfr. No.* Unit PriceStandard, single groove for splitless applications, 0.8 mm dia. inlet holeAG0-7518 Gold Inlet Base Seal, splitless (single
groove), 0.8 mm18740-20885 2/pk $ 70
AG0-7519 Gold Inlet Base Seal, splitless (single groove), 0.8 mm
18740-20885 10/pk 295
High Split Flow, cross groove for split applications, 0.8 mm dia. inlet holeAG0-7520 Gold Inlet Base Seal, split (double
groove/cross), 0.8 mm5182-9652 2/pk 79
AG0-7521 Gold Inlet Base Seal, split (double groove/cross), 0.8 mm
5182-9652 10/pk 309
Replacement Inlet Seal WashersAG0-7522 Inlet Seal Washers, for Agilent GC
injection port– 12/pk 33
Cool-Lock™ for Agilent HP GC System Part No. Description Unit PriceAG0-8319 Cool-Lock GC Capillary Nut For Use With Short-
Style Ferrulesea $ 75
AG0-8320 Cool-Lock GC Capillary Nut For Use With Long- Style Ferrules
ea 75
AG0-8349 Cool-Lock Nut Installation Gauge ea 69
Sealing O-RingsSealing Rings for Agilent Inlet LinersPart No. Description Similar to Mfr. No.* Unit PriceAG0-7326 Sealing ring, Viton, rated to
< 300 °C5180-4182 10/pk $ 28
AG0-7327 Sealing ring, graphite, rated to > 250 °C (450 °C max.)
5180-4168 10/pk 41
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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hPLc coLumnS
HPLC
SecurityGuard™ Analytical Cartridges require universal holder Part No.: KJO-4282
™
Luna®
High Speed Technology (HST) Columns2.5 μm High Speed Technology (HST) Columns (mm)Phase 30 x 2.0 50 x 2.0 100 x 2.0 50 x 3.0 100 x 3.0
$ 430 $ 475 $ 610 $ 475 $ 610Luna 2.5 µm C18(2)-HST 00A-4446-B0 00B-4446-B0 00D-4446-B0 00B-4446-Y0 00D-4446-Y0
4 µm Analytical Columns (mm) SecurityGuard™ Cartridges (mm)Phases 30 x 4.6 50 x 4.6 100 x 4.6 150 x 4.6 250 x 4.6 4 x 3.0
$ 375 $ 399 $ 540 $ 615 $ 635 $ 319 /10pkMax-RP 00A-4337-E0 00B-4337-E0 00D-4337-E0 00F-4337-E0 00G-4337-E0 AJ0-6074Hydro-RP 00A-4375-E0 00B-4375-E0 00D-4375-E0 00F-4375-E0 00G-4375-E0 AJ0-7511Fusion-RP 00A-4424-E0 00B-4424-E0 00D-4424-E0 00F-4424-E0 00G-4424-E0 AJ0-7557
for ID: 3.2-8.0 mm
Synergi HPLC Columns4 µm Microbore and Minibore Columns (mm) SecurityGuard™ Cartridges (mm)Phases 50 x 1.0 150 x 1.0 250 x 1.0 30 x 2.0 50 x 2.0 100 x 2.0 150 x 2.0 250 x 2.0 4 x 2.0
$ 410 $ 610 $ 635 $ 375 $ 425 $ 510 $ 599 $ 635 $ 319 /10pkMax-RP 00B-4337-A0 00F-4337-A0 – 00A-4337-B0 00B-4337-B0 00D-4337-B0 00F-4337-B0 00G-4337-B0 AJ0-6073Hydro-RP 00B-4375-A0 00F-4375-A0 00G-4375-A0 00A-4375-B0 00B-4375-B0 00D-4375-B0 00F-4375-B0 00G-4375-B0 AJ0-7510Fusion-RP 00B-4424-A0 00F-4424-A0 – 00A-4424-B0 00B-4424-B0 00D-4424-B0 00F-4424-B0 00G-4424-B0 AJ0-7556
for ID: 2.0-3.0 mm
4 µm Narrow Bore Columns (mm) SecurityGuard™ Cartridges (mm)Phases 50 x 3.0 75 x 3.0 100 x 3.0 150 x 3.0 250 x 3.0 4 x 2.0
$ 405 $ 499 $ 540 $ 605 $ 630 $ 319 /10pkMax-RP 00B-4337-Y0 00C-4337-Y0 00D-4337-Y0 00F-4337-Y0 00G-4337-Y0 AJ0-6073Hydro-RP 00B-4375-Y0 00C-4375-Y0 00D-4375-Y0 00F-4375-Y0 00G-4375-Y0 AJ0-7510Fusion-RP 00B-4424-Y0 00C-4424-Y0 00D-4424-Y0 00F-4424-Y0 00G-4424-Y0 AJ0-7556
for ID: 2.0-3.0 mm
3 μm Microbore and Minibore Columns (mm) SecurityGuard™ Cartridges (mm)Phases 30 x 1.0 50 x 1.0 150 x 1.0 30 x 2.0 50 x 2.0 100 x 2.0 150 x 2.0 4 x 2.0
$ 385 $ 420 $ 635 $ 385 $ 430 $ 550 $ 635 $ 319 /10pkC8(2) 00A-4248-A0 00B-4248-A0 00F-4248-A0 00A-4248-B0 00B-4248-B0 00D-4248-B0 00F-4248-B0 AJ0-4289C18(2) 00A-4251-A0 00B-4251-A0 00F-4251-A0 00A-4251-B0 00B-4251-B0 00D-4251-B0 00F-4251-B0 AJ0-4286HILIC — — — — 00B-4449-B0 00D-4449-B0 00F-4449-B0 AJ0-8328PFP(2) — — — 00A-4447-B0 00B-4447-B0 00D-4447-B0 00F-4447-B0 AJ0-8326
for ID: 2.0-3.0 mm
3 μm Analytical Columns (mm) SecurityGuard™ Cartridges (mm)Phases 50 x 3.0 150 x 3.0 30 x 4.6 50 x 4.6 100 x 4.6 150 x 4.6 4 x 2.0 4 x 3.0
$ 420 $ 635 $ 385 $ 420 $ 550 $ 630 $ 319 /10 pk $ 319 /10 pkC8(2) 00B-4248-Y0 00F-4248-Y0 00A-4248-E0 00B-4248-E0 00D-4248-E0 00F-4248-E0 AJ0-4289 AJ0-4290C18(2) 00B-4251-Y0 00F-4251-Y0 00A-4251-E0 00B-4251-E0 00D-4251-E0 00F-4251-E0 AJ0-4286 AJ0-4287HILIC 00B-4449-Y0 00F-4449-Y0 — — 00D-4449-E0 00F-4449-E0 AJ0-8328 AJ0-8329PFP(2) 00B-4447-Y0 00F-4447-Y0 — 00B-4447-E0 00D-4447-E0 00F-4447-E0 AJ0-8326 AJ0-8327
for ID: 2.0-3.0 mm 3.2-8.0 mm
5 μm Analytical Columns (mm) SecurityGuard™ Cartridges (mm)Phases 50 x 3.0 150 x 3.0 30 x 4.6 50 x 4.6 75 x 4.6 4 x 2.0 4 x 3.0
$ 405 $ 590 $ 375 $ 399 $ 495 $ 319 /10 pk $ 319 /10 pkC8(2) 00B-4249-Y0 00F-4249-Y0 00A-4249-E0 00B-4249-E0 00C-4249-E0 AJ0-4289 AJ0-4290C18(2) 00B-4252-Y0 00F-4252-Y0 00A-4252-E0 00B-4252-E0 00C-4252-E0 AJ0-4286 AJ0-4287PFP(2) 00B-4448-Y0 00F-4448-Y0 00A-4448-E0 00B-4448-E0 — AJ0-8326 AJ0-8327
for ID: 2.0-3.0 mm 3.2-8.0 mm
5 μm Microbore and Minibore Columns (mm) SecurityGuard™ Cartridges (mm)Phases 30 x 2.0 50 x 2.0 150 x 2.0 4 x 2.0
$ 375 $ 425 $ 585 $ 319 /10 pkC8 (2) 00A-4249-B0 00B-4249-B0 00F-4249-B0 AJ0-4289C18 (2) 00A-4252-B0 00B-4252-B0 00F-4252-B0 AJ0-4286PFP(2) 00A-4448-B0 00B-4448-B0 00F-4448-B0 AJ0-8326
for ID: 2.0-3.0 mm
5 μm Analytical Columns (mm) continued SecurityGuard™ Cartridges (mm)Phases 100 x 4.6 150 x 4.6 250 x 4.6 4 x 3.0
$ 540 $ 615 $ 635 $ 319 /10 pkC8(2) 00D-4249-E0 00F-4249-E0 00G-4249-E0 AJ0-4290C18(2) 00D-4252-E0 00F-4252-E0 00G-4252-E0 AJ0-4287HILIC 00D-4450-E0 00F-4450-E0 00G-4450-E0 AJ0-8329PFP(2) 00D-4448-E0 00F-4448-E0 00G-4448-E0 AJ0-8327
for ID: 3.2-8.0 mm
Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com Phenomenex | TeL: 310-212-0555 | Fax: 310-328-7768 | emaiL: [email protected] | Web: WWW.Phenomenex.com
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If Luna, Gemini, or Synergi analytical columns do not perform as well or better than your current HPLC column of similar phase, mass and size, send in your comparative data within 45 days and keep the Gemini, Luna or Synergi analytical column for FREE!
p. 33
hPLc coLumnS
HPLC
Trademarks Gemini, Luna, and Strata are registered trademarks of Phenomenex, Inc. Cool-Lock, MercuryMS, PhenoBlue, PhenoGreen, PhenoGrey, PhenoRed, Strata-X, Synergi, and Zebron are trademarks of Phenomenex, Inc. Strata-X is patented by Phenomenex, Inc. Bond Elute Certify is a registered trademark of Varian, Inc. Clean Screen and XtrackT are registered trademarks of United Chemical Technologies, Inc. Narc-2 is a trademark of Mallinckrodt Baker, Inc. ISOLUTE is a registered trademark of Biotage. Oasis is a registered trademark of Waters Corp.
Disclaimer Phenomenex is not affiliated with Agilent, Varian, Inc., United Chemical Technologies, Inc., Mallinckrodt Baker, Inc., or Biotage. Subject to Phenomenex Standard Terms and Conditions, which may be viewed at www.phenomenex.com/TermsAndConditions.
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MercuryMS™ Cartridge HoldersStandard Cartridge HoldersPart No. Description PriceCH0-5846 10 mm standard holder $ 115CH0-5845 20 mm standard holder 109Direct-Connect Cartridge HoldersPart No. Description PriceCH0-7187 10 mm direct-connect holder $ 109CH0-7188 20 mm direct-connect holder 109
MercuryMS® Cartridges and ColumnsCartridges (mm) Columns (mm)Qty Pricing 10 x 2.0 10 x 4.0 20 x 2.0 20 x 4.0 20 x 2.0 20 x 4.0
1 @ $ 270 /ea 1 @ $ 270 /ea 1 @ $ 270 /ea 1 @ $ 270 /ea $ 390 $ 390 3 @ $ 265 /ea 3 @ $ 265 /ea 3 @ $ 265 /ea 3 @ $ 265 /ea — — 5 @ $ 260 /ea 5 @ $ 260 /ea 5 @ $ 260 /ea 5 @ $ 260 /ea — — 10 @ $ 250 /ea 10 @ $ 250 /ea 10 @ $ 250 /ea 10 @ $ 250 /ea — —
2.5 μm PhaseSynergi Hydro-RP 00N-4387-B0-CE 00N-4387-D0-CE 00M-4387-B0-CE 00M-4387-D0-CE 00M-4387-B0 00M-4387-D0Synergi Max-RP 00N-4372-B0-CE 00N-4372-D0-CE 00M-4372-B0-CE 00M-4372-D0-CE 00M-4372-B0 00M-4372-D0Synergi Fusion-RP 00N-4423-B0-CE 00N-4423-D0-CE 00M-4423-B0-CE 00M-4423-D0-CE 00M-4423-B0 00M-4423-D0
3 μmLuna C18(2) 00N-4251-B0-CE 00N-4251-D0-CE 00M-4251-B0-CE 00M-4251-D0-CE 00M-4251-B0 00M-4251-D0Luna C8(2) 00N-4248-B0-CE 00N-4248-D0-CE 00M-4248-B0-CE 00M-4248-D0-CE 00M-4248-B0 00M-4248-D0Gemini C18 Inquire Inquire 00M-4439-B0-CE 00M-4439-D0-CE 00M-4439-B0 00M-4439-D0
5 μm Luna C18(2) 00N-4252-B0-CE 00N-4252-D0-CE 00M-4252-B0-CE 00M-4252-D0-CE — —Luna C8(2) 00N-4249-B0-CE 00N-4249-D0-CE 00M-4249-B0-CE 00M-4249-D0-CE — —Gemini C18 — — 00M-4435-B0-CE 00M-4435-D0-CE — —
3 μm Analytical Columns (mm) SecurityGuard™ Cartridges (mm)Phases 30 x 4.6 50 x 4.6 100 x 4.6 150 x 4.6 250 x 4.6 4 x 3.0*
$ 390 $ 450 $ 575 $ 645 $ 675 $ 319 /10pkC18 00A-4439-E0 00B-4439-E0 00D-4439-E0 00F-4439-E0 00G-4439-E0 AJ0-7597
for ID: 3.2-8.0 mm
5 μm Analytical Columns (mm) SecurityGuard™ Cartridges (mm)Phases 30 x 4.6 50 x 4.6 100 x 4.6 150 x 4.6 250 x 4.6 4 x 3.0*
$ 380 $ 420 $ 550 $ 620 $ 650 $ 319 /10pkC18 00A-4435-E0 00B-4435-E0 00D-4435-E0 00F-4435-E0 00G-4435-E0 AJ0-7597
for ID: 3.2-8.0 mm
Gemini®3 μm Microbore, Minibore and Narrow Bore Columns (mm) SecurityGuard™ Cartridges (mm)
Phases 50 x 1.0 30 x 2.0 50 x 2.0 100 x 2.0 150 x 2.0 50 x 3.0 100 x 3.0 150 x 3.0 4 x 2.0*$ 425 $ 399 $ 450 $ 575 $ 650 $ 420 $ 575 $ 640 $ 319 /10pk
C18 00B-4439-A0 00A-4439-B0 00B-4439-B0 00D-4439-B0 00F-4439-B0 00B-4439-Y0 00D-4439-Y0 00F-4439-Y0 AJ0-7596for ID: 2.0-3.0 mm
5 μm Minibore and Narrow Bore Columns (mm) SecurityGuard™ Cartridges (mm)Phases 30 x 2.0 50 x 2.0 150 x 2.0 250 x 2.0 50 x 3.0 100 x 3.0 150 x 3.0 250 x 3.0 4 x 2.0*
$ 380 $ 435 $ 590 $ 655 $ 655 $ 550 $ 625 $ 655 $ 319 /10pkC18 00A-4435-B0 00B-4435-B0 00F-4435-B0 00G-4435-B0 00B-4435-Y0 00D-4435-Y0 00F-4435-Y0 00G-4435-Y0 AJ0-7596
for ID: 2.0-3.0 mm
* SecurityGuard Analytical Cartridges Require Holder, Part No.: KJ0-4282
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