certificate of analysis · unbroken chain of measurements. uncertainty of concentration is...
TRANSCRIPT
Item No.:Batch No.:
CAS Registry No.:Molecular Formula:
Formula Weight:
Expiry Date:Supplied as:
Volume per Ampule:
Storage:Safety:
Intended Use:Instructions for Use:
ISO60156056796213956-29-1C21H30O2314.50 amu
13AUG2023 (valid from date of certification)A 1 mg/ml (nominal) solution in methanol Not less than 1 ml. Ampules are overfilled.
Unopened at -20˚C.Refer to Safety Data Sheet
For analytical testing purposes only, not intended for human or animal use.This product is designated for one-time use and should be used immediately after opening. It is advised that laboratories warm the vial to room temperature prior to opening and use measured volumes.
Approval: Title: ISO Quality Manager Certification Date: 13AUG2019
HO
OH
Page 1 of 6 Certificate #60156-0567962-01
Certified Concentration · 1.000 mg/ml ± 0.021 mg/mlConcentration is calculated based on product mass, solution mass, corrected purity, and density at 20˚C. It is traceable to SI units through an unbroken chain of measurements. Uncertainty of concentration is expressed as an expanded uncertainty in accordance with ISO standards for Testing Laboratories and Reference Material Producers at the approximate 95% confidence interval using a coverage factor of k=2 and incorporates uncertainties from the corrected purity, solution preparation, homogeneity, and long- and short-term stability. Concentration was verified bycomparison to an independently prepared calibration standard.
Corrected Purity · 99.70% ± 0.56%Corrected purity is determined as follows: Corrected Purity = [(100 - % LOD - % ROI)*Chromatographic Purity/100] or [(100 - % KF - % RS - % ROI)*Chromatographic Purity/100]. All measurement uncertainties are expressed as expanded uncertainties in accordance with ISO standards for Testing Laboratories and Reference Material Producers at the approximate 95% confidence interval using an appropriate coverage factor. Where applicable, optical rotation, chiral purity, and/or isotopic purity testing are performed to support the identification of the reference material, therefore the uncertainty is considered null.
Cannabidiol (CRM) Certified Reference Material
Cayman Chemical certifies that this standard meets the specifications stated in this certificate and warrants this product to meet the stated acceptance criteria through the expiration date when stored unopened as recommended.
CERTIFICATE of ANALYSISCRM
EXAMPLE
Page 2 of 6 Certificate #60156-0567962-01
Neat Material Quality Information (Item No.: 90080, Batch No.: 0542338)
NMR and optical rotation (if applicable) are provided as supplemental information but are not within scope of ISO accreditation.Property values are traceable to SI units through an unbroken chain of measurements.
Qualifier Method Result
Chromatographic Purity, HPLC Cayman Method TST SD151 >99.90% ± 0.18%
Identity, LC-MS Cayman Method TST SD13, +ESI 315.2 amu
Identity, GC-MS Cayman Method TST SD12 Conforms
Identity, FTIR USP<851> (diamond ATR) Conforms
% LOD Cayman Method TST SD24 <0.10% ± 0.48%
% ROI Cayman Method TST SD06 <0.10% ± 0.21%
Identity, NMR 1H NMR Conforms
Homogeneity
CRM Assay
A minimum sample size of 2.0 μg was used to determine homogeneity. Homogeneity was determined by HPLC usingampules selected from a random sampling plan from early, middle, and late fill positions.
The recommended minimum quantity for use is 2.0 μg. Quantities below this have not been evaluated.
%RSD Acceptance Criteria
1.20% ≤3%
Method ParametersCayman Method TST SD151
Column 4.6 x150 mm, 5 μm Kinetex Biphenyl
Mobile PhaseA: 0.1% Trifluoroacetic Acid in WaterB: Acetonitrile
Gradient
Time (min) %B0-12 50-90%12-17 90%17.1-22 50%
Flow Rate 1 ml/min
Column Temp 30˚C
Wavelength UV monitored at 232 nm
CERTIFICATE of ANALYSIS
EXAMPLE
Page 3 of 6 Certificate #60156-0567962-01
GC-MS
50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 3100
100000
200000
300000
400000
500000
600000
700000
800000
900000
1000000
1100000
1200000
1300000
1400000
1500000
m/z-->
Abundance Average of 10.023 to 10.074 min.: 90080-0542338.D\data.ms (-)231
246174 31419367 1219141 29977 27114710755 207159 258131 217185 28613999 239167 307279
ConditionsInstrument Agilent GC MSD
Column30 m x 0.32 mm, 0.5 µm Rtx-5MS
Carrier Gas He
Flow Rate 2 ml/min
Inlet Temp 300˚C
Split Ratio 15:1
Oven Program50oC hold for 1 min, ramp to 300oC at 30oC per min, hold at 300oC to 15 minutes
Transfer Line Temp 300˚C
Voltage 70ev EI MS
Scan Range 40-600 m/z
Tune File stune
Supplemental Data (Neat Material)
min0 2.5 5 7.5 10 12.5 15 17.5 20
mAU
0
100
200
300
400
500
600
700
800
DAD1 A, Sig=232,8 Ref=450,16 (C:\CAYMAN DATA\DATA\90080 PUR\90080 PUR 2018-10-10 15-09-10\003-0501.D)
7.54
3
HPLC-UV ConditionsInstrument Agilent 1100/1200 Series
Column4.6 x 150 mm, 5 μm Kinetex Biphenyl
Mobile PhaseA: 0.1% Trifluoroacetic Acid in WaterB: Acetonitrile
Gradient
Time (min) %B0-12 50-90%12-17 90%17.1-22 50%
Flow Rate 1 ml/min
Column Temp 30˚C
Wavelength UV monitored at 232 nm
Apex spectrum – background (1 min window in front of peak)
CERTIFICATE of ANALYSIS
EXAMPLE
Page 4 of 6 Certificate #60156-0567962-01
ESI-MS ConditionsInstrument Agilent 1100 HPLC/MSD
Mobile Phase50:50:0.1methanol/water/acetic acid
Flow Rate 0.5 ml/min
Ionization Mode +ESI
Mass Range 100-1,000 m/z
Nebulizer 60 psi
Desolvation Gas 13 L/min
Desolvation Temp 350˚C
Electrospray Voltage
4kV
100 200 300 400 500 600 700 800 900 1000
0
20
40
60
80
100
*MSD1 SPC, time=3.273 of C:\CAYMAN\DATA\FIA\CAY030.D ES-API, Pos, Scan, Frag: 70, "+ESI"
Max: 1.75565e+006
315.
231
6.2
337.
2
90080-0542338
***90080-0542338Wed Oct 10 11:44:18 2018 (GMT-04:00)Number of sample scans: 32Number of background scans: 32Resolution: 4.000Sample gain: 2.0Optical velocity: 0.4747Aperture: 80.00Detector: DTGS KBrBeamsplitter: KBrSource: IR
883.
4489
6.57
1019
.1211
50.3
312
15.5
1
1374
.81
1444
.49
1515
.20
1582
.39
1623
.32
2855
.57
2925
.15
2964
.52
3076
.09
3409
.32
3519
.74
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
%Tr
ansm
ittan
ce
100015002000250030003500Wavenumbers (cm-1)
FTIR Conditions
InstrumentThermo Nicolet iS10 FTIR / Diamond SmartATR (single bounce)
Scans32 scans /32 background scans
Range 650-4,000 cm-1
Resolution 4.000
ATR and background corrected
MS collected across peak width at half height
CERTIFICATE of ANALYSIS
EXAMPLE
Page 5 of 6 Certificate #60156-0567962-01
Stability
Short-Term Stability
The effect of the components of stability on the combined standard uncertainty of the CRM property value are considered negligible unless indicated in stability studies.
A decrease in property value was observed at 60°C during the two-week stability study. No decrease was observed at ambient temperature during the study. This data supports cold shipment of this product.
Date Oct 2 2018File Name \\sulfur\private\nmrdata\_2018\BB-1755-137_20181002_\BB-1755-137_20181002_01\BB-1755-137_20181002_001.fid\fidFrequency (MHz) 399.9677 Nucleus 1H Number of Transients 32Solvent METHANOL-d4 Temperature (degree C) 25.0001H NMR (METHANOL-d4, 400 MHz) δ 6.08 (s, 2H), 5.29 (s, 1H), 4.5-4.5 (m, 1H), 4.43 (quin, 1H, J=1.0 Hz), 3.93 (qdd, 1H, J=2.2, 4.2, 10.6 Hz), 2.8-3.0 (m, 1H), 2.38 (t, 2H, J=7.8 Hz), 2.1-2.3 (m, 1H), 2.0-2.1 (m, 1H), 1.7-1.8 (m, 2H), 1.68 (s, 3H), 1.64 (dd, 3H, J=0.8, 1.6 Hz), 1.55 (td, 2H, J=7.6, 14.9 Hz), 1.2-1.4 (m, 4H), 0.90 (t, 3H, J=6.6 Hz)
Chemical Shift (ppm)10 9 8 7 6 5 4 3 2
2.974.152.163.113.152.071.031.052.101.011.011.001.071.001.92
Water
METHANOL-d4
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
6.08
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29
5.29 4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47
4.47 4.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
474.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
444.
44 4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
4.43
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95
3.95 3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.94
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.93
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.92
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
3.91
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95
2.95 2.
942.
942.
942.
942.
942.
942.
942.
942.
942.
942.
942.
942.
942.
942.
942.
942.
942.
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942.
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942.
942.
922.
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922.
922.
922.
922.
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922.
922.
922.
922.
922.
922.
922.
92 2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.91
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.90
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89
2.89 2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.87
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.40
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.38
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.36
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02
2.02 1.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
771.
77 1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76
1.76 1.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
741.
681.
681.
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681.
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64 1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.64
1.57
1.57
1.57
1.57
1.57
1.57
1.57
1.57
1.57
1.57
1.57
1.57
1.57
1.57
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1.57
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1.57
1.57 1.
551.
551.
551.
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511.
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321.
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311.
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31
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
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1.27
1.27
1.27
1.27
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1.27
1.27
1.27
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1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
1.27
0.91
0.91
0.91
0.91
0.91
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0.91
0.91
0.91
0.91
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0.91
0.91
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0.91
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0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.90
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
0.88
NMR (not within scope of ISO accreditation)
ConditionsInstrument Varian Inova 400MHz NMR
Scans 64 scans
Long-Term Stability
Long-term stability data predicts four years stability at the -20˚C storage temperature. Long-term stability studies are ongoing and the Certificate of Analysis will be updated upon study completion.
CERTIFICATE of ANALYSIS
EXAMPLE
Page 6 of 6 Certificate #60156-0567962-01
Revision History
Revision No. Date Reason for Revision
01 13AUG2019 Initial version
Disclaimers
Material Safety DataThis material should be considered hazardous until information to the contrary becomes available. Do not ingest, swallow, or inhale. Do not get in eyes, on skin, or on clothing. Wash thoroughly after handling. This information contains some but not all of the information required for the safe and proper use of this material. Before use, review the complete Safety Data Sheet, which has been sent via email to your institution.
Warranty and Limitation of RemedyCayman Chemical Company makes no warranty or guarantee of any kind, whether written or oral, expressed or implied, including without limitation, any warranty of fitness for a particular purpose, suitability and merchantability, which extends beyond the description of the chemicals hereof. Cayman warrants only to the original customer that the material will meet our specifications at the time of delivery.
Cayman will carry out its delivery obligations with due care and skill. Thus, in no event will Cayman have any obligation or liability, whether in tort (including negligence) or in contract, for any direct, indirect, incidental or consequential damages, even if Cayman is informed about their possibleexistence.
This limitation of liability does not apply in the case of intentional acts or negligence of Cayman, its directors or its employees.
Buyer’s exclusive remedy and Cayman’s sole liability hereunder shall be limited to a refund of the purchase price, or at Cayman’s option, the replacement,at no cost to Buyer, of all material that does not meet our specification.
Said refund or replacement is conditioned on Buyer giving written notice to Cayman within thirty (30) days after arrival of the material at its destination. Failure of Buyer to give said notice within thirty (30) days shall constitute a waiver of Buyer of all claims hereunder with respect to said material.
For further details, please refer to our Warranty and Limitations of Remedy located on our website and in our catalog.
This Certificate shall not be reproduced except in full, without written approval from the Cayman Chemical ISO Quality Manager.
ISO CRT SD02 v 4.1
CERTIFICATE of ANALYSIS
CAYMAN CHEMICAL1180 EAST ELLSWORTH RDANN ARBOR, MI 48108 · USA
www.caymanchem.com
PHONE: [800] 364-9897 [734] 971-3335 FAX: [734] 971-3640
EXAMPLE