ultra fast mass spe ctrometry - shimadzu · 20.75ppb (%rsd 8.60) vitamin e 10x sample dilution...
TRANSCRIPT
NO.3
C146-E164
Analysis of Fat Soluble VitaminsUsing the LCMS-8030 Triple Quadrupole Mass Spectrometer
Speed Beyond Comparison
Ultra Fast Mass Spectrometry
Food
No.3
High ReliabilityRobust System Provides Long-term Data Stability
UFsweeper™ Technology Dramatically Minimizes Cross Talk
Excellent Linearity with Wide Dynamic Range
User-FriendlyEasy Maintenance for Minimized Instrument Downtime
Single-vendor Solution Provides Seamless Operation
Quantitation Browser for Effective Multi-analyte Quantitation
Ultra Fast SpeedFusion of Ultra Fast MRM and Ultra Fast Polarity Switching
An Ultra Fast Scan Speed of 15,000 u/sec
500 MRMs per Second, the Most Ever Possible
Triple Quadrupole LC/MS/MS System
Liquid Chromatograph Mass Spectrometer
LCMS-8030Triple Quadrupole Mass Spectrometer
Analysis of Fat Soluble Vitamins Quantitation of Fat Soluble Vitamins in SupplementThis document describes simultaneous analyses of 7 fat soluble vitamins and
derivatives by ESI negative mode. Excellent linearity (R2=0.99 or better) was obtained in each analysis.
Table 1 Analytical Conditions
Column������Mobile phase AMobile phase BGradient programFlow rateInjection volumeColumn temperatureNebulizing gas flowDrying gas flowDL temperatureBH temperature
: Shim-pack XR-ODSⅡ (75 mmL. x 2.0 mmI.D., 2.2 μm): Methanol: Ethanol: 0 %B (0 -4min) - 50 %B (6-7 min) - 30 %B (7.01 - 10 min): 0.5 mL / min: 1μL�: 40 ˚C: 1.5 L / min: 10 L / min: 250 ˚C: 400 ˚C
MRM Mode Parameter
Transition
Vitamin AVitamin D2Vitamin D3Vitamin EVitamin E acetateVitamin K1Vitamin A palmitate
269>93397>69385>107431>165473>207451>187269>93
5555555
-25-35-20-15-20-30-25
UnitUnitUnitUnitUnitUnitUnit
Sample Preparation
103.8 ng
Vitamin D210x Sample Dilution
20.75ppb (%RSD 8.60)
Vitamin E10x Sample Dilution
2379ppb (%RSD 4.48)
Vitamin E acetate1000x Sample Dilution8913ppb (%RSD 1.46)
Vitamin K110x Sample Dilution
1191ppb (%RSD 2.04)
11.90μg 44.57μg 5.955μg
Transition Dwell time (ms)
CE(eV)
MS2resolution
5tablets Add 25mL n-hexane and mix for 30 seconds then heat (60˚C, 45min)
Mix for 30 seconds,Centrifuge(3,000rpm, 10min)
Filter supernatant (0.2um)
→ → →
Vitamin A
0.0
2.5
(x1,000,000)
Vitamin D2
1.0
2.0
(x1,000,000)
0.0
Vitamin E
0.0
1.0
2.0
3.0
(x1,000,000)
Vitamin K1
0.0
2.5
5.0 (x1,000,000)
Vitamin A palmitate
0.0 1.0 2.0 3.0 4.0 5.0 6.0 min
0.5
1.0
(x100,000)
0.0
Vitamin E acetate
0.5
1.0
(x10,000,000)
0.0
Vitamin D3
1.0
2.0
(x1,000,000)
0.0
0 250 500 750 Con. 0.00
0.50
1.00
1.50
Area (x100,000)
0 250 500 750 Con. 0.00
0.25
0.50
0.75
1.00
Area (x100,000)
Area (x100,000)
0 250 500 750 Con.
0 250 500 750 Con.
0.0
0.5
1.0
0.0
0.5
1.0 Area (x10,000,000)
0.0
2.0
4.0
6.0
8.0
Area (x100,000)
Area (x100,000)
1.25 1.50
0.0
2.0
4.0
6.0
8.0
397.40>69.15(+)
1.34
4
1.50 1.75
0.0
0.5
1.0
(x100,000) (x100) 431.40>165.10(+)
1.67
9
2.25 2.46
0.0
0.5
1.0
1.5
(x1,000,000) 473.40>207.05(+)
2.27
2
3.00 3.25
0.0
1.0
2.0
(x1,000) 451.40>187.25(+)
3.06
8
0 20000 40000 Con.
0 20000 40000 Con.
0.0
2.0
4.0
6.0
0 20000 40000 Con. 0.0
1.0
2.0
3.0
Area (x100,000)
Printed in Japan 3295-05104-30AIT