SimultaneousDetermination of SevenWater SolubleVitamins inProducts byLC-MS/MS
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TableA5. Mass Spectrometer (XevoTQ-S_ operating conditions
IonizationMode
ESI+ (Electrospray; Positive Ion)
CapillaryVoltage
2.50KV
SourceTemperature
150 ºC
SourceOffset (V)
30.0
DesolvationTemperature
500 ºC
ConeGas Flow
300L/Hr
DesolvationGas Flow
700L/Hr
Nebulizer
7 bar
MS 1Resolution
0.7PWHH*
EntranceLens
1
CollisionEnergy
Various (SeeMSParameters)
Exit Lens
1
MS 2Resolution
0.7PWHH*
Gain
1.0
CollisionCell Pressure
~3 e-3
InterscanDelay (sec)
0.003
*Parameters optimizedby IntelliStart to achieve a resolution of ~ 0.7 amu
PWHH
TableA6. Mass Spectrometer divert settings
Time (min)
Event
0.01
SolventDelay1 begin
0.01
FlowStateWaste
0.75
SolventDelay1End
0.75
FlowState LC
5.5
SolventDelay2Begin
5.5
FlowStateWaste
p)
QualityControl
i)
Analysis
(1)
Uponverifying equilibration of theUPLC system, inject theworking standards (WS1 toWS5)
followedby amobile phase blank, control sample and sample extracts.
(2)
Samplesmust be bracketedbetween two sets ofworking standards. Vitamin content inproduct
samples is thendeterminedby comparison of the response ratio for the sample to the calibration
curve.
ii)
CalibrationCurve
(1)
Inject working standards approximately every6 h of samples (e.g., 40 sampleswith analysis
cycle time of 9min) injected after the analysis of the last sample extract.
(2)
The calibration curve residuals (% deviation) are defined below:
(3)
Folic andbiotin in the 1-4 dilutionmust have deviation less than 7%
(4)
Folic acid andbiotin in the 1-16 dilutionmust have%deviations of less than 10%.
(5)
Pantothenic acid, niacin, pyridoxine, riboflavin, and thiaminemust have% deviations less than
5% in the 1-16dilution.
BIO-03
FORWORKINGGROUP/ERPUSEONLY
DONOTDISTRIBUTE
