AOAC SPIFAN Review Team Meeting Book-December 2015
2011.06 (Fol-22) w/SLV FOR ERP USE ONLY DO NOT DISTRIBUTE
Silliker Chem, Res. Center Crete, IL – Report of A Validation of LC-MS/MS Method for Folate Analysis
6.50 6.55 9.00
0.500 0.500 0.500
100.0
0.0
0.0 A = 1%Acetic Acid in Water B = 100% Methanol
Column Temperature: 40 ° C Autosampler Temperature: 6 ° C
Injection Solvent: Std., samples and blanks injection solvent is 90% MeOH + 10% Formic acid + 1% ascorbic acid neutralized to pH 7 with ammonium hydroxide (29%) containing 50 uL/mL. Injection Volume = 2 uL
Table 6: LC Conditions using Shimadzu LC in front of API 3200 MS detector :
Flow (mL/min)
Time (min)
%B
0.10 1.00 8.00 8.01 8.02
0.1 0.1 100
0.2 0.2
0.2 0.3
10.00 10.10 11.00 11.01 12.00 15.00
100 0.1
0.3 0.2
0.1
(Stop)
A = 1%Acetic Acid in Water B = 100% Methanol
Column Temperature: 40 ° C Autosampler Temperature: 6 ° C
Injection Solvent: Std., samples and blanks injection solvent is 90% MeOH + 10% Formic acid + 1% ascorbic acid neutralized to pH 7 with ammonium hydroxide (29%) containing 50 uL/mL. Injection Volume = 2 uL MS Conditions for API 5500 (Qtrap): MS conditions API 5500 (Qtrap) for detection of different transitions of the analytes in the scope Table 7: MS conditions API 5500 (Qtrap) for detection of different transitions of the analytes in the scope Comp ound Q1 Q3 DP EP CEP CE CXP FA 442.2 295.2 75 6 6 20 6
13
Made with FlippingBook