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Silliker

Chem, Res. Center Crete, IL – Report of A Validation of LC-MS/MS Method for Folate Analys

5

Results

Optimization of compound based mass-spec (Sciex 3200/ 5500/6500) parameters:

The compound based parameters were determined by pumping the mobile phase at 0.5 mL/min

through the HPLC pump without column. The analyte mixture solution was pumped into the MS

source by the syringe pump in the Mobile phase. The compound dependent parameters were ramped

with infusion of the analytes and the optimum values were determined for the corresponding Q1/Q3

transitions providing the strongest response. Results of the optimization of the parameters Sciex 3200

are presented in Table 1. Parameters later on optimized for the Sciex 5500 and 6500 LC-MS/MS are

provided in the method.

Table 1: Optimization of MS conditions 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

442.2 176.2

75

6

6

45

6

5-CH3-THF

460.2 313.2

75

6

6

28

6

460.2 194.2

75

6

6

46

6

5-CHO-THF

474.2 327.2

75

6

6

25

6

474.2 299.2

75

6

6

40

6

THF

446.2 299.2

75

6

6

30

6

446.2 166.2

75

6

6

50

6

5,10-CH=CH-

THF

456.2 412.2

75

6

6

42

6

456.2 282.2

75

6

6

70

6

10-CH3-FA

456.2 309.2

75

6

6

20

6

456.2 176.2

75

6

6

50

6

10-CHO-FA

470.2 295.2

75

6

6

35

6

470.2 176.2

75

6

6

50

6

13

C

5

-FA

447.2 295.2

75

6

6

20

6

13

C

5

-5-CH3-THF 465.2 313.2

75

6

6

28

6

13C5-5-CHO-THF

479.2 327.2

75

6

6

25

6

DP: Declustering potential;

EP Entrance potential;

CEP collision cell entrance potential;

CE Collision cell;

CXP collision cell exit potential.

These conditions were used for analytes detection through the study. More intense transition was used

for quantification and the other for qualification.

2011.06/Fol-22 (February 2016)

FOR ERP USE ONLY

DO NOT DISTRIBUTE