AOAC Final Action Methods in 2019

Table 2015.14D. Conditions for MS transitions on a Waters TQ-S along with retention time windows

Collision energy (V) Dwell time, s

Compound

Function No.

Start, min End, min

Molecular ion Fragment ion Cone voltage

Nicotinamide a Nicotinamide

1 1 1 1 2 2 2 2 3 3 3 3 4 4 4 4 5 5 5 5 6 6 6 6 7 7 7 7

2.71 2.71 2.71 2.71 0.50 0.50 0.50 0.50 1.76 1.76 1.76 1.76 0.50 0.50 0.50 0.50 2.41 2.41 2.41 2.41 3.01 3.01 3.01 3.01 4.21 4.21 4.21 4.21

3.20 3.20 3.20 3.20 1.70 1.70 1.70 1.70 2.70 2.70 2.70 2.70 1.70 1.70 1.70 1.70 3.00 3.00 3.00 3.00 3.60 3.60 3.60 3.60 5.00 5.00 5.00 5.00

122.9 122.9 127.0 127.0 124.0 124.0 128.0 128.0 168.0 168.0 171.0 171.0 169.0 169.0 172.0 172.0 170.0 170.0 174.0 174.0 265.1 265.1 269.0 269.0 377.0 377.0 383.0 383.0

80.1 96.0 84.0

20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0

16.0 16.0 16.0 16.0 16.0 16.0 16.0 16.0 22.0 12.0 22.0 12.0 20.0 12.0 20.0 12.0 18.0 12.0 18.0 12.0 30.0 12.0 30.0 12.0 35.0 20.0 35.0 20.0

0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025 0.025

2 H 2 H

4 -nicotinamide a 4 -nicotinamide

100.0

Nicotinic acid a Nicotinic acid

80.0

106.0

2 H 2 H

4 -nicotinic acid a 4 -nicotinic acid

84.1

109.0

Pyridoxal Pyridoxal a

94.0

150.0

2 H 2 H

3 -pyridoxal 3 -pyridoxal a

97.0

153.0 134.0 152.0 136.0 155.0 134.0 152.0 138.0 156.0

Pyridoxamine Pyridoxamine a

2 H 2 H

3 -pyridoxamine 3 -pyridoxamine a

Pyridoxine a Pyridoxine

13 C 13 C

4 -pyridoxine a 4 -pyridoxine

Thiamine Thiamine a

81.0

122.0

13 C 13 C

4 -thiamine 4 -thiamine a

81.0

122.0 172.0 243.0 175.0 249.0

Riboflavin Riboflavin a

13 C 13 C

4 , 4 ,

15 N 15 N

2 -riboflavin 2 -riboflavin a

0.025 Although the mass transitions are expected to remain the same across instrument platforms, the other parameters may need to be adjusted to maximize sensitivity. a  Primary transition used in quantitation.

(e)  For vitamins B 3 and B 6 , the reported concentration of the directly measured forms are summed to report total. For example, concentration of nicotinamide and nicotinic acid are summed to report “Total B 3 ” and concentration of pyridoxal, pyridoxamine, and pyridoxine are summed to report “Total B 6 .” Thiamine and riboflavin do not require this step as their forms are hydrolyzed into a single directly measured form. References: J. AOAC Int . 99 , 776(2016)

where [Vit] WSx = vitamin concentration in the working standard in ng/mL; [Vit] MWS = concentration of vitamin in the MWS in ng/mL; Vol MWS = volume of the MWS in μL; and 500 = dilution factor. (d)  Vitamin concentration calculated in product from analytical result:

DOI: 10.5740/jaoacint.15-0315 (First Action) J. AOAC Int . (future issue) (Final Action) DOI: 10.1093/jaoacint/qsaa012 AOAC SMPR 2015.002 (Vitamin B 1 ) J. AOAC Int . 98 , 1094(2015) DOI: 10.5740/jaoac.int.SMPR2015.002

where [Vit] sample = vitamin concentration in product, μg/kg; [Vit] AS = vitamin mass in the analytical sample as calculated from calibration curve, ng/mL; RW = reconstitution weight (total), g, for direct weight (liquid) samples RW = 1; SW = analytical sample weight, g; PW = powder weight (for reconstituted samples), g, for liquid samples, this value is 1; and 500 = dilution factor.

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