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AOAC Official Method 993.22
p-Toluenesulfonamide Residues in Ice Cream
Combined Continuous Flow and
Liquid Chromatographic Method
First Action 1993
B. Apparatus
C. Reagents
(a) Methanol.
(b) Phosphate buffer.pH 7.00, containing 3.522 g potassium
dihydrogen phosphate (KH2PO4) and 7.265 g disodium hydrogen
phosphate dihydrate (Na2HPO42H2O) in 1 L H2O (commercial
buffer solutions are suitable).
(c) CF buffer solution.Dissolve 2 g sodium chloride in 1 L
phosphate buffer, (b).
(d) Sampler wash solution.Add 1 mL polyoxyethylene lauryl
ether (Brij 35, 30% [volume/volume] in H2O, Atlas Chemical Ind.,
Wilmington, DE, and E. Merck are suitable sources) to 1 L H2O.
Mix.
(e) LC mobile phase.Methanolwater (1 + 3). Dilute 250 mL
methanol with 750 mL H2O. Filter mobile phase through 0.45 m
filter.
(f) p-TSA stock solution.1.000 mg p-TSA/L. Dissolve 100 mg
p-TSA in 10 mL 95% (volume/volume) ethanol and dilute to 100
mL with H2O. Solution is stable for at least 4 months at 4.
(g) p-TSA intermediate and standard solutions.(1) Intermediate solution.Pipet 1 mL p-TSA stock solution, (f), into 100 mL
volumetric flask and dilute to volume with H2O. (2) Standard
solutions.0.1, 0.2, 0.3, 0.4, and 0.5 mg p-TSA/L. Pipet 1, 2, 3, 4,
and 5 mL of intermediate solution into separate 100 mL volumetric
flasks and dilute to volume with H2O. Standard solutions are stable
for at least 4 weeks at 4.
(h) Vanillin stock solution.1 mg/mL. Dissolve 100 mg vanilla
(4-hydroxy-3-methoxy-benzaldehyde) in 100 mL H2O. Solution is
stable for 4 months at 4.
Dilute melted ice cream samples (ca 510 g) 1:4 (by weight) with
H2O, using balance or gravimetric diluter, B(a). Homogenize mixture ca 1 min. Remove and discard upper, fat and/or foam, layer by
suction.
E. Procedure