
Contents
23.1.12
AOAC Official Method 993.32
Multiple Sulfonamide Residues in Raw Bovine Milk: Liquid Chromatographic Method
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Published:January 2023
Cite
Multiple Sulfonamide Residues in Raw Bovine Milk: Liquid Chromatographic Method', in Dr. George W Latimer, Jr. (ed.), Official Methods of Analysis of AOAC INTERNATIONAL, 22nd Edition (
Extract
First Action 1993
Final Action 1996
[Applicable to determination of 5–20 ng/mL of eight sulfonamides in raw bovine milk: sulfadiazine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfachloropyridazine, sulfadimethoxine, and sulfaquinoxaline. See also 988.08 (see 33.2.61).]
See Table 993.32 for results of the interlaboratory study supporting acceptance of the method.
Results of interlaboratory study for determination of multiple sulfonamides in raw bovine milk by liquid chromatographic method
...
(Note: In the collaborative study, post-dose milk contained peaks in addition to parent drug, and these are assumed to be metabolites. For confirmation of eluate identity, additional specificity comparable to that provided by liquid or gas chromatography combined with mass spectrometry is required.)
Principle
Sulfonamides in milk are extracted by chloroform–acetone. After solvent evaporation, residues are dissolved in aqueous potassium phosphate solution. Fatty residues are extracted with hexane. Aqueous layer is filtered and analyzed by liquid chromatography (LC). Sulfonamides are measured by ultraviolet (UV) absorption at 265 nm. Eight sulfonamides can be quantitated isocratically: five sulfonamides using 12% methanol and 4 using 30% methanol in mobile phase. Sulfamethazine is measured under either condition.
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