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Quantitative Determination Method for Residual Colistin A/B in Edible Meats and Milk by Liquid Chromatography-Tandem
Takayuki Nakajima1, Chieko Nagano2, Hiroki Okubo3
1Meiji Pharmaceutical University, Laboratory of Food Hygienic Chemistry, 2-522-1, Noshio, Kiyose city, Japan.
Background:
Colistin is a polypeptide antibiotic serving as a crucial "last-resort" agent against multidrug-resistant Gram-negative bacteria.
Objective:
This study aimed to develop a reliable analytical method for the determination of colistin A and B residues in food matrixes using LC-tandem mass spectrometry (LC-MS/MS).
Methods:
Test portions were extracted with methanol-water (1 + 1) under hydrochloric acid-acidified conditions, followed by a secondary extraction with 0.1 mol/L hydrochloric acid. The extracts were cleaned using a weak cation-exchange (WCX) cartridge, and chromatographic separation was performed on a biphenyl column with gradient elution, followed by LC-MS/MS.
Results:
The developed method produced sharp and symmetrical peaks for colistin A and B, with no significant matrix effects (ME). Recoveries ranged from 81 to 105.9% across all analytes and matrixes, and both repeatability and reproducibility met the target criteria specified in the Japanese guidelines for method validation. The LOQs were 20 ng/g in bovine and swine muscles for colistin A and 10 ng/g for others.
Conclusion:
An LC-MS/MS method was established for quantitative determination of colistin A and B residues in food matrixes. The validation results met all performance criteria of the Japanese guidelines, confirming that the method provides reliable and precise measurements suitable for food residue monitoring.
Highlights:
Reliable quantification of colistin residues was achieved using three distinct retention modes, enabling reliable monitoring of residues in foods.
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