Journal of AOAC International · 2026
Quantitative Determination Method for Residual Colistin A/B in Edible Meats and Milk by Liquid Chromatography-Tandem Mass Spectrometry.
СтатьяНазвание и аннотация: Перевод в очереди
Обработка статьи · этапы, ошибки и управление
Загрузка состояния…
Ошибки и ограничения
История · было → стало
Состояние обновляется каждые 5 секунд, пока блок открыт. Процент показывается только там, где известен объём работы. Пауза останавливает продолжение этапа; текущий запрос к источнику может завершиться.
Nakajima Takayuki, Nagano Chieko, Okubo Hiroki, Koike Hiroshi, Ohba Yumi
Аннотация
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.
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.