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KMID : 0881720160310050319
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Journal of Food Hygiene and Safety
2016 Volume.31 No. 5 p.319 ~ p.326
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Development of Analytical Method for Colistin in Fish and Shrimp using Liquid Chromatography Mass Spectrometry
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Shin Da-som
Kang Hui-Seung
Lee Soo-Bin
Cho Yoon-Jae
Cheon So-Young
Jeong Ji-Yoon
Rhee Gyu-Sik
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Abstract
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Colistin is a last resort antimicrobial agent against multi-drug resistant Gram-negative bacteria. This study was conducted to develop an analytical method to determine colistin in fish and shrimp. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with acidified 5% methanol (containing 0.5% formic acid). Then, solid phase extraction (SPE) was used for cleanup. Matrix-matched calibration curves were linear over the calibration ranges (0.05-1.2 mg/kg) for all the analytes into blank sample with r 2 > 0.99. All the values fulfilled the criteria requested by the Codex guidelines. Average recoveries ranged from 85.9% to 107.9%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was less than 15%. The limit of detection (LOD) was 0.02 mg/kg, and the limit of quantitation (LOQ) was 0.05 mg/kg. This improved method showed higher accuracy and acceptable sensitivity to meet the CAC guideline requirements and is applicable for the analysis of residual colistin (A+B) in fish and shrimp.
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KEYWORD
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colistin, fish, shrimp, analytical method, LC-MS/MS
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