Development of Analytical Method for Colistin in Fish and Shrimp using Liquid Chromatography Mass Spectrometry
2016
Shin, D., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Kang, H.S., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Lee, S.B., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Cho, Y.J., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Cheon, S.Y., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Jeong, J., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea | Rhee, G.S., National Institute of Food and Drug Safety Evaluation, Osong, Republic of Korea
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 greater than 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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