LC-MS/MS를 이용한 어류 및 갑각류의 잔류 Erythromycin 항생제 분석

Determination of Residual Erythromycin Antibiotic in Fishery Products by Liquid Chromatography-electrospray Ionization Mass Spectrometry

A simple and sensitive method for erythromycin quantification by liquid chromatography electrospray mass spectrometry (LC-MS/MS) in fishery products was developed. Samples were extracted by liquid-liquid extraction using 70% acetonitrile. Lipids were removed by acetonitrile saturated hexane. LC separation was performed on a Shiseido UG C-18 column ($150\;mm{\times}2.0\;mm$ internal diameter.) with a gradient system of 0.2% acetic acid-acetonitrile containing 0.2% acetic acid as a mobile phase at flow rate of 0.2 mL/min. The mass spectrometer was operated in selected reaction monitoring with positive electro-spray interface. Transitions were monitored a m/z $734{\to}577$ and $734{\to}158$, with m/z $734{\to}577$ chosen for quantification. Recovery of erythromycin from fish and shrimp fortified at the 10 ng/mL, 50 ng/mL and 100 ng/mL were 91.6-109.4%, 84.4-111.2% and 98.8-109.6% with high precision, respectively. Limits of quantification and limits of detection of erythromycin in both fish and shrimp were 10.0 ng/mL and 1.0 ng/mL, respectively. This analysis method for erythromycin has been proposed for registration in the Korean Official Methods of Food Analysis and has been utilized for fishery products analysis by the Korea Food and Drug Adminstration and the National Fisheries Products Quality Inspection Service.