Development of analytical method for determination of spinetoram residues in livestock using LC-MS/MS

Abstract: An analytical method was developed to determine the amount of spinetoram (spinetoram J andspinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primarysecondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquidchromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactionsmonitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg)into a blank extract with r 2 > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg,respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ,10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent withthe criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conductedto validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoramdetermination. The method will be used as an official analytical method in Korea.요약: 이 연구는 수입을 포함한 국내 유통 축산물 중 spinetoram의 안전관리를 위한 공정시험법을 확립하기 위해 수행하였으며 시험법의 선택성, 검출한계 및 정량한계, 회수율에 대한 검증을 통하여 공정시험법으로의 유효성을 확인하였다. Spinetoram을 효과적으로 분석하기 위하여 LC-MS/MS를 분석기기로 사용하였고, acetonitrile으로 추출 후 PSA를 이용한 d-SPE정제법을 적용하여 시료의 불순물을 정제하