液相色谱—串联质谱法测定牛奶中粘杆菌素和多粘菌素B的残留量

Determination of Colistin and Polymycin B Residues in Milk by Liquid Chromatography-Tandem Mass Spetrometry

建立了同时测定牛奶中粘杆菌素和多粘菌素B素残留量的液相色谱-串联质谱（LC-MS/MS）的方法。样品通过5%高氯酸溶液沉淀蛋白,经乙醚除脂,Strata-X固相萃取柱净化,浓缩后经LC-MS/MS电喷雾正离子多反应检测模式（ESI＋MRM）检测。结果显示,粘杆菌素和多粘菌素B在25～1 000 ng/mL范围内均具有良好的线性关系,相关系数不低于0.997 2,加标回收率为71.5%～98.1%,相对标准偏差为3.8%～9.5%。试验证明该方法前处理简单,快速,稳定性好,适用于大量样品中粘菌素和多粘菌素B残留的同时检测。

A method was established to simultaneously detect colistinin and polymyein B in milk by liquid chromatography tandem mass spetrometry （LC-MS/MS）.The samples, protein was precipitated with 5% perchloric acid and the fat was removed with diethyl ether, the other impurities were removed with Strata-X solid phase extraction cartridge, after concentration, theanalvtes were detected by LC-MS/MS （ESI）with multiple reaction monitoring（MRM）.The results indicated that the calibration curves were in good linearity between the peak area and the concentration of 25~1 000 ng/mL for colistinin and polymycin B with correlation cofficients not less than 0.997 2 ,the spiked recoveries ranged from 71.5%-98.1% with reative standard deviations of 3.8%-9.5% .The proposed method was simple and rapid,the stability was good and it was suitable for the simultaneous quantitative detection of colistinin and polymycin B in milk.