液相色谱-串联质谱法测定羊肉中红霉素残留量

Determination of Erythromycin Residue in Mutton by High Performance Liquid Chromatography Tandem Mass Spectrometry

建立测定羊肉中红霉素残留量的高效液相色谱-串联质谱法(LC-MS/MS),为羊肉的监督检验和红霉素残留量监控提供技术支持。采用乙腈提取,正己烷除脂低温离心的前处理方法。电喷雾离子源ESI正离子扫描,选择MRM多反应监测等质谱条件进行样品检测,内标法定量。在5μg/kg^200μg/kg浓度范围内线性关系良好(r=0.9999,n=5)。10、50、200μg/kg 3个浓度的相对回收率为97.54%~102.70%,日内精密度<7%,日间精密度<9%,检测限(LOD)为5μg/kg,定量限(LOQ)为20μg/kg,符合检测要求。建立的羊肉中红霉素残留量的LC-MS/MS检测方法操作简便,实用性强,灵敏度高,稳定性好,分离完全,峰形良好,适合羊肉中红霉素的残留量检测。

The aim of this paper was to establish a method for the determination of erythromycin residue in mutton by LC-MS/MS in order to provide a technical support for the detection of erythromycin residue in mutton.The samples were extracted with acetonitrile,centrifuged after degreased with n-hexane,cryogenic centrifugation for petreatment method.The samples were detected by electrospray ion source ESI,positive ion scanning and MRM multi reaction monitoring,and the internal standard method was used to quantify it.The linear range was 5μg/kg-200μg/kg with correlation coefficients(r=0.9999)(n=5).The relative recoveries of 10,50,200μg/kg concentrations ranged from 97.54%-102.70%while the inter-day precision was<7%and inter-day precision was<9%.The limit of detection(LOD)of the method was 5μg/kg.The limit of quantitation(LOQ)was 20μg/kg.All results met the test requirements.The developed LC-MS/MS method of the residue analysis of erythromycin in mutton has high sensitivity,good stability,complete separation and good peak shape.And it is suit for residue detection of erythromycin in mutton.