超高效液相色谱—串联质谱法检测猪肝中乙酰异戊酰泰乐菌素残留

摘要

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for determination of acetylisovaleryltylosin in swine liver. The target drug was extracted from sample with EDTA-Mcll-vaine's and the extract was cleaned up on an Oasis HLB cartridge. Separation was performed on C18 column with acetonitrile-0. 1% formic acid(7:3.V/V) as the mobile phase. The identification of drug was carried out by positive electrospray ioniza-tion (ESI+) under selective ion monitoring mode (SIM). The calibration curve of the drug showed excellent linearity within the range of 5 to 2000 ng/mL and the correlation coefficient was more than 0. 99. The average recoveries from spiked swine liver at levels of 5 to 500 μg/kg ranged from 84. 9% to 88.1 % , the intra-day coefficient variation was in range of 8. 2% to 15. 1 % and inter-day coefficient variation was in range of 14. 7% to 16. 5%. The limit of detection (LOD) was 0. 76 μg/kg and limit of quantification (LOQ) was 2. 51 μg/kg. The method was accurate and sensitive, so it could be used for determining of acetylisovaleryltylosin in swine liver.%本研究建立了猪肝中乙酰异戊酰泰乐菌素残留的超高效液相色谱—串联质谱检测方法(UPLC-MS/MS).样品经EDTA-McIlvaine's缓冲液提取,HLB固相萃取柱净化后,采用C18色谱柱分离,以乙腈-0.1％甲酸(7；3,v/v)为流动相洗脱,电喷雾正离子模式电离,选择离子监测模式检测.结果表明,药物浓度与峰面积在5～2000 ng/mL范围内呈现良好的线性关系,相关系数大于0.99,对空白猪肝组织进行5～500 μg/kg的药物添加回收试验,经统计分析获得平均回收率约为84.9％～88.1％,批内变异系数为8.2％～15.1％,批间变异系数为14.7％～16.5％.本方法对乙酰异戊酰泰乐菌素的检测限为0.76 μg/kg,定量限为2.51μg/kg,方法灵敏、准确,适用于猪肝脏中乙酰异戊酰泰乐菌素残留的检测.