QuEChERS-超高效液相色谱串联质谱法同时测定鸡肉中7类42种兽药残留的研究

Simultaneous Determination of 7 Kinds of 42 Veterinary Drugs Residues in Chicken Meat by QuEChERS-ultra High Performance Liquid Chromatography-tandem Mass Spectrometry

为了建立Qu ECh ERS结合超高效液相色谱-电喷雾电离串联质谱同时测定鸡肉中磺胺类、喹诺酮类、四环素类、酰胺醇类、大环内酯类、镇静剂类和金刚烷胺药物残留的分析方法,试验通过准确称取2 g均质样品,经Mcllvaine-Na_(2)EDTA缓冲溶液、[C_(4)MIN]Cl溶液和甲酸乙腈溶液超声提取,氯化钠(Na Cl)盐析,无水硫酸镁(Mg SO_(4))、乙二胺-N-丙基硅烷化硅胶(PSA)和十八烷基硅烷键合硅胶(C18)净化后,超高效液相色谱-电喷雾电离串联质谱采用正、负电喷雾电离源,多反应监测(Multiple reaction monitoring,MRM)模式进行检测。结果显示:在最优试验条件下测得磺胺类、四环素类、氟喹诺酮类、酰胺醇类、大环内酯类、镇静剂类和金刚烷胺在1.0~100.0 ng/mL范围内线性良好,相关系数(R2)均大于0.99;方法定量限为2.0~6.0μg/kg;在3个浓度添加水平下,平均回收率为72.5%~104%,RSD为2.37%~13.6%。研究结果表明试验建立的方法操作简单,具有很好的精密度与准确度,适合鸡肉中磺胺类、四环素类、氟喹诺酮类、酰胺醇类、大环内酯类、镇静剂类和金刚烷胺药物残留的同时检测。

This study aimed to establish a method for simultaneous determination of sulfonamides,quinolones,tetracyclines,amphenicols,macrolides,sedatives,amantadine residues in chicken meat by QuEChERS-ultra high performance liquid chromatography-electrospray ionization tandem mass spectrometry(UHPLC-MS/MS).The target analytes in 2.0 g homogeneous samples were extracted by Mcllvaine-Na_(2)EDTA buffer solution,[C_(4)MIN]Cl solution and formic acid acetonitrile and salted out with sodium chloride(NaCl),then purified with magnesium sulfate(MgSO_(4)),primary secondary amine(PSA),C18 sorbent,and finally quantified by UHPLC-MS/MS in multiple reaction monitoring mode(MRM)via positive and negative electrospray ionization.The results showed that the calibration curves were linear(R2>0.99)over a concentration range of 1.0 to 100.0 ng/mL.The limits of quantification were 2.0 to 6.0μg/kg.At three spiked levels,the average recoveries ranged from 72.5%to 104%with the relative standard deviation(RSD)of 2.37%to 13.6%.This method was simple and accurate,which was suitable for the simultaneous determination of sulfonamides,quinolones,tetracycline,amphenicols,macrolides,sedatives,amantadine residues in chicken meat.