多壁碳纳米管净化-超高效液相色谱-串联质谱法测定鸡蛋中44种药物残留

Determination of 44 Drug Residues in Eggs by Purified Multi-wall Carbon Nanotubes-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立超高效液相色谱-串联质谱(HPLC-MS/MS)法同时测定鸡蛋中44种药物的残留量。样品加入乙腈沉淀蛋白后,再经多壁碳纳米管、十八烷基键合硅胶、乙二胺-N-丙基硅烷组合技术净化后,以0.1%甲酸溶液-0.1%甲酸甲醇为流动相进行梯度洗脱分离,以电喷雾离子源在正、负离子多反应监测模式下进行测定,用基质匹配标准曲线外标法定量。结果表明,44种药物在0.1~200 ng/mL范围内线性良好,R^2为0.9909~0.9999,方法检出限0.007~0.3571μg/kg,定量限为0.005~1.190μg/kg,样品回收率在77.9%~114.5%,相对标准偏差小于10%(n=6)。该方法操作简便,灵敏度高,适用于鸡蛋中药物残留的高通量筛查。

A method was established for the simultaneous determination of 44 kinds of residues in eggs by ultra-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The sample was added with acetonitrile for protein deposition,then purified by techniques function composition of multi-walled carbon nanotubes,octadecyl bonded silica gel and ethylenediamine-N-propyl silane portfolio.It was gradient eluted and seperated with a 0.1%formic acid solution-0.1%formic acid methanol as mobile phase,measured under the monitoring mode that with electrospray ion source multiple reaction monitoring mode in positive and negative ions,and quantitated by using the matrix matching quantitative standard curve external standard method.The results showed that the 44 drugs had good linearity in the range of 0.1~200 ng/mL,R^2 was 0.9909~0.9999,the detection limit was 0.007~0.3571μg/kg,the quantitative limit was 0.005~1.190μg/kg,the recovery rate was 77.9%~114.5%,and the relative standard deviation was less than 10%(n=6).The method is simple,sensitive and apply to a high throughput screening of drug residues in eggs.