QuEChERS EMR-Lipid结合LC/MS/MS测定水产品中15种喹诺酮类抗生素

Determination of 15 Kinds of Quinolones Antibiotics in Aquaculture Products Employing QuEChERS EMR-Lipid Combined with UPLC-MS/MS

建立QuEChERS EMR-Lipid技术结合超高效液相色谱-串联三重四极杆质谱(UPLC-MS/MS)同时测定养殖水产品中15种喹诺酮抗生素的快速检测方法。使用1%甲酸乙腈水溶液(V_(乙腈)︰V_(水)=4︰1)提取,净化方法采用QuEChERS EMR-Lipid技术,氮吹浓缩后的溶液通过Agilent Eclipse Plus C18色谱柱分离,采用0.2%乙腈-0.2%甲酸水溶液梯度洗脱,多反应监测(MRM)模式监测,采用电喷雾正离子扫描。试验表明, 15种抗生素方法检出限(S/N=3)在0.5~2.0μg/kg,在2, 20和50μg/kg这3个添加浓度下,平均回收率为75.8%~112.3%,在1~200 ng/mL浓度范围内线性关系良好(r^(2)>0.998),δRSD在2.3%~10.2%(n=6)。以该方法对多种养殖水产样品进行分析,共检出2种喹诺酮类。试验方法前处理简单快速、净化效果好、灵敏度高,适用于养殖水产品中多组分喹诺酮类抗生素的检测。

A rapid method was developed for the simultaneous determination of 15 kinds of quinolones antibiotics in aquaculture products by QuEChERS EMR-Lipid combined with ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The samples were extracted by acetonitrile-water(4︰1, V/V) containing 1% formic acid, purified by QuEChERS EMR-Lipid, concentrated by nitrogen, separated on an Agilent Eclipse Plus C18 column by gradient elution with acetonitrile(containing 0.2% formic acid)-0.2% formic acid as mobile phase, ionized with positive electrospray ionization(ESI+/-), and detected under multiple reaction monitoring mode(MRM). The result showed that the 15 kinds of analytes presented favorable linearity between 1 ng/mL and 200 ng/mL, with correlation coefficients(r^(2))>0.998. The method detection limits(S/N=3) were 0.5-2.0 μg/kg. The average recoveries(n=6) ranged from 75.8%-112.3% at spiked levels of 2-50 μg/kg, with the relative standard deviations between 2.3% and 10.2%(n=6). The method was applied to 6 kinds of aquaculture products and 15 kinds of analytes were detected, in which enrofloxacin and ofloxacin were detected. The developed method, which was characteristic by simple pre-treatment procedure, satisfactory purification and sensitivity, was suitable for the simultaneous determination of 15 kinds of quinolones antibiotics in aquaculture products.