分散固相萃取-高效液相色谱-串联质谱法测定水产品中19种喹诺酮类兽药残留

Simultaneous Determination of 19 Quinolones Residues in Aquatic Product Using DSPE and High Performance Liquid Chromatography-tandem Mass Spectrometry

建立了高效液相色谱-电喷雾串联质谱联用测定水产品中19种喹诺酮类兽药残留的方法。采用酸化乙腈溶液进行提取,用固相填料进行分散固相萃取净化。以甲醇和0.1%甲酸溶液作为流动相,C18作为分析色谱柱,采用梯度洗脱方式进行液相色谱分离,选择离子反应监测模式检测19种喹诺酮类药物,内标方法定量。在2.0~100.0μg/L范围内,19种喹诺酮类药物的线性相关系数均大于0.99。通过添加回收试验,方法的定量限（S/N=10）为1.0μg/kg,3个添加水平中,小龙虾的回收率为70.5%~112.6%,相对标准偏差为3.5%~8.9%,鮰鱼的回收率为70.2%~113.8%,相对标准偏差为4.5%~8.9%。

A method for the simultaneous analysis of 19 quinolones residues in aquatic product was developed by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.The treated samples were extracted using buffered acetonitrile and cleaned up using Dispersive SPE（DSPE）.The HPLC separation was performed on a C18 column with a linear gradient elution program of methanol and 0.1% formic acid solution as the mobile phase.Selective reaction monitoring（SRM） was used for the selective detection of 19 quinolones.The linearity of all the 19 quinolones in the range from 2 μg/L to 100 μg/L had correlation coefficient greater than 0.99.In the detection of spiked samples,the detection limit of the method was 1.0 μg/kg for all the 19 quinolones.The method recovery in red swamp crayfish was 70.5%～112.6%,the RSD was 3.5%～8.9%,and the method recovery in longsnout catfish was 70.2%～113.8%,the RSD was 4.5%～8.9%.