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

关键词:  分散固相萃取  高效液相色谱/串联质谱法  水产品  喹诺酮类兽药

Key words:  Dispersive-Solid Phase Extraction (DSPE)  HPLC-MS/MS  aquatic product  quinolones

摘要:

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。采用乙腈缓冲溶液进行提取，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。通过实际样品的添加回收试验，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 71.5%～112.4%，相对标准偏差为3.2%～9.2%，鮰鱼的回收率为70.5%～113.4%，相对标准偏差为 4.0%～8.7%。

Abstract:

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 2μg /L to 100μg /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 71.5%～112.4%， the RSD was 3.2%～9.2%, and the method recovery in longsnout catfish was 70.5%～113.4%, the RSD was 4.0%～8.7%。