通过式固相萃取结合UPLC-MS/MS同时检测水产品中麻醉剂及其代谢物残留

Simultaneous Determination of Anesthetics and Metabolites in Aquatic Products by UPLC-MS/MS Coupled with Pass-through Solid Phase Extraction

目的 建立通过式固相萃取净化-超高效液相色谱串联质谱技术同时检测水产品中多种麻醉剂及其代谢物的方法。方法 样品均质后,使用80%乙腈水溶液提取,使用ProElt PLS-A通过式固相萃取柱进行通过式净化。以0.1%甲酸水和0.1%甲酸乙腈为流动相按比例进行梯度洗脱,使用正离子模式。采用质谱多重反应监测模式,空白基质绘制标准曲线定量。结果 14种麻醉剂及其代谢物中,麻醉剂在1~50μg·L^(–1)内呈现良好的线性关系,代谢物在10~500μg·L^(–1)内均呈现良好的线性关系,相关系数均>0.99,其中麻醉剂药物检出限为0.5μg·kg^(–1),代谢物检出限为5μg·kg^(–1),麻醉剂药物定量下限为1μg·kg^(–1),代谢物定量下限为10μg·kg^(–1)。方法高、中、低浓度加样回收率为62.48%~116.5%,RSDs均<10%。结论该方法操作流程简便,结果准确可靠,可用于水产品中麻醉剂及其代谢物的检测。

OBJECTIVE To establish an analytical method for the simultaneous determination of multiple anesthetics and their metabolites in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction purification.METHODS After homogenization,the samples were extracted by 80%acetonitrile aqueous solution,and purified by ProElt PLS-A pass-through solid phase extraction column.The extract was determined by positive ion mode with mobile phase of 0.1%formic acid water and 0.1%formic acid acetonitrile in the separation by programmed gradient.Multiple reaction monitoring mode was used to draw standard curves with the matrix-matched method.RESULTS The calibration curves of the 14 anesthetics showed good linearity in the concentration range of 1−50μg·L^(–1) and their metabolites showed good linearity in the concentration range of 10−500μg·L^(–1),with the correlation coefficients>0.99.The limits of detection were 0.5μg·kg^(–1) in anesthetics and 5μg·kg^(–1) in their metabolites.The lower limits of quantification were 1μg·kg^(–1) in anesthetics and 10μg·kg^(–1) in their metabolites.The recoveries at high,medium and low concentrations ranged from 62.48%to 116.5%with RSDs<10%.CONCLUSION The method is simple and can be used for the accurate detection of anesthetics and their metabolites in aquatic products with high reliabilities.