通过式固相萃取-超高效液相色谱-串联质谱法测定水产品中地西泮

Determination of diazepam in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction

建立了通过式固相萃取-超高效液相色谱-串联质谱测定水产品中地西泮残留量的分析方法。样品用乙腈直接提取,经Prime HLB通过式固相萃取柱(60 mg/3 mL)净化,以Acquity UPLC BEH C 18(100 mm×2.1 mm,1.7μm)为色谱柱,甲醇-0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱。在多反应监测(MRM)、正离子电离模式下检测,采用基质匹配标准曲线外标法进行定量分析。结果显示:在0.1~10 ng/mL范围内,地西泮线性关系良好(r 2>0.99)。在1.5、3.0和15.0μg/kg 3个加标水平下,地西泮的加标回收率为88.2%~101.1%,日间和日内精密度(RSD)均在10%以下。该法简便快速,灵敏度高,可用于水产品中地西泮的准确测定。

A method was developed for the determination of diazepam in aquatic products by pass-through solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The analyte was extracted with acetonitrile directly and purified on a Prime HLB solid phase extraction column(60 mg/3 mL).The separation was performed on an Acquity UPLC BEH C 18 column(100 mm×2.1 mm,1.7μm)using methanol-0.1%(v/v)formic acid aqueous solution as the mobile phase in gradient elution mode.Qualitative analysis was performed in the multiple reaction monitoring(MRM)mode.The analyte was quantified by matrix-matched external standard curves.The results showed good linear relationship in the range of 0.1-10 ng/mL,and the correlation coefficient(r 2)was greater than 0.99.The spiked recoveries of diazepam were 88.2%-101.1%at the spiked levels of 1.5,3.0 and 15.0μg/kg,and both the intra-and inter-day precisions were less than 10%.The developed method is simple,rapid and accurate,and it can meet the requirements for diazepam determination in aquatic product samples.