超高效液相色谱-串联质谱法测定水产品中8种苯二氮卓类镇静药物残留

Determination of drug residues of 8 kinds of benzodiazepine in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  水产品  药物残留  苯二氮卓  镇静剂  超高效液相色谱-串联质谱法

英文关键词:aquatic products  drug residues  benzodiazepines  sedativetetracyclines  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定水产品中地西泮、奥沙西泮、咪达唑仑、氯硝西泮、劳拉西泮、三唑仑、阿普唑仑和硝西泮8种苯二氮卓类药物残留的方法。方法 样品经含有0.2%甲酸的80%乙腈水溶液提取, 采用Waters PRIME HLB固相萃取柱净化, 水浴氮吹浓缩后用于检测。样液通过C18色谱柱分离, 以0.1%甲酸水溶液与甲醇流动相经系统梯度洗脱后, 于UPLC-MS/MS选择电喷雾正离子多反应监测模式下分析测定, 基质添加标准曲线, 外标法定量。结果 8种苯二氮卓类药物标准曲线相关系数均大于0.999, 检出限为0.064~0.226 μg/kg, 方法的回收率为70.4%~107.0%, 相对标准偏差为2.1%~10.2%。结论 本方法快速、准确, 可应用于水产品中多种苯二氮卓类镇静药物残留的快速准确筛查和检测。

英文摘要:

      Objective To establish a method for the determination of 8 kinds of benzodiazepines residues, including diazepam, oxazepam, midazolam, clonazepam, lorazepam, triazolam, alprazolam and nitrazepam in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS). Methods The sample was extracted by 80% acetonitrile aqueous solution containing 0.2% formic acid, purified by Waters PRIME HLB solid phase extraction column, concentrated by nitrogen blowing in water bath. The residue contents were separated by C18 chromatographic column, eluted by 0.1% formic acid aqueous solution-methanol mobile phase systems, and analyzed by electrospray ion source in positive ion multi-reaction monitoring mode. The quantitative information was obtained by matrix-added calibration with external standard. Results The correlation coefficient of calibration curves of 8 kinds of benzodiazepines residues were above 0.999. The limits of detection were 0.064–0.226 μg/kg, the recovery rates of the method were 70.4%–107.0%, and the relative standard deviations were 2.1%–10.2%. Conclusion The method is rapid, simple and accurate, and it is suitable for the determination of benzodiazepine sedative drug residues in aquatic products.