磁固相萃取-液相色谱-串联质谱法检测牛肉中 4种苯二氮卓类药物的残留

Magnetic solid phase extraction-liquid chromatography-tandem mass spec-trometry for the determination of 4 kinds of benzodiazepines residues in beef

中文关键词:  磺酸化磁珠  磁固相萃取法  液相色谱-串联质谱法  苯二氮卓类物质  牛肉

英文关键词:sulfo-functionalized magnetic beads  magnetic solid phase extraction  liquid chromatography- tandem mass spectrometry  benzodiazepines  beef

中文摘要:

      目的 以磺酸化磁珠作为磁固相萃取吸附剂, 建立了磁固相萃取-液相色谱-串联质谱法联用分析苯二氮卓类药物的新方法。方法 萃取和吸附条件优化后, 地西泮、奥沙西泮、三唑仑和氯氮卓4种苯二氮卓类药物经磺酸化磁珠富集后, 采用液相色谱-串联质谱的多反应方法检测牛肉样品中4种苯二氮卓类药物的残留。结果 4种苯二氮卓类药物的方法回收率为49.6%~83.5%, 相对标准偏差(RSD, n=5)为2.2%~16.0%, 检出限范围为0.13~0.79 ng/mL, 定量限范围为0.44~2.63 ng/mL, 在1.0~25.0 μg/L 范围内线性相关系数为0.9992~0.9999。结论 该法具有操作简便、灵敏度高、测定准确等特点, 适用于牛肉中苯二氮卓类物质的残留检测。

英文摘要:

      Objective To establish a novel method for the determination of 4 kinds of benzodiazepines (BZDs, chlordiazepoxide, diazepam, oxazepam, and triazolam) by magnetic solid phase extraction (MSPE)-liquid chromatography-tandem mass spectrometry (LC-MS/MS), based on the sulfo-functionalized magnetic beads. Methods After optimization of the extraction/desorption conditions, 4 BZDs were extracted with sulfo- functionalized magnetic beads, and detected by liquid chromatography-tandem mass spectrometry in multiple-reaction monitoring mode. Results The average recoveries of 4 benzodiazepines were 49.6%~83.5%, the relative standard deviation (RSD) of this method was between 2.2%~16.0%. The limits of detection (LOD) and limits of quantification (LOQ) of 4 kinds of benzodiazepines were in the range of 0.13~0.79 and 0.44~2.63 ng/mL, respectively. This method had a good linearity in the range of 1.0~25.0 μg/L between the peak areas and concentration in 4 kinds of benzodiazepines with the correlation coefficients were 0. 9992~0.999. Conclusion The method was fast, accurate and sensitive, which could be applied in the routine assay on benzodiazepines in beef.