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/m L,定量限范围为0.44~2.63 ng/m L,在1.0~25.0μg/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。
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 sulfofunctionalized 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/m L, 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.
出处
《食品安全质量检测学报》
CAS
2015年第9期3677-3683,共7页
Journal of Food Safety and Quality
基金
江西省质量技术监督局重大科技项目(GZJK201202)~~
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
sulfo-functionalized magnetic beads
magnetic solid phase extraction
liquid chromatographytandem mass spectrometry
benzodiazepines
beef
