熬制汤料中巴豆苷测定的方法学研究  

Methodology research on crotonoside determination in the stewed soup

作　　者：李帮锐[1,2] 冯家力[1] 曾栋[1] 王一红[1] 刘先军[1] 陈东洋[1] 

机构地区：[1]湖南省疾病预防控制中心,湖南长沙410005 [2]湖南大学化学化工学院,湖南长沙410082

出　　处：《中国卫生检验杂志》2015年第1期8-10,17,共4页Chinese Journal of Health Laboratory Technology

基　　金：湖南省科技厅科技计划项目(2013SK3226)

摘　　要：目的开展熬制汤料中巴豆苷测定的方法学研究。方法采用乙腈提取、氯化钠分层的预处理方法,液相色谱与质谱、光谱联用法测定巴豆苷。通过优化色谱条件,更换检测器排除鸟苷的干扰。结果采用乙腈提取与氯化钠分层的预处理办法,样本提取时间短、效率高、操作简单,并且净化效果好;液相色谱与质谱、光谱联用法测定巴豆苷的抗干扰能力强,定性、定量准确。该方法在1 ng/ml^1 000 ng/ml,质谱测定的线性关系良好,线性相关系数为0.9985;在浓度为1μg/ml^100μg/ml时,紫外-可见光谱测定的线性关系良好,线性相关系数为0.9993。巴豆苷质谱测定的检出限为0.1 ng/g,紫外-可见光谱测定的检出限为0.1μg/g。结论乙腈提取,氯化钠分层预处理,结合液相色谱与质谱、光谱联用法测定熬制汤料中的巴豆苷,方法简单可靠、耗时少、能有效去除干扰,非常适合巴豆中毒事件中的应急检测。Objective To research methods for determination of crotonoside in the stewed soup. Methods The method of pretreatment include ultrasonic extraction using acetonitrile and solution lamination by adding sodium chloride. Then the samples were separated by reverse phase liquid chromatography and detected by mass spectrometer and UV- Visible Spectrometer. The interference was eliminated by optimizing the chromatographic conditions and replace the detector. Results Dealing with samples was very simple,high efficient and easy operating and the purification effect was excellent. The liquid chromatography-mass spectrometer / UV- Visible Spectrometer method had strong anti- interference ability and was accurate on qualification and quantification,this method had good linear from 1 ng / ml to 1 000 ng / ml with correlation coefficient 0. 9985 for mass spectrometer; The curve of peak area with concentration had good linear from 1 μg / ml to 100 μg / ml with correlation coefficient 0. 9993 for UV- Visible Spectrometer. The detection limits of crotonoside were 0. 1 ng / g and 0. 1 μg / g with mass spectrometer and UV- Visible Spectrometer respectively. Conclusion The union determination method is simple,reliable,time- saving and effective to remove interference,which was very suitable to the emergency determination of food poisoning samples.

关 键 词：巴豆苷 液相色谱与质谱、光谱联用 熬制汤料 

分 类 号：O657.63[理学—分析化学]