固相萃取-超高效液相色谱串联质谱法同时测定保健品中5种生物碱

Simultaneous determination of five alkaloids in health products by SPME-UPLC-MS/MS

该研究建立了一种高效、灵敏的同时测定保健品中可能违法添加的5种有毒生物碱(烟碱、毛果芸香碱、茶碱、毒扁豆碱、阿托品)的方法。试样经0.1%甲酸水-乙腈(3∶1,V/V)混合溶剂提取,Cleanert PEP固相萃取柱净化,采用超高效液相色谱-串联质谱联用(UPLC- MS/MS)技术,用Waters ACQUITY HSS T3色谱柱分离后在多反应监测(MRM)模式下进行定性定量分析。结果表明,5种生物碱的线性范围为0.2~20.0 μg/L,相关系数R^2≥0.999 0;方法检出限在0.6~0.8 μg/kg;平均加标回收率为87.9%~99.1%,相对标准偏差范围在1.2%~5.7%。该方法操作简单、定量准确,可为保健品的质量安全监管提供技术支持。

An efficient and sensitive method for the simultaneous determination of five alkaloids (nicotine, pilocarpine, theophylline, physostigmine, atropine) added illegally in health products was established. The samples were extracted with 0.1% formic acid-acetonitrile mixed solvent, and cleaned up by Cleanert PEP solid phase extraction column. After separated by Waters ACQUITY HSS T3 chromatographic column, these compounds were qualitatively and quantitatively analyzed in the multiple reaction monitoring (MRM) mode by UPLC-MS/MS. The results showed that the linear ranges of five alkaloids were 0.2-20.0 μg/L and the correlation coefficients R^2 were higher than 0.999 0. The limits of detection for five alkaloids were in the range of 0.6-0.8 μg/kg, the average adding standard recoveries were in the range of 87.9%-99.1% with relative standard deviations of 1.2%-5.7%. The method was simple and accurate, which could provide technical support for the quality and safety supervision of health products.