超高效液相色谱-串联质谱法同时快速测定卷烟烟丝中的6种生物碱

Rapid Determination of Six Alkaloids in Tobacco by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了超高效液相色谱-串联质谱（UPLC-MS/MS）同时快速测定烟草中6种生物碱的方法。对样品前处理条件和仪器分离条件进行了优化,样品经去离子水超声提取后,于UPLC BEH C18色谱柱上分离,在多反应监测模式下采用同位素内标法定量以排除基质效应。结果表明,6种生物碱的线性范围为0.1~8 000μg/L,样品的加标回收率为87%~115%,相对标准偏差为1.9%~9.7%,检出限为50~1 250μg/kg。该方法前处理简单,分析时间短,具有良好的灵敏度和准确性,适用于烟草中该6种生物碱的测定。

An ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS） method was developed for the rapid determination of six alkaloids in tobacco.The sample pretreatment and parameter separation conditions were optimized.The samples were extracted with deionized water,and separated on UPLC BEH C18 chromatographic column.The mass spectrometer with electrospray in positive ionization was operated under multiple reaction monitoring（MRM） mode.Six alkaloids was quantified by the isotope internal standard method to avoid matrix effects.The result indicated that,the calibration curves of six alkaloids were in the range of 0.1-8 000 μg/L.The spiked recoveries ranged from 87% to 115% with relative standard deviations of 1.9%-9.7%.The limits of detection ranged from 50 μg/kg to 1 250 μg/kg.This method was simple,accurate and reproducible,and could be used for the rapid analysis of six alkaloids in batches of tobacco samples.