液相色谱-大气压化学电离离子阱质谱法测定烟草中的游离茄尼醇

用液相色谱/大气压化学电离离子阱质谱建立了一种分析烟草中游离茄尼醇的方法。烟草样品用甲醇振荡提取30 min,在分析前无需进行其它前处理。在1.8μm快速分离C18色谱短柱上用V(甲醇)∶V(异丙醇)=85∶15等梯度洗脱实现了茄尼醇的快速分离。用不带碰撞能量的二级质谱全扫描选择监测离子m/z 613.6进行定量,检出限为0.4μg/L,RSD为1.1%,两种添加量的回收率分别为97%和99%。方法应用于不同烟草和烟草制品样品的检测分析。

Determination of free solanesol in tobacco by liquid chromatography and atmospheric pressure chemical ionization ion trap mass spectrometry

A rapid, sensitive and reliable liquid chromatography/atmospheric pressure chemical ionization-ion trap mass spectrometric (LC/APCI-ITMS) method was developed for the determination of free solanesol in tobacco. Solane-sol was extracted from tobacco with methanol by shaking extraction in 30 min and no further workup procedure was needed before analysis. Solanesol was separated by using a short 1.8 pm rapid separation C18 column with methanol-isopropanol (85%: 15%, V/V) in the isocratic gradient to achieve a fast chromatographic analysis. In the positive APCI mode, the ion mlz 613.6 selected for quantitation was sensitively detected in the two-stage mass (MS~2) full scan mode without employing collision energy. The limit of detection (LOD) was 0.4 /ug/L. The precision was 1.1%. The recoveries were 97% and 99% for two different spiked levels. The established method has been successfully applied to analyze the samples of various tobacco and tobacco products.