LC-MS/MS同时检测烟草中的6种杀菌剂

Simultaneous Determination of 6 Antiseptics in Tobacco with LC-MS/MS Method

为测定烟草中的杀菌剂残留量，利用液相色谱-串联质谱（LC—MS／MS）建立了一种同时检测烟草中6种杀菌剂的方法：烟草样品提取液经处理后，在AtlantisdC18柱上以乙腈-水（含0．1％甲酸）为流动相进行分离，用LC—MS／Ms在多反应监测（MRM）模式下测定，内标法定量。采用该方法测定了145个国内外烟草样品中6种杀菌剂农药的残留量。结果表明：①6种杀菌剂线性范围是5～200ng／mL，线性关系良好限。〉0．999），平均回收率为85．3％～118．8％，相对标准偏差（RSD）小于7．7％，定量限在0．007～0．033mg／kg之间。②所测样品中，有52个烟叶和30个卷烟样品中未检出任何杀菌剂农药，分别占所选烟叶和卷烟样品数的52％和66．7％；在6种杀菌剂农药中，除苯茵灵未检出外，其他5种农药均有检出。该方法适用于烟草及烟草制品中6种杀菌剂残留的快速检测。

A method basing on high performance liquid chromatography-tandem mass spectrometry （LC-MS/ MS） was developed for determining the antiseptic residues in tobacco. The analytes extracted from tobacco samples were separated on C18 column （150 mm × 2.1 mm × 3 μm）using acetonitrile-water （containing 0.1% formic acid）as mobile phase. The antiseptics were determined by a tandem mass spectrometer with internal standard under multiple reaction monitoring （MRM）mode. The 145 domestic and imported tobacco samples were determined with this method. The results showed that： 1）The linear range was 5-200 ng/mL （R2〉0.999）. The average recoveries ranged from 85.3% to 118.8% with the relative standard deviations （RSD） less than 7.7%. 2）No antiseptic residue was detected in 52 tobacco samples and 30 cigarette samples, which accounted for about 52% of all leave samples and 66.7% of all cigarette samples; all the mentioned antiseptics, except benomyl, were detectable in samples. This method was suitable for the fast determination of the residues of the 6 antiseptics in tobacco and tobacco products.