摘要
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.
出处
《烟草科技》
EI
CAS
北大核心
2012年第11期45-50,共6页
Tobacco Science & Technology
基金
国家烟草专卖局标准项目"烟草及烟草制品农残限量要求"(项目编号502011AB0450)
中国烟草总公司郑州烟草研究院院长基金项目(512012CA0080)