凝胶渗透色谱-高效液相色谱-串联质谱法同时测定烟草中3种抑芽剂残留

建立了用凝胶渗透色谱净化-液相色谱-串联质谱分析烟草中3种抑芽剂残留的方法。卷烟中的待测抑芽剂组分用V(乙酸乙酯)∶V(环己烷)=1∶1超声提取后通过凝胶渗透色谱净化;凝胶色谱柱为Biobeads S-X3玻璃柱(50 g,400 mm×25 mm),流动相为V(乙酸乙酯)∶V(环己烷)=1∶1溶液,流速5 mL/min;收集第10~25 min流出的液体用液相色谱色谱-三重四极杆串联质谱仪测定。在0.5~100 ng/mL的质量浓度范围内,各种抑芽剂标准溶液的线性相关系数均大于0.99。在样品中添加3种抑芽剂(添加水平为5,20,100μg/kg)的混合标准溶液,平均回收率在86.2%~108.4%之间,3种抑芽剂的RSD在1.1%~7.5%之间;方法的检测限在0.01~0.06μg/kg之间。

Determination of 3 kinds of suckercide residues in tobacco by GPC and HPLC-MS/MS

A new method using gel permeation chromatographic (GPC) cleanup followed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) has been established for quantitative determination of Maleic hydrazide, Prowl and butralin residues in tobacco. In the method, the samples were extracted ultrasonically with ethyl acetate-cyclohexane (1∶1, V/V), and 5 mL of extract was injected into a 400 mm×25 mm S-X3 GPC column, with ethyl acetate-cyclohexane (1∶1, V/V) as the mobile phase at a flow rate of 5 mL/min. The 10～25 min fraction was collected for subsequent analysis. The portions collected from GPC were dissolved in methanol after taking the extract to dryness with nitrogen gas. The correlation coefficient of each suckercides was r~2>0.99. The relative standard derivations (RSD) of suckercides were between 1.1% and 7.5%, the recoveries fell within 86.2%～108.4%, and the limits of detection for the method were 0.01～0.06 μg/kg.