用HPLC柱后衍生法分析烟草中氨基甲酸酯类农药残留

Determination of Carbamates Residues in Tobacco by HPLC with Post-column Derivatization

采用反相高效液相色谱法对烟草中涕灭威亚砜、涕灭威砜、灭多威、三羟基克百威、涕灭威、克百威、甲萘威、异丙威等8种氨基甲酸酯类农药同时进行残留分析。样品采用乙腈/水提取,NH2-SPE柱净化,柱后衍生荧光检测器(FLD)测定。8种农药在0.1～1.0 mg/L范围内线性良好,相关系数为0.9951～0.9999,在0.05、0.1、0.5 mg/kg添加水平的平均回收率分别为80.8%～110.6%、84.4%～109.7%和81.6%～112.9%,相对标准偏差分别为3.2%～10.8%、3.8%～11.8%和3.7%～8.5%。各种农药的检出限为0.008～0.01 mg/kg。方法适用于烟草中氨基甲酸酯类农药多残留检测。

Residue analysis of 8 carbamate pesticides in tobacco by reversed-phase high performance： liquid chromatography was assessed. Residues were first extracted with acetonitrile and water, filtrated with NH2-SPE columns, and then determined by post-column derivatization with fluorescence detector. The proposed methods showed a good linearity between analytical signal in the range of 0.1-1.0 mg/L with linear correlation coefficients of 0.9951-0.9999 and limits of detection of 0.008-0.01 mg/kg. The average recoveries obtained from samples spiked with standards at concentration level 0.05, 0.1 and 0.5 mg/kg were in the range of 80.8%-110.6%, 84.4%-109.7%to/81.6%-112.9%, respectively, with relative standard deviations of 3.2%-10.8%, 3.8%-11.8%to N 3.7%-8.5%. Asatisfactory result was obtained in the simultaneous determination of carbamate pesticide residues in tobacco.