气相色谱-质谱法测定烟叶和土壤中丁硫克百威及其代谢产物的残留  

Determination of carbosulfan and its metabolites residues in tobacco leaf and soil by gas chromatography-mass spectrometry

作　　者：罗俊凯[1] 龚道新[1,2] 丁春霞[1,3] 黄雪[1] 杨丽华[1] 张佳仕[1] 

机构地区：[1]湖南农业大学资源环境学院,长沙410128 [2]湖南农业大学农业环境保护研究所,长沙410128 [3]湖南农业大学理学院,长沙410128

出　　处：《农药学学报》2014年第1期66-71,共6页Chinese Journal of Pesticide Science

基　　金：湖南省烟草及其产品中农药残留污染与控制技术研究(湖南省科技厅06FJ4266)

摘　　要：建立了气相色谱．质谱法同时检测烟叶和土壤中丁硫克百威及其代谢产物（克百威和3．羟基克百威）残留量的分析方法。土壤样品用丙酮-石油醚[y（丙酮）：V（石油醚）=1：4]混合溶液提取，无需净化；鲜烟叶样品用丙酮-乙腈[V（丙酮）-V（乙腈）=1：9]混合溶液提取；烤后烟叶用乙腈提取。鲜烟叶和烤后烟叶提取液经旋转蒸发浓缩后，用弗罗里硅土柱净化。结果表明：在0．05-1mg／kg添加水平下，丁硫克百威及其代谢产物的平均回收率在74％～99％之间，相对标准偏差（RSD，n=5）在1．5％～9．2％之间。该方法的前处理相对于萃取过程较简单，其准确度、精密度和灵敏度均符合农药残留分析与检测的技术要求，适合于丁硫克百威及其代谢产物在烟叶和土壤中的残留分析与检测。An analytical method was developed for the simultaneous determination of carbosulfan and its metabolites （carbofuran and 3-hydroxycarbofuran ） residues in tobacco leaf and soil by gas chromatography-mass spectrometry （GC-MS）. Soil samples were extracted with acetone-petroleum ether [ V（acetone）： V（petroleum ether） = 1：4]; Fresh tobacco samples and flue-cured tobacco leaf samples were extracted with acetone-acetonitrile [ V（acetone） ： V（acetonitrile） = 1： 9 ] and acetonitrile, respectively. The extracts were concentrated by rotary evaporation, and followed by cleanup on Florisil column. With fortified concentration range of 0. 05 - 1 mg,/kg, the average recoveries ranged from 74% to 99%, and with relative standard deviation （RSD, n =5） of 1.5% -9.2%. The pre-treatment step of the current method is relatively simple, and the accuracy, precision and sensitivity of themethod meet with the technical requirements for the analysis and detection of pesticide residues. The method is suitable for analysis and detection of carbosulfan and its major metabolites in tobacco leaf and soil.

关 键 词：气相色谱-质谱法 烟叶 土壤 丁硫克百威 代谢产物 残留 

分 类 号：O657.7[理学—分析化学] S482.4[理学—化学]