固相萃取－气相色谱法测定小麦粉中六六六和滴滴涕残留量
Determination of BHC and DDT Pesticide Residues in Wheat Flour by Solid-phase Extraction and Capillary Gas Chromatography
梁瑞 1段兰萍 1赵静 1吴旭妍 1廖若宇1
作者信息
- 1. 宁夏粮油产品质量检测中心，宁夏银川750002
- 折叠
摘要
[目的]建立小麦粉中六六六和滴滴涕农药残留量的固相萃取－气相色谱分析方法。[方法]以乙腈为提取剂，超声提取，采用CarbonNH2固相萃取柱净化，用乙腈－甲苯（3＋1，V／V）作为洗脱液，经HP－1毛细管色谱柱分离后使用电子捕获检测器（ECD）测定。[结果]六六六和滴滴涕农药的质量浓度为0．005～0．400μg／mL时线性良好，相关系数为0．9986～0．9995。在0．05、0．10、0．20 mg／kg 3个添加水平下，六六六和滴滴涕的加标回收率在80．21％～113．41％，相对标准偏差在1．30％～4．33％（n＝6），检出限为0．10～1．51μg／kg。[结论]该方法具有样品前处理操作简单、灵敏度高、试剂用量少、重现性好等优点，适用于小麦粉中六六六、滴滴涕的定性定量分析。
Abstract
Objective] A capillary gas chromatography method was developed for determination of BHC and DDT pesticide residues in wheat flour.[ Method] The pesticide residues in the samples were extracted by ultrasonic assisting oscillation and using acetonitrile as extraction agent . The extract solution was purified by Carbon NH2 Cartridges and eluted with the mixture of acetonitrile-toluene (3+1, V/V) .Finally, the target components were determined using electron capture detector (ECD) after separated from each other through HP-1 capillary column.[Result] The calibration curves were linear in the range of 0.005-0.400 μg/mL with the correlations coefficients of 0.998 6-0.999 5.The recoveries for BHC and DDT in three added levels were in the range of 80.21%-113.41%.The relative standard deviations were 1.30%-4.33%(n=6).The limits of detection (LODs) were in the range of 0.10-1.51μg/kg.[Conclusion] The method is simple, sensitive, less reagent and reproducible, and it is suitable for quantitative and qualitative analysis of BHC and DDT in wheat flour .
关键词
六六六/滴滴涕/固相萃取/毛细管气相色谱法/小麦粉Key words
BHC/DDT/Solid-phase extraction/Capillary gas chromatography/Wheat flour引用本文复制引用
出版年
2016
国家科技期刊平台
NSTL
维普
万方数据