摘要
目的:探索乙腈和甲苯在不同体积比的混合洗脱液及其洗脱液用量对蔬菜中联苯菊酯和甲氰菊酯在PestiCarb/NH2固相萃取柱(SPE柱)上的洗脱效率,以气相色谱ECD测定。方法:试样用乙腈提取,浓缩后经PestiCarb/NH2SPE柱、乙腈∶甲苯=3∶1混合洗脱液净化,用气相色谱ECD,以OV-1701毛细管柱分离测定。结果:联苯菊酯的最低检出浓度为0.3μg/kg,最低检测定量浓度为0.8μg/kg,相对标准偏差(RSD)为6.1%～3.8%;甲氰菊酯的最低检出浓度为1.0μg/kg,最低检测定量浓度为3.3μg/kg,相对标准偏差(RSD)为6.4%～3.4%。平均回收率均为95%～105%。结论:在该净化条件下,试样经气相色谱ECD测定,联苯菊酯和甲氰菊酯有较好回收率和理想的重复性,适用于该类样品的测定。
Objective：To explore the elution efficiency of bifenthrin and fenpropathrin in vegetables,eluted with miscible liquids of acetonitrile and methylbenzene with different volume ratio and different elution volume,cleaned up by PestiCarb/NH2 solid phase extraction column（SPE column） with gas chromatography（GC）ECD detector.Methods：The sample was extracted with acetonitril.After concentration,the extract was purified by PestiCarb/NH2SPE column and miscible liquids of acetonitrile：methylbenzene=3：1,separated with OV-1701 capillary column and determined by GC ECD.Results：The detectable concentration of bifenthrin by this method was 0.3 μg/kg.The limit of quantification was 0.8 μg/kg.The relative standard deviations（RSDs） were in the range of 6.1%～3.8%.The detectable concentration of fenpropathrin by this method was 1.0 μg/kg.The limit of quantification was 3.3 μg/kg.The RSDs were in the range of 6.4%～3.4%.The average recoveries were in the range of 95%～105%.Conclusion：With the clean-up condition,the method with satisfactory recoveries and repeatability is suitable for determination of bifenthrin and fenpropathrin in vegetables.
出处
《中国卫生检验杂志》
CAS
2011年第8期1867-1869,共3页
Chinese Journal of Health Laboratory Technology
基金
贵州省疾病预防控制中心基金项目(2010-2-8)
关键词
联苯菊酯
甲氰菊酯
固相萃取
气相色谱
Bifenthrin
Fenpropathrin
Solid Phase Extraction
Gas Chromatography
