气相色谱法测定荔枝中7种拟除虫菊酯类农药残留量  

GC Determination of Residual Amounts of 7 Pyrethroid Pesticides in Litchi

作　　者：黄惠玲[1] 何翠花[1] 王玉健[1] 黄海民[1] 黄杰英 柯慧贤[2] 

机构地区：[1]海南出入境检验检疫局技术中心,海口570311 [2]海南大学食品学院,海口570228

出　　处：《理化检验（化学分册）》2017年第2期130-133,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：海南省重点科技计划项目(ZDXM20120039;ZDXM20120040);海南省自然科学基金(212018);国家质检总局科技计划项目(2013IK153)

摘　　要：采用气相色谱法测定荔枝中联苯菊酯、甲氰菊酯、氯氟氰菊酯、氟氯氰菊酯、氯氰菊酯、氰戊菊酯和溴氰菊酯等7种拟除虫菊酯类农药的残留量。荔枝样品用丙酮-正己烷(1+1)混合液提取,所得提取液用活性炭柱和中性氧化铝柱的串联柱净化,用DB-35毛细管色谱柱分离,电子捕获检测器检测。7种拟除虫菊酯类农药的质量浓度均在0.05~0.8mg·L^(-1)内与其峰面积呈线性关系,方法的检出限(3S/N)在0.005~0.01mg·kg^(-1)之间。在0.05,0.1,0.2mg·kg^(-1)等3个浓度水平进行加标回收试验和精密度试验,回收率在81.0%~104%之间,测定值的相对标准偏差(n=6)在1.7%~5.1%之间。采用此法测定了荔枝样品中联苯菊酯的含量,所得测定值与行业标准方法测定结果相符。GC was applied to the determination of residual amounts of 7 pyrethroid pesticides, i. e. bifenthrin, fenpropathrin, cyhalothrin, cyfluthrin, cypermethrin, fenvalerate and deltamethrin in litchi. The litchi sample was extracted with a mixture of acetone-n-hexane （1＋1）, and the extract was purified with activated carbon column and neutral alumina column in series. The analytes were separated on DB-35 capillary column and detected hy ECD. Linear relationships between values of peak area and mass concentration of the 7 pesticides were kept in the same range of 0. 05-0. 8 mg · L^-1 , with detection limits （3S/N） in the range of 0. 005--0. 01 mg · kg^-1. Tests for recovery and precision were made by standard addition method at 3 concentration levels of 0.05, 0. 1, 0. 2 mg · kg^-1 , giving values of recovery and RSD＇s （n=6） in the ranges of 81.0%-104% and 1.70%-5. 1% respectively. The proposed method was used to determine bifenthrin in litchi samples, giving results in consistency with values given by the professional standard method.

关 键 词：气相色谱法 拟除虫菊酯类农药 荔枝 

分 类 号：O657.7[理学—分析化学]