加速溶剂萃取-气相色谱-串联质谱法测定罗非鱼中拟除虫菊酯类农药残留量  

GC-MS/MS Determination of Residual Amount of Pyrethroid Pesticides in Tilapia with Accelerated Solvent Extraction

作　　者：朱晓华[1,2,3] 王凯[1,2,3] 高钰一[1,2,3] 朱超[4] 吴光红[1,2,3] 

机构地区：[1]江苏省水产质量检测中心,南京210017 [2]农业部渔业产品质量监督检验测试中心(南京),南京210017 [3]江苏省淡水水产研究所,南京210017 [4]中国药科大学药学院,南京210009

出　　处：《理化检验（化学分册）》2013年第1期39-43,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：江苏省科技公共服务平台(BM2008158);江苏省科技支撑计划-社会发展项目(BE2011813)

摘　　要：提出了气相色谱-串联质谱法测定罗非鱼中7种拟除虫菊酯类农药(联苯菊酯、甲氰菊酯、三氟氯氰菊酯、氯菊酯、氯氰菊酯、氰戊菊酯和溴氰菊酯)残留量的方法。样品以环己烷-乙酸乙酯(1+1)混合液为萃取剂,经加速溶剂萃取仪提取后,经Florisil固相萃取小柱净化后,用丙酮-正己烷(1+9)混合液淋洗,洗脱液于45℃水浴氮吹近干后用正己烷定容至1 mL,通过TR-5MS毛细管色谱柱分离,采用电子轰击离子源选择反应监测模式进行质谱测定。7种拟除虫菊酯类农药的检出限(3S/N)在0.20～2.1μg·kg^(-1)之间。以空白罗非鱼样品为基体,加入标准溶液进行回收试验,测得回收率在57.9%～107%之间,测定值的相对标准偏差(n=6)均小于12.0%。GC-MS/MS was applied to the determination of residual amounts of 7 pyrethroid pesticides （i. e , bifenthrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, fenvalerate and deltamethrin） in tilapi＆ The sample was extracted with a mixture of cyclohexane-ethyl acetate （1＋1） by accelerated solvent extraction, and the extract was purified on Florisil solid phase extraction （SPE） column. The 7 pyrethroid pesticides were eluted from the SPE column with a mixture of acetone-n-hexane （1 ＋ 9） and the eluate was evaporated to near dryness by N2-blowing on a water bath at 45 ℃. The residue obtained was dissolved and made up to 1.0 mL with n-hexane, which was used for GC-MS/MS analysis. TR- 5MS capillary chromatographic column was used for separation, and the selected reaction monitoring （SRM） with electron impact ionization source was adopted in MS. Values of detection limit of 7 pyrethroid pesticides were found in the rmage of 0. 20--2. 1 μg ·kg^-1. On the base of blank sample of tilapia, test for recovery was made by standard addition method, values of recovery found were in the range of 57. 9%--107%, with RSD＇s （n=6） less than 12. 0%.

关 键 词：气相色谱-串联质谱法 加速溶剂萃取 罗非鱼 拟除虫菊酯类农药 

分 类 号：O657.63[理学—分析化学]