GC-MS/MS Determination of Residual Amount of Pyrethroid Pesticides in Tilapia with Accelerated Solvent Extraction
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0.20~2.1 μg·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%。
Abstract
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 tilapia. 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 range 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%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 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)
收稿日期 2011/10/22
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联系人作者朱晓华(xhz824@sina.com)
备注朱晓华(1975-),女,江苏无锡人,高级工程师,主要从事药物残留检测与技术研究。
引用该论文: ZHU Xiao-hua,WANG Kai,GAO Yu-yi,ZHU Chao,WU Guang-hong. GC-MS/MS Determination of Residual Amount of Pyrethroid Pesticides in Tilapia with Accelerated Solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(1): 39~43
朱晓华,王凯,高钰一,朱超,吴光红. 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[J]. 理化检验-化学分册, 2013, 49(1): 39~43
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【4】刘占山,廖建平,李旭君,等.拟除虫菊酯类农药用于水田害虫防治探讨及应用前景展望[J].江西农业学报, 2008,20(2):68-71.
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【8】髙钰一,沈美芳,宋红波,等.气相色谱法测定水产品中7种拟除虫菊酯的残留量[J].水产学报, 2009,33(1):132-138.
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【10】陈剑刚,朱克先,张亦庸,等.固相萃取-气相色谱-质谱联用测定水体中拟除虫菊酯残留[J].现代预防医学, 2005,32(6):648-650.
【11】祝金凤,梁颖,刘媛,等.氯氰菊酯和三氟氯氰菊酯酶联免疫检测方法的建立[J].江苏农业学报, 2009,25(2):407-410.
【12】林子俺,龚巧燕,谢增鸿.高效液相色谱测定蔬菜中拟除虫菊酷类农药残留[J].福州大学学报:自然科学版, 2008,36(1):122-125.
【13】李永夫,高华鹏,张健玲,等.超高效液相色谱-串联质谱法测定鳗鱼中呋线威和溴氰菊酯残留[J].分析化学研究报告, 2008,36(6):755-759.
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