中空纤维膜液相微萃取-气相色谱-质谱法测定水样中拟除虫菊酯类农药
GC-MS Determination of Pyrethroid Pesticides in Water Samples with Hollow Fibrous Membranes-Liquid Phase Micro-extraction
摘 要
提出了气相色谱-质谱法测定水中的拟除虫菊酯类农药胺菊酯、甲氰菊酯、氯菊酯的方法.样品采用中空纤维膜液相微萃取法萃取,以甲苯为萃取剂,于35 ℃在600 r·min-1转速下萃取20 min.在优化的试验条件下,胺菊酯、甲氰菊酯和氯菊酯的富集倍数分别为292,63,76倍.3种拟除虫菊酯类农药的响应信号值与其质量浓度在一定的线性范围呈线性关系,检出限(3S/N)均小于0.5 μg·L-1.方法用于分析实际水样,回收率为92.4%~98.0%,相对标准偏差(n=6)为1.9%~8.6%.
中空纤维膜
液相微萃取
拟除虫菊酯
水样
GC-MS
Hollow fibrous membranes
Liquid phase micro-extraction
Pyrethroid pesticides
Water samples
Abstract
GC-MS was used in the determination of pyrethroid pesticides,including tetramethrin,fenpropathrin and permethrin in water samples.The sample was extracted by hollow fibrous membranes-liquid phase micro-extraction method (HFM-LPME) with methylbenzene as extraction solvent.The extraction was carried out under magnetic stirring for 20 min,at the rate of 600 r·min-1 and at the temperature of 35 ℃.Under the optimal extraction conditions,enrichment factors for tetramethrin,fenpropathrin and permethrin obtained were 292,63 and 76,respectively.Linear relationships between values of response signal and mass concentration of the 3 pyrethroid pesticides were obtained in definite ranges,with detection limits (3S/N) less than 0.5 μg·L-1.Tests for recovery and precision were made and values of recovery and RSD′s (n=6) found were in the ranges of 92.4%-98.0% and 1.9%-8.6% respectively.
中图分类号 O657.63
所属栏目 试验与研究
基金项目 苏州市社会发展基金项目(SS0734)
收稿日期 2008/12/27
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备注李刚(1982-),男,河北泊头人,硕士研究生,研究方向为环境监测.
引用该论文: LI Gang,ZHANG Zhan-en. GC-MS Determination of Pyrethroid Pesticides in Water Samples with Hollow Fibrous Membranes-Liquid Phase Micro-extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(3): 227～229
李刚,张占恩. 中空纤维膜液相微萃取-气相色谱-质谱法测定水样中拟除虫菊酯类农药[J]. 理化检验－化学分册, 2010, 46(3): 227～229
被引情况:
【1】闻亚,徐心怡,聂晶,李祖光,吴先伟,邓丰涛, "超声辅助-表面活性剂增强乳化微萃取-气相色谱-质谱法测定薄荷芳香水中的挥发性成分",理化检验－化学分册 50, 1065-1069(2014)
【2】耿新华,李晓,刘汝锋,温必花,谢连心, "顶空单滴液相微萃取-气相色谱法测定水中苯胺类化合物",理化检验－化学分册 50, 202-205(2014)
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参考文献
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【3】李拥军,黄志强,张莹.茶叶中多种拟除虫菊酯类农药残留量的气相色谱-质谱测定[J].分析化学,2002,30(7):865-868．
【4】罗明标,刘维,李伯平.多孔中空纤维液相微萃取技术的研究进展[J].分析化学,2007,35(7):1071-1077．
【5】RATOLA N,ALVES A.Hollow-fibre liquid-phase microextraction: A simple and fast cleanup step used for PAHs determination in pine needles[J].Anal Chim Acta,2008,618(1):70-78．
【6】付新梅,戴树桂,傅学起.液膜微萃取技术在环境样品前处理中的应用[J].分析测试学报,2006,25(2):126-131．
【7】张月琴,吴淑琪.水中有机污染物前处理方法进展[J].分析测试学报,2003,22(3):107-109．
【8】LEE J Y,LEE H K.Environmental and bioanalytical applications of hollow fiber membrane liquid-phase microextraction: A review[J].Anal Chim Acta,2008,624(2):253-268．
【9】罗三珊,张占恩.水中氯苯类污染物的顶空液相微萃取GC-MS法测定[J].分析测试学报,2007,26(6):817-819．
【10】LI G H,ZHANG L J,ZHANG Z E.Determination of polychlorinated biphenyls in water using dynamic hollow fiber liquid-phase microextraction and gas chromatography-mass spectrometry[J].J Chromatogr A,2008,1204(1):119-122．
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