分散固相萃取-气相色谱-质谱法测定地表水中的3种拟除虫菊酯含量
SPE-GC-MS Determination of 3 Pyrethroids in Surface Water
摘 要
采用分散固相萃取-气相色谱-质谱法测定地表水中的3种拟除虫菊酯。以HC-C18萃取剂为固相萃取填料,以二氯甲烷为洗脱剂对水样进行分散固相萃取。萃取液在HP-5MS石英毛细管柱上分离,质谱中采用电子轰击离子源和选择离子监测模式。在最优条件下,3种拟除虫菊酯的质量浓度在0.05~10.0 μg·L-1范围内呈线性,检出限(3S/N)在0.001~0.005 μg·L-1之间,方法用于实际水样的分析,加标回收率在95.0%~99.8%之间,测定值的相对标准偏差(n=6)在4.3%~11%之间。
分散固相萃取
拟除虫菊酯
地表水
GC-MS
Dispersive solid-phase extraction
Pyrethroids
Surface water
Abstract
GC-MS with dispersive solid phase extraction was applied to the determination of 3 pyrethroids in surface water. The water sample was treated by passing a SPE column packed with HC-C18 as extractant. Dichloromethane was used as eluant. The eluate was separated on HP-5MS quartz capillary column. EI and SIM were adopted in MS. Under optimal conditions. Linearity ranges of the 3 pyrethroids were same between 0.05-10.0 μg·L-1, with detection limits (3S/N) in the range of 0.001-0.005 μg·L-1. The proposed method was used for analysis of surface water samples, and recovery was tested by standard addition method, giving results in the range of 95.0%-99.8%, and RSDs (n=6) found were in the range of 4.3%-11%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201512019
所属栏目 工作简报
基金项目
收稿日期 2014/11/25
修改稿日期
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备注李佳(1990-),女,江苏江阴人,硕士研究生,主要 研究方向为环境监测。
引用该论文: LI Jia,ZHANG Zhan-en,ZHANG Lei. SPE-GC-MS Determination of 3 Pyrethroids in Surface Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(12): 1717～1720
李佳,张占恩,张磊. 分散固相萃取-气相色谱-质谱法测定地表水中的3种拟除虫菊酯含量[J]. 理化检验－化学分册, 2015, 51(12): 1717～1720
被引情况:
【1】李友培, "固相萃取-气相色谱法测定地表水中的痕量苯酚",理化检验－化学分册 52, 1071-1072(2016)
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参考文献
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【2】PINHEIRO A D S, ROCHA G O D, ANDRADE J B D. A SDME/GC-MS methodology for determination of organophosphate and pyrethroid pesticides in water［J］. Microchemical Journal, 2011,99(2):303-308.
【3】WANG Hui, YAN Hong-yuan, QIAO Jin-dong. Miniaturized matrix solid-phase dispersion combined with ultrasound-assisted dispersive liquid-liquid microextraction for the determination of three pyrethroids in soil［J］. Journal of Separayion Science, 2012,35(2):292-298.
【4】GB 5749-2006 生活饮用水卫生标准［S］.
【5】宋伟,林姗姗,孙广大,等.固相萃取-气相色谱-质谱联用同时测定河水和海水中87种农药［J］.色谱, 2012,30(3):318-326.
【6】王松,孙铁珩,孙丽娜,等.畜牧业污水中大环内酯和拟除虫菊酯类驱虫剂物质的LC-MS/MS检测［J］.安全与环境学报, 2009,9(6):94-100.
【7】陈猛,陆婉清,韩燕,等.固相萃取-气相色谱法对河水与海水中36种农药残留的同时测定［J］.分析测试学报, 2009,28(12):1378-1383.
【8】ROCHAABC M J, RIBEIROAD M F T, CRUZEIROB C, et al. Development and validation of a GC-MS method for determination of 39 common pesticides in estuarine water-targeting hazardous amounts in the Douro River estuary［J］. International Journal of Environmental Analytical Chemistry, 2012,92(14):1587-1608.
【9】李红光,李永波,徐清,等.采用不同萃取方法测定饮用水中7种拟除虫菊酯类农药残留量的比较研究［J］.中国卫生检验杂志, 2008,18(12):2557-2558.
【10】CASAS V, LLOMPART M, GARCIA-JARES C, et al. Effects of sample pretreatment and storage conditions in the determination of pyrethroids in water samples by solid-phase microextraction and gas chromatography-mass spectrometry［J］. Anal Bioanal Chem, 2007,387(5):1841-1849.
【11】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, 2012,46(3):227-229.
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