固相膜萃取-气相色谱法测定养殖用水中痕量有机磷农药
GC Determination of Trace Amount of Organophosphorous Pesticides in Aquaculture Water with Solid Phase Disk Extraction
摘 要
采用固相膜萃取-气相色谱法测定养殖用水中乐果、甲基对硫磷和马拉硫磷等3种有机磷农药的含量.水样经C18固相萃取膜萃取后,用丙酮和二氯甲烷洗脱.用SPB-608毛细管色谱柱分离,氮磷检测器检测.3种有机磷农药的质量浓度均在0.02~1.0 μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.0025~0.004 μg·L-1之间.以空白样品为基体进行加标回收试验,回收率在93.0%~111%之间,测定值的相对标准偏差(n=5)在0.13%~5.2%之间.
固相膜萃取
有机磷农药
养殖用水
GC
Solid phase disk extraction
Organophosphorous pesticides
Aquaculture water
Abstract
GC with solid phase disk extraction was applied to the determination of 3 organophosphorous pesticides,i.e. roxion,methyl parathion and malathion in aquaculture water. The water sample was extracted by C18 solid phase disk,and eluted with acetone and dichloromethane. The analytes were separated on a SPB-608 capillary column and detected by NPD. Linear relationships between values of peak area and the mass concentration of 3 organophosphorous pesticides were kept in the same range of 0.02-1.0 μg·L-1,with detection limits (3S/N) in the range of 0.002 5-0.004 μg·L-1. The recovery rates measured by standard addition method were in the range of 93.0%-111%,with RSD (n=5) in the range of 0.13%-5.2%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201506009
所属栏目 工作简报
基金项目 浙江省科技计划项目(2012F30026;2013C37088);2012年度省重大科技专项(2012C13005);浙江省科技计划项目(2013F10065)
收稿日期 2014/5/11
修改稿日期
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联系人作者胡红美(huhm@zju.edu.cn)
备注胡红美(1986-),女,浙江衢州人,工程师,主要从事渔业环境及水产品质量安全研究.
引用该论文: HU Hong-mei,GUO Yuan-ming,JIN Yan-jian,LI Tie-jun,ZHU Jing-ping,DING Yue-ping,HE Yi-na. GC Determination of Trace Amount of Organophosphorous Pesticides in Aquaculture Water with Solid Phase Disk Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(6): 770～774
胡红美,郭远明,金衍健,李铁军,朱敬萍,丁跃平,何依娜. 固相膜萃取-气相色谱法测定养殖用水中痕量有机磷农药[J]. 理化检验－化学分册, 2015, 51(6): 770～774
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参考文献
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【17】THURMAN E M,SNAVELY K. Advances in solid-phase extraction disks for environmental chemistry[J]. TrAC Trends in Analytical Chemistry,2000,19(1):18-26．
【18】许鹏翔,袁东星,邓永智,等.水样中痕量有机磷农药的膜萃取-气相色谱法测定[J].分析化学,2002,30(3):321-323．
【2】孙耀,杨琴芳.养殖水中有机磷农药的毛细管气相色谱分析[J].海洋环境科学,1996,15(4):48-51．
【3】王艳洁,周传光,马新东,等.海水中14种有机磷农药的气相色谱测定方法[J].分析试验室,2008,27(增):436-440．
【4】PICO Y,FERNANDEZ M,RUIZ M J,et al. Current trends in solid-phase-based extraction techniques for the determination of pesticides in food and environment[J]. Journal of Biochemical and Biophysical Methods,2007,70(2):117-131．
【5】白红妍,韩彬,郑立桑,等.桑沟湾水体中有机磷农药残留组成与分布[J].岩矿测试,2012,31(4):632-637．
【6】WANG Yuan-feng,DU Ran. Simultaneous extraction of trace organophosphorous pesticides from plasma sample by automated solid phase extraction and determination by gas chromatography coupled with pulsed flame photo metric detector[J]. Forensic Science International,2010,198(1/3):70-73．
【7】周憨,石雷,李取生,等.珠江河口水体有机磷农药的含量与季节变化[J].中国环境科学,2013,33(2):312-318．
【8】YAO Zi-wei,JIANG Gui-bin,LIU Jie-min,et al. Application of solid-phase microextraction for the determination of organophosphorous pesticides in aqueous samples by gas chromatography with flame photometric detector[J]. Talanta,2001,55(4):807-814．
【9】LAMBROPOULOU D A,PSILLAKIS E,ALBANIS T A,et al. Single-drop microextraction for the analysis of organophosphorous insecticides in water[J]. Analytical Chimica Acta,2004,516(1/2):205-211．
【10】金晓英,袁东星.动态液相微萃取-气相色谱法测定水样中有机磷农药残留[J].分析化学,2005,33(3):347-350．
【11】KHALILI-ZANJANI M R,YAMINI Y,YAZDNFAR N,et al. Extraction and determination of organophosphorus pesticides in water samples by a new liquid phase microextraction-gas chromatography-flame photometric detection[J]. Analytical Chimica Acta,2008,606(2):202-208．
【12】AHMADI F,ASSADI Y,HOSSEINI S M R M,et al. Determination of organophosphorus pesticides in water samples by single drop microextraction and gas chromatography-flame photometric detector[J]. Journal of Chromatography A,2006,1101(1/2):307-312．
【13】BERIJANI S,ASSADI Y,ANBIA M,et al. Dispersive liquid-liquid microextraction combined with gas chromatography-flame photometric detection: Very simple,rapid and sensitive method for the determination of organophosphorus pesticides in water[J]. Journal of Chromatography A,2006,1123(1):1-9．
【14】SCHELLIN M,HAUSER B,POPP P. Determination of organophosphorus pesticides using membrane-assisted solvent extraction combined with large volume injection-gas chromatography-mass spectrometric detection[J]. Journal of Chromatography A,2004,1040(2):251-258．
【15】JIA Chun-hong,ZHU Xiao-dan,CHEN Li,et al. Extraction of organophosphorus pesticides in water and juice using ultrasound-assisted emulsification-mixroextraction[J]. Journal of Separation Science,2010,33(2):244-250．
【16】SU Yi-song,JEN J. Determination of organophosphorous pesticides in water using in-syringe ultrasound-assisted emulsification and gas chromatography with electron-capture detection[J]. Journal of Chromatography A,2010,1217(31):5043-5049．
【17】THURMAN E M,SNAVELY K. Advances in solid-phase extraction disks for environmental chemistry[J]. TrAC Trends in Analytical Chemistry,2000,19(1):18-26．
【18】许鹏翔,袁东星,邓永智,等.水样中痕量有机磷农药的膜萃取-气相色谱法测定[J].分析化学,2002,30(3):321-323．
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