GC Determination of 21 Organochlorine and 4 Organophosphorus Pesticides in Soil
摘 要
应用气相色谱法测定土壤中21种有机氯农药和4种有机磷农药(OCP′s及OPP′s)的含量。土壤样品(10 g)以丙酮正己烷(1+1)混合液(200 mL)在65 ℃用索氏提取7 h。提取液蒸缩至约2 mL,用经固相萃取小柱净化。用上述混合液6 mL分3次从柱上洗脱,洗脱液浓缩至1 mL供气相色谱分析。测定OCP′s时用CLPⅡ型毛细管色谱柱分离,电子捕获检测器检测;测定OPP′s时用1701型毛细管色谱柱分离,火焰光度检测器检测。21种OCP′s和4种OPP′s在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.14~0.38 μg·kg-1之间。加标回收率在68.0%~125%之间,测定值的相对标准偏差(n=10)在2.8%~5.9%之间。
Abstract
GC was applied to the determination of 21 organochlorine and 4 organophosphorus pesticides (OCP′s and OPP′s) in soil. The sample (10 g) was extracted for 7 h with 200 mL of a mixture of acetone and nhexane (1+1) at 65 ℃ by soxhlet extraction. The extract was evaporated to ca. 2 mL and purified on SPE column. The column was eluted thrice with acetonnhexane (1+1) mixture, 2 mL of which were used in each elution. The eluate was evaporated to 1 mL and used for GC analysis. Separation on CLPⅡcapillary column and detection by ECD were used for determination of OCP′s, and separation on 1701 capillary column and detection by FPD were used for determination of OPP′s. Linear relationships between values of peak area and mass concentration of the 21 organochlorines and 4 organophosphoruses were kept in definite ranges. Detection limits (3S/N) found were ranged from 0.14 to 0.38 μg·kg-1. Values of recovery found by standard addition method were in the range of 68.0%-125%, with values of RSD′s (n=10) the range of 2.8%-5.9%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2013/5/11
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联系人作者马健生(mjs1015@163.com)
备注马健生(1983-),男,吉林省吉林市人,工程师,硕士,研究方向为有机地球化学。
引用该论文: MA Jiansheng,WANG Xin,WANG Haijiao,LI Lijun,XIAO Gang,HU Jianfei. GC Determination of 21 Organochlorine and 4 Organophosphorus Pesticides in Soil[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(6): 740~744
马健生,王鑫,王海娇,李丽君,肖刚,胡建飞. 气相色谱法测定土壤中21种有机氯农药和4种有机磷农药[J]. 理化检验-化学分册, 2014, 50(6): 740~744
被引情况:
【1】卢亚玲,贾清华,肖加加,刘文杰, "固相萃取-气相色谱-质谱法测定果蔬中36种农药残留",理化检验-化学分册 51, 828-832(2015)
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【6】德吉,次仁,刘勇.气相色谱火焰光度法测定土壤中有机磷农药残留[J].分析试验室, 2012,31(3):89-91.
【7】张丽,李楠,万延延,等.采用气相色谱法测定土壤中有机磷农药[J].污染防治技术, 2004,24(2):69-73.
【8】佟玲,黄园英,张玲金,等.气相色谱质谱法测定土壤中有机氯农药及多氯联苯[J].理化检验化学分册, 2009,45(7):858-861.
【9】陈卫明,邓天龙,张勤,等.土壤中有机氯农药残留的分析技术研究进展[J].岩矿测试, 2009,28(2):151-156.
【10】马云云,王斌之,时杰.微波萃取气相色谱法测定土壤中有机氯残留[J].环境监测管理与技术, 2009,21(4):56-58.
【11】NATALIA F U, GIUSEPPE C, ELISA B C, et al. Soildphase microextraction as a clean up and preconcentration procedure for organochlorine pesticedes determination in fish tissue by gas chromatography with electron captures detection[J]. Chromatography A, 2003,1017:35-44.
【12】李月娥,孙欣阳,顾海东,等.加速溶剂萃取固相萃取小柱净化气相色谱法测定土壤中有机磷农药[J].中国环境监测, 2012,28(5):88-91.
【13】封棣,阎正,赵亚奎,等.固相萃取毛细管气相色谱法测定中草药及其土壤中多种有机氯农药残留量[J].分析试验室, 2005,24(10):8-12.
【14】吴丽华,李建科.气相色谱法在农药残留分析中的应用[J].粮油食品科技, 2006,14(4):57-58.
【15】ANNA B, ROSITSA M, DEYANA S. Solid/phase extraction on sorbents of different retention mechanisms followed by determination by gas chromatography mass spectrometric and gas chromatographyelectron capture detection of pesticide residues in crops[J]. Journal of Chromatography A, 2007,1150(1/2):136-144.
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