GC-MS Determination of Residual Amounts of 36 Pesticides in Drinking Water with Enrichment by Solid Phase Extraction
摘 要
提出了固相萃取-气相色谱-质谱联用法测定饮用水中36种农药的残留量。样品用石墨化碳/氨基复合型小柱净化和富集后,经DB-1701P弹性石英毛细管柱分离,用电子轰击离子源及选择离子监测扫描模式进行质谱测定。36种农药在一定浓度范围内呈线性关系,检出限(3S/N)在0.001 3~0.070 mg·L-1之间。 按方法在水样的基础上加入农药混合标准溶液做回收试验,测得回收率在90.8%~112.4%之间 ,测定值的相对标准偏差(n=5)在3.20%~13.2%之间。
Abstract
GC-MS with enrichment by solid phase extraction was applied to the determination of residual amounts of 36 pesticides in drinking water. The sample was purified and enriched by passing through graphitized carbon/amino-compound column. DB-1701P elastic quartz capillary column was used for separation, and EI source with SIM mode was used in MS determination. Linearities for the 36 pesticides were obtained in definite concentration ranges, with values of detection limits (3S/N) ranged from 0.001 3-0.070 mg·L-1. Following the proposed method test for recovery was made by addition of mixed standard of the pesticides, values of recovery obtained were in the range of 90.8%-112.4%, with RSD′s (n=5) in the range of 3.20%-13.2%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 四川省医学重点实验室、成都市医学重点实验室建设经费资助
收稿日期 2011/2/19
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联系人作者杨元(zx2132@163.com)
备注杨元(1951-),男,四川成都人,主任技师,从事光谱、色谱、质谱应用研究工作。
引用该论文: YANG Yuan,GAO Ling,JING Lu,QIAO Bin-zong,LUO Xiao-fei. GC-MS Determination of Residual Amounts of 36 Pesticides in Drinking Water with Enrichment by Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(3): 283~286
杨元,高玲,景露,谯斌宗,罗小飞. 固相萃取-气相色谱-质谱法测定饮用水中36种农药残留量[J]. 理化检验-化学分册, 2012, 48(3): 283~286
被引情况:
【1】王秀丽,董民强, "固相萃取-毛细管柱-气相色谱法测定水中11种有机磷农药",理化检验-化学分册 50, 220-223(2014)
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参考文献
【1】USEPA Method 1657The determination of organo-phosphorus pesticides in municipal and industrial wastewater[S].
【2】GB/T 5750.9-2006生活饮用水标准检验方法 农药指标[S].
【3】ROSSIA S, DALPEROA A P, GHINI S, et al. Multi residual method for the gas chromatography analysis of pesticides in honeybees cleaned by gel permeation chromatography[J]. Journal of Chromatography A, 2001,905(1/2):223-232.
【4】杨元,高玲,景露.SPE-GC/MS法测定饮水中20种有机磷和氨基甲酸酯农药[J].中国测试技术, 2009,35(2):86-89.
【5】张潜,黎源倩,陈刚.固相萃取-气相色谱法测定饮用水中15种农药残留[J].中国卫生检验杂志, 2007,17(12):2147-2150.
【6】刘芃岩,马育松.固相萃取技术在农药残留分析中的应用[J].河北大学学报:自然科学版, 2005,44(1):109-115.
【7】EUROPEAN COMMUNITIES 2002/657/ECImplementing council directive 96/23/EC concerning the performance of analytical methods and the interpretation of results[S].
【2】GB/T 5750.9-2006生活饮用水标准检验方法 农药指标[S].
【3】ROSSIA S, DALPEROA A P, GHINI S, et al. Multi residual method for the gas chromatography analysis of pesticides in honeybees cleaned by gel permeation chromatography[J]. Journal of Chromatography A, 2001,905(1/2):223-232.
【4】杨元,高玲,景露.SPE-GC/MS法测定饮水中20种有机磷和氨基甲酸酯农药[J].中国测试技术, 2009,35(2):86-89.
【5】张潜,黎源倩,陈刚.固相萃取-气相色谱法测定饮用水中15种农药残留[J].中国卫生检验杂志, 2007,17(12):2147-2150.
【6】刘芃岩,马育松.固相萃取技术在农药残留分析中的应用[J].河北大学学报:自然科学版, 2005,44(1):109-115.
【7】EUROPEAN COMMUNITIES 2002/657/ECImplementing council directive 96/23/EC concerning the performance of analytical methods and the interpretation of results[S].
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