GC Determination of Residual Amounts of Pyrethroid and Endosulfan Insecticides in Tea
摘 要
应用气相色谱法对茶叶中拟除虫菊酯及硫丹类杀虫剂残留量作快速测定.用正己烷-丙酮(1+1)混合溶剂提取样品中的杀虫剂,残渣用正己烷-乙酸乙酯(1+1)混合溶剂溶解.此溶液先后经凝胶渗透色谱和固相萃取法进行纯化,固相萃取系ENVI-Carb柱和氟罗里硅土固相萃取柱连续净化.以正己烷-乙酸乙酯(1+1)混合溶液将杀虫剂从柱上洗脱,所得洗脱液在40 ℃蒸干,用正己烷溶解残渣,将此溶液引入气相色谱仪测定,测定采用电化学检测器并用外标法定量.共测定了茶叶样品中7种拟除虫菊酯和3种硫丹类杀虫剂,所得响应信号值与杀虫剂浓度在0.01~0.10 mg·kg-1范围呈线性关系,方法的检出限(3S/N)为0.01 mg·kg-1,方法的回收率在87.4%~91.9%之间,测定值的相对标准偏差(n=10)小于7%.
Abstract
Gas chromatography was used in the rapid determination of residual amounts of pyrethroid and endosulfan insectisides.Insecticides in the sample were extracted with mixture of n-hexane and acetone mixed in the ratio of 1 to 1 by volume,and the residue was dissolved in mixed solvent of n-hexane and ethylacetate (1+1 by vol.).The solution obtained was purified sequentially by gel permeation chromatography and solid phase extraction with ENVI-Carb column and fluorisil column in succession.The eluate in n-hexane-ethyl acetate mixture (1+1) was evaporated to dryness at 40 ℃,and the residue was dissolved and determined by GC.GC determination of 7 pyrethroids and 3 endosulfans was carried out by external standard method with EC detection.Linear relationship between values of response signal and concentration of the insecticides was obtained in the range of 0.01-0.10 mg·kg-1,and detection limit (3S/N) of the method found was 0.01 mg·kg-1.Tests for recovery and precision were made and values of recovery and RSD′s (n=10) found were in the ranges of 87.4%-91.9% and 7% respectively.
中图分类号 O657.37
所属栏目 工作简报
基金项目 国家科技部重点课题资助项目(2002EE550021)
收稿日期 2008/11/19
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备注李爱军(1968-),男,长春市人,硕士,主要研究方向为食品分析、农残检验工作.
引用该论文: LI Ai-jun,ZHAO Dong-han,LU Li-jun,MU Jun,ZHOU Xiao,LIU He-pin,YAO Tian-ling. GC Determination of Residual Amounts of Pyrethroid and Endosulfan Insecticides in Tea[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(6): 642~644
李爱军,赵冬晗,卢利军,牟峻,周晓,刘和平,姚天玲. 气相色谱法测定茶叶中拟除虫菊酯及硫丹类杀虫剂残留量[J]. 理化检验-化学分册, 2009, 45(6): 642~644
被引情况:
【1】王兴宁,蔡秋,朱明,舒丹丘,刘康书,王缅, "凝胶渗透色谱-固相萃取净化-气相色谱-串联质谱法测定茶叶中33种农药的残留量",理化检验-化学分册 47, 412-416(2011)
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参考文献
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【2】SHASHI B Singh,GITA Kulshrestha.Determination of endosulfan residues in eggplant (solanum melongena) by ELISA[J].Environmental Science,2004,39:411-418.
【3】ATMAKURU Ramesh,PERUMAL Elumalai Ravi.Determination of residues of endosulfan in human blood by a negative ion chemical ionization gas chromatographic/mass spectrometric method:impact of long-term aerial spray exposure[J].Pest Management Science,2003,59(3):252-258.
【4】GB/T 5009.162-2003动物性食品中有机氯农药和拟除虫农药多组分残留量的测定[S].
【5】朱坚.食品中危害残留物的现代分析技术[M].上海:同济大学出版社,2003:112-114.
【6】江桂斌.环境样品前处理技术[M].北京:化学工业出版社,2004:140-141.
【7】葛志荣,李元平,黄冠胜,等.日本肯定列表制度-食品中农业化学品残留限量:食品卷[M].北京:中国标准出版社,2004.
【8】PAPADOPULOU-MOURKIDOU E.Analysis of established pyrethroids insecticide[J].Residue Rev,1983,89:79-208.
【9】SHARP G J,BRAYAN J G,DILLIS S,et al.Clearup and chromatographic determination of organophosphate,pyrethroid and carabamate grain protectants[J].Analyst,1988,113:1493-1507.
【10】MESRES R,ATAWIJAYA S,CHERALIER C.Methods for the study and determination of pestcide in cereal products.XXXIV Organchlorine.organophosphorus and pyrethroid residues[J].Ann Falsif Expert Chem,1979,72:577-58.
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