固相萃取-高效液相色谱法测定茶叶中有机氮农药残留量
HPLC Determination of Residual Organonitrogen Pesticides in Tea by Solid-phase Extraction
摘 要
提出了茶叶中5种有机氮农药(速灭威、残杀威、呋喃丹、甲萘威、抗蚜威)残留的高效液相色谱法.样品用丙酮-正己烷 (1+2)混合溶剂提取,经石墨碳固相小柱净化,以VP-ODS C18柱分析,乙腈-60 mmol·L-1磷酸(40+60)溶液为流动相,流速为1.0 mL·min-1,检测波长210 nm,外标法定量.在0.10~2.0 mg·kg-1之间的添加水平,5种有机氮农药的平均回收率在80.1%~94.8%之间,相对标准偏差在2.21%~7.13%之间,检出限在0.0125~0.05 mg·kg-1之间.
茶叶
固相萃取
有机氮农药
HPLC
Tea
Solid-phase extraction
Organonitrogen pesticides
Abstract
A methd based on solid-phase extraction (SPE) combined with HPLC for the determination of residual organonitrogen pesticides,namely,metolcarb,propoxur,carbofuran,carbaryl and pirimicarb,in tea was proposed.Pasticides in sample were extracted with solvent mixture of acetone-hexane (vol.ratio 1∶2),purified on a SPE column and eluted with acetonitrile-toluene mixture (vol.ratio 4∶1).HPLC analysis was carried out on a VP-ODS C18 column using a mobile phase of acetonitrile and 60 mmol·L-1 phosphoric acid solution mixture (vol.ratio 40∶60),and detected at 210 nm.At concentration levels between 0.10 and 2.0 mg·kg-1,recoveries of these pesticides were in range of 80.1%-94.8% and RSD′s in the range of 2.21%-7.13%.DL′s were in the range of 0.012 5-0.05 mg·kg-1.
中图分类号 O657.37
所属栏目 工作简报
基金项目 国家科技支撑计划(2006BAD06B01)
收稿日期 2007/5/10
修改稿日期
网络出版日期
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备注汤富彬(1971- ),男,浙江富阳人,副研,从事农药残留研究.
引用该论文: TANG Fu-bin,LOU Zhen-yun,CHEN Zong-mao*,LIU Guang-ming,LUO Feng-jian,WANG Wen-da. HPLC Determination of Residual Organonitrogen Pesticides in Tea by Solid-phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(10): 947～949
汤富彬,楼正云,陈宗懋,刘光明,罗逢健,王文达. 固相萃取-高效液相色谱法测定茶叶中有机氮农药残留量[J]. 理化检验－化学分册, 2008, 44(10): 947～949
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参考文献
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【2】Krause.Richard THigh-performance liquid chromatographic determination of aryl-methylcabamate residue using post-column hydrolysis electrochemical detection[J].J Chromatogr,1998:442-448．
【3】刘长武,刘潇威,翟广书,等.固相萃取-高效液相色谱法测定蔬菜、水果中的氨基甲酸酯杀虫剂及其代谢物残留[J].色谱,2003,21(3):255-257．
【4】Hsu Jong P,Schattenberg Herbet J,Garza Martham.Fast turnaround multiresidues screen for pesticide in produce[J].J Assoc of Anal Chem,1991,74(5):886-889．
【5】薛健,陈建明,杜志刚.槟榔中克百威的残留量分析[J].农药,1989,28(1):35-36．
【6】董顺玲,胡家枳,何志强,等.中药材中氨基甲酸酯类农药残留量的反相高效液相色谱法[J].药物分析杂志,2002,22(3):178-182．
【7】梁祈,魏雪芳.中药材黄芪中有机氮农药残留量的液相色谱检测方法[J].分析测试学报,2000,19(2):25-28．
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