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    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.

       

      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.

       

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