蜂蜜中多种有机磷农药残留的液相色谱串联质谱检测
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国家认证认可监督管理委员会资助项目(2006B407)


Simultaneous determination of multiple organophosphorus pesticides residues in honey by liquid chromatography tandem mass spectrometry
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    摘要:

    针对敌百虫、敌敌畏和蝇毒磷为常用的防治蜜蜂天敌或虫害的有机磷农药杀虫剂,易在蜂蜜中产生残留,建立了蜂蜜中敌百虫、敌敌畏和蝇毒磷残留的液相色谱串联质谱(LC-MS/MS)同时测定方法。蜂蜜样品经乙酸乙酯提取、浓缩,用甲醇溶解残渣,液相色谱(LC)分离,电喷雾(ESI)-MS/MS多反应监测(MRM)模式检测,外标基体曲线定量。3种有机磷农药在20~500 μg/L范围内线性响应良好,相关系数均大于0.994;获得的检出限均为0.1 μg/kg,定量限均为4 μg/kg。在加标浓度为10~40 μg/kg范围内,平均回收率为78.5%~96.8%,相对标准偏差为9.1%~13.1%。

    Abstract:

    The trichlorfon, dichlorvos, and coumafos are commonly used as organophosphorus pesticides to control pests or natural enemies of bees, but they easily contaminate the honey. A simultaneous determination method for trichlorfon, dichlorvos and coumafos residues in honey is developed by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Samples are extracted with ethyl acetate and concentrated extracts, and then the residue is dissolved by methanol, and separated by HPLC, detected by electrospray ionization (ESI)-MS/MS with multiple reaction monitoring mode (MRM). It is found that the linear ranges of the three organophosphate pesticides are 20~500 μg/L with correlation coefficients over 0.994, the detection limits (LODs) are 0.1 μg/kg and the limits of quantification (LOQs) are 4 μg/kg for all of the three pesticides. The average recoveries of the three pesticides in spiked honeies at concentration levels of 10~40 μg/kg range from 78.5% to 96.8%, and the relative standard deviations are in the range of 9.1%~13.1%.

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王国民,李应国,戴滑,谢文,张进忠,周启明,李正国.蜂蜜中多种有机磷农药残留的液相色谱串联质谱检测[J].重庆大学学报,2011,34(7):131-136.

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  • 收稿日期:2011-03-02
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