液相色谱-串联质谱法同时测定丹参中139种农药残留
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广西壮族自治区科学技术厅重大专项计划(2015AC05038);国家中药标准化项目(ZYBZH-C-GX-09);国家药典委员会项目(ZG2016-2)


Simultaneous Determination of 139 Pesticide Residues in Salvia miltiorrhiza by LC-MS/MS
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    摘要:

    目的:采用液相色谱-串联质谱法建立丹参中农药多残留的测定方法。方法:样品经改良的QuEChERS方法提取,采用分散固相萃取(d-SPE)二次净化法净化,并采用液相色谱-串联质谱技术在多反应监测(MRM)模式下测定,内标法定量。结果:丹参中139种农药在0.005~0.2 mg/L范围内线性关系均良好;在10、50和100 μg/kg添加水平下,除了噻菌灵回收率偏低(67.2~67.9)外,其余农药的平均回收率为70.2%~126.1%,相对标准偏差(RSD)为1.2%~19.5%,139种农药的检测限为0.005~0.05 mg/kg。结论:该方法样品前处理简单快速,灵敏度、准确度和精密度均符合农药多残留检测技术的要求,适用于丹参中139种农药残留的快速筛查测定。

    Abstract:

    To study the multi-residues detection methods for Salvia miltiorrhiza by LC-MS/MS.Methods:A method using a modified QuEChERS and d-SPE clean-up followed by LC-MS/MS has been established for the quantitative determination of the residues.The extract was determined by LC-MS/MS in multi-reaction monitoring(MRM)mode,and internal standard method was applied to quantify the pesticides.Results:All the 139 pesticides showed good linearity in the range of 0.005~0.2 mg/L.The average recoveries of the pesticides at the spiked levels of 10,50,100 μg/kg ranged from 70.2~126.1% with the RSDs of 1.2~19.5%,except for Thiabendazole(67.2~67.9%).The limits of detection(LODs)of 139 pesticides were 0.005~0.05 mg/kg.The results demonstrated that this method was simple,rapid and suitable for the determination of 139 pesticide residues in Salvia miltiorrhiza.Conclusion:The analytical sensitivity and accuracy can meet the requirements of multiple pesticide residue analysis.

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李雯婷,苗水,陈铭,周恒,兰岚,毛秀红,季申.液相色谱-串联质谱法同时测定丹参中139种农药残留[J].世界中医药,2019,(04).

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  • 收稿日期:2019-03-10
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  • 在线发布日期: 2019-05-09
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