中药材黄芪中有机磷农药残留量的超高效液相色谱-串联质谱法研究

目的:建立了中药材黄芪中25种有机磷杀虫剂残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法:样品中的有机磷农药残留物经乙腈提取,PSA固相萃取柱(填料为N-丙基乙二胺)净化,丙酮-正己烷(20∶80)洗脱,最后采用超高效液相色谱-电喷雾串联质谱法在正离子多反应监测(MRM)扫描模式下进行测定。结果:25种有机磷农药成分在各自的线性范围内,线性关系良好,相关系数在0.993和0.999之间。在LOQ、5LOQ和10LOQ 3个添加浓度水平进行了添加回收率试验,平均回收率在74.1%和94.4%之间,RSD在2.5%和12.4%之间。各种有机磷农药成分的定量限在2～120μg·kg-1。结论:该方法操作简便,净化效果好,灵敏度、准确度和精密度均符合多残留检测技术的要求,可为中药材中有机磷农药污染状况调查提供新检测方法支持。

Determination of organophosphorus pesticide residues in Astragali Radix by UPLC-MS/MS

Objective: An ultra performance liquid chromatography-tandem mass spectrometric method was developed for the determination of twenty-five organophosphorus pesticides in traditional Chinese medicine Astragali Radix.Methods: The pesticides were extracted with acetonitrile,cleaned up by PSA solid phase extraction column,and finally analyzed by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) in the multiple-reaction-monitoring(MRM) mode via positive electrospray ionization(ESI+).Results:The method was validated at three fortification levels in milkvetch root.The standard calibration curves for twenty-five organophosphorus pesticides showed high correlation coefficient(0.993-0.999) over their respective concentration range.The average recoveries of all the twenty-five organophosphorus pesticides at the three fortification levels(LOQ,5LOQ and 10LOQ) were between 74.1% and 94.4% with the relative standard deviation between 2.5% and 12.4%.The limits of quantification(LOQ) of the twenty-five pesticides were between 2.0 μg·kg-1 and 120 μg·kg-1.Conclusion: It was indicated that the method developed in this study is easier,more sensitive and has a better purification effect.So,this method can be further applied to investigate the contamination status of traditional Chinese medicine by the organophosphorus pesticides.