超高效液相色谱-串联质谱法测定大米中的敌瘟磷、莠去津和多菌灵

Determination of ediphenghos,atrazine and carbendazim in rice by high performance liquid chromatography with tandem mass spectrometric method

建立高效液相色谱-串联质谱法同时测定大米中敌瘟磷、莠去津和多菌灵的方法。大米采用C18固相萃取小柱净化,以C18色谱柱为分离柱,以水-乙腈为流动相进行梯度洗脱,用高效液相色谱-串联质谱,电喷雾电离,多反应监测模式检测,外标法同时定量测定敌瘟磷、莠去津和多菌灵。该方法的线性范围敌瘟磷、莠去津、多菌灵2～200ng/ml,线性相关系数均≥0.999,检出限为4μg/kg,定量限10μg/kg;平均加标回收率61.7%～90.2%;相对标准偏差均小于8.0%。该方法可应用于同时定量检测大米中敌瘟磷、莠去津和多菌灵,操作简单、快速、准确可靠。

The high perfoamance liquid chromatography(HPLC)method with tandem mass spectrometric determination for ediphenghos,atrazine and carbendazim in rice was established.Using C18 solid phase extraction column to purify the rice,the separation was performed by a C18 column with the gradient elution of water and acetonitrile.The ediphenghos,atrazine and carbendazim in rice were detected by tandem quadrupole mass spectrometry by multiple reaction monitoring(MRM)under positive electrospray ionization(ESI).Quantification was performed by external standard calibration.The results showed that the calibration curves of the 3 compounds showed a good linearity in the range of 2-200 ng/ml for ediphenghos,atrazine and carbendazim,and the correlation were all above 0.999.The detection limit of the method was 4μg/kg,and the limit of quantification was 10μg/kg.The average recoveries were in the range of 61.7%-90.2%,and the relative standard deviations of the 3 compounds were all less than 8.0%.The HPLC-MS/MS method for simultaneous determination of ediphenghos,atrazine and carbendazim in rice had the advantages of simple operation,rapidity ang accuracy.