QuEChERS结合高效液相色谱-串联质谱法同时检测蔬菜水果中10种农药残留

Simultaneous determination of 10 kinds of pesticide residues in vegetables and fruit by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  QuEChERS  农药残留  蔬菜  水果

英文关键词:high performance liquid chromatography-tandem mass spectrometry  QuEChERS  pesticide residues  vegetable  fruit

中文摘要:

      目的 建立QuEChERS结合高效液相色谱-串联质谱法(high performance liquid chromatography -tandem mass spectrometry, HPLC-MS/MS)同时检测蔬菜水果中10种农药残留的分析方法。方法 称取粉碎后的样品使用乙腈提取, 采用QuEChERS法进行前处理, 即加入硫酸镁等盐类及乙二胺-N-丙基硅烷化硅胶(primary secondary amine, PSA)等吸附剂进行除水除杂等净化过程, 得到的净化液过滤膜后经高效液相色谱仪分离, 在多反应监测模式(multiple reaction monitoring, MRM)下进行检测, 外标法定量。结果 10种农药在0.13~180.00 ng/mL范围内线性关系良好, 相关系数均大于0.999, 方法检出限(limits of detection, LODs)为0.13 ~3.00 μg/kg。在低、中、高3个添加水平(LOQ、3 LOQ、10 LOQ)下, 10种农药的平均回收率为69.7%~106.9%, 相对标准偏差在0.5%~9.0%之间。结论 该方法具有操作简便、灵敏度高、速度快、准确可靠、稳定性强、对人员要求低、重现性强、检测成本低等的优点, 适用于蔬菜水果中10种农药残留量的同时测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of 10 kinds of pesticide residues in vegetables and fruits by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The weighed and crushed samples were extracted with acetonitrile, pretreated with QuEChERS method, that was, MgSO4 and other salts and primary secondary amine (PSA) and other adsorbents were added to carry out purification processes such as water and impurity removal, the purified solution obtained was filtered, and separated by high performance liquid chromatography and tested in multiple reaction monitoring (MRM), and quantified by external standard method. Results Ten kinds of pesticides had good linear relationship in the range of 0.13-180.00 ng/mL, the correlation coefficients were greater than 0.999, the limits of detection (LODs) were 0.13-3.00 μg/kg. Under 3 levels of low, medium and high (LOQ, 3 LOQ, 10 LOQ), the average recoveries of 10 kinds of pesticides were 69.7%-106.9%, the relative standard deviations were ranged from 0.5% to 9.0%. Conclusion The method has the advantages of simple operation, high sensitivity, fast speed, accuracy, reliability, strong stability, low personnel requirements, strong reproducibility and low detection cost, et c., it is suitable for the simultaneous determination of 10 kinds of pesticide residues in vegetables and fruits.