超高效液相色谱-串联质谱测定菊花中11种农药残留

Determination of 11 pesticide residues in chrysanthemum by ultra performance liquid chromatography-tandem mass spectrometry

建立了非茶叶类饮用植物菊花中11种农药残留的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。菊花样品经乙腈提取,凝胶渗透色谱（GPC）净化,收集16~38 min洗脱液,浓缩定容后采用UPLC-MS/MS在正离子模式下以多反应监测扫描方式进行监测。结果表明,GPC净化后能够有效去除杂质的干扰,11种农药3个添加水平的回收率为74.5%~115.8%,相对标准偏差（RSD）为1.8%~10.0%,决定系数（R2）在0.9990~0.9998之间。该方法操作简单、净化效果好且灵敏度高,准确度和精密度均符合农药残留分析的要求。

An ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS） method was developed for the determination of 11 pesticides in chrysanthemum. Pesticides were extracted with acetonitrile, cleaned up by GPC; eluent was collected at 16-38 min, and then separated with UPLC and detected with MS /MS in multiple reaction monitoring（ MRM） mode via positive electrospray ionization（ESI＋）. The results showed that it can effectively remove the interference of impurity. The average recoveries of the 11 pesticides at three fortification levels were between 74.5%-115.8%, with relative standard deviations（ RSDs） between 1.8%-10.0%, and determination coefficient（R2） between 0.9990-0.9998. The result indicated that this method is easy, sensitive and can achieve a good cleanup effect. The sensitivity, accuracy and precision of the method are all suitable and can meet the requirements of the multiple pesticide residues analysis.