QuEChERS-HPLC-MS/MS法测定西葫芦中霜霉威

Determination of Propamocarb Residue in Summer Squash by QuEChERS-HPLC-MS/MS

[目的]建立西葫芦中霜霉威残留的QuEChERS-高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。[方法]样品用含2.5%甲酸的乙腈提取,QuEChERS法净化,用高效液相色谱串联质谱法分析,采用多反应离子检测模式(MRM)检测,外标法定量。[结果]霜霉威在0.0001~0.2 mg/L范围内线性响应良好,在0.01、0.1、1 mg/kg 3个添加水平下,平均回收率为91.4%~95.7%,相对标准偏差(RSD)为1.1%~1.8%,方法的检出限(LOD)为8×10-5ng,定量限(LOQ)为0.01 mg/kg。[结论]建立样品前处理方法简单、高效、节省溶剂,残留检测方法灵敏度高、结果准确、可靠,满足农药残留分析要求。

[Aims]An analytical method for determination of propamocarb residues in summer squash was developed using QuEChERS and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).[Methods]Propamocarb residues in summer squash were extracted with acetonitrile containing 2.5%formic acid and purified by QuEChERS method.Finally,the residues were detected by HPLC-MS/MS under multiple reaction monitoring mode(MRM)and quantified by external standard method.[Results]The instrument response at 0.0001-0.2 mg/L concentration of propamocarb had a good linearity.At the spiked concentration of 0.01,0.1 and1 mg/kg,mean recoveries of propamocarb in summer squash ranged from 91.4 to 95.7%,and the relative standard deviation(RSD)was 1.1-1.8%.The limit of detection(LOD)was 8×10-5 ng and the limit of quantitation(LOQ)was 0.01 mg/kg.[Conclusions]The developed method is simple,efficient,and solvent-saving.The results show its accuracy and precision meet the requirements of pesticide residue analysis.