高效液相色谱串联质谱法检测枣中吡丙醚和氟啶虫酰胺的残留量

Determination of Pyriproxyfen and Flonicamid in Jujube by HPLC-MS/MS

建立高效液相色谱串联质谱检测枣中吡丙醚和氟啶虫酰胺的分析方法。样品用乙腈提取,PSA净化,多反应监测模式检测,外标法定量。在0.01~2.00 mg/L范围内,吡丙醚和氟啶虫酰胺在枣中的质量浓度与峰面积均呈良好的线性关系,其相关系数均大于0.9981。在0.02~1.00 mg/kg添加水平下,吡丙醚和氟啶虫酰胺在枣中的平均回收率为77.3%~103.1%,相对标准偏差(RSD)为0.8%~4.5%。吡丙醚和氟啶虫酰胺在枣中的定量限(LOQ)均为0.02 mg/kg。该方法快速简便,准确可靠。施药后28 d,枣最终样品中吡丙醚的残留量为0.11 mg/kg,氟啶虫酰胺的残留量<0.02 mg/kg。

The method for determining pyriproxyfen and flonicamid residues in jujube was established based on HPLC-MS/MS.The samples were extracted with acetonitrile and purified with primary secondary amine(PSA).The mass spectrometer was performed in multi-reaction monitoring mode.The pyriproxyfen and flonicamid residues were quantified by the external standard method.The results indicated that there was a good linear relationship between mass concentration and peak area of pyriproxyfen and flubendamide in jujube in the range of 0.01~2.00 mg/L with correlation coefficients more than 0.9981.The average recoveries of pyriproxyfen and flonicamid were 77.3%~103.1%,and the relative standard deviation(RSD)were 0.8%~4.5%at the addition level of 0.02~1.00 mg/kg.The limit of quantitation(LOQ)of pyriproxyfen and flonicamid were 0.02 mg/kg.The method was fast,simple,accurate and reliable.The final residues of pyriproxyfen and flonicamid were 0.11 mg/kg and<0.02 mg/kg,respectively.