分散固相萃取-气相色谱三重四极杆串联质谱法测定玫瑰花茶中13种菊酯类农药残留

Determination of 13 Pyrethrin Pesticide Residues in Rose Tea by Dispersed Solid Phase Extraction-Gas Chromatography Triple Quadrupole Tandem Mass Spectrometry

建立了分散固相萃取-气相色谱三重四极杆串联质谱法测定玫瑰花茶中的13种菊酯类农药的分析方法。玫瑰花茶经乙腈和甲酸(99∶1_(v/v))提取后,QuEChERs净化,MRM模式测定,外标法定量。以QuEChERs作为前处理方法,优化吸附剂组合和用量,以及碰撞能和驻留时间。结果表明:13种菊酯含量在10～200μg/L间呈良好的线性关系,相关系数r^2均大于0.995。以空白基质进行3个水平添加浓度0.02～0.20 mg/kg,平均回收率为75.4%～87.6%,相对标准偏差(RSD)为1.9%～7.7%,该方法的简单快速,灵敏度、准确度和精密度均符合菊酯类农药测定的技术要求。

A method for the determination of 13 pyrethroid pesticides in Rose Tea by dispersive solid phase extraction coupled with gas chromatography triple quadrupole tandem mass spectrometry was established. Rose tea was extracted by acetonitrile and formic acid (99:1v/v), purified by QuEChERs, determined by MRM mode and quantified by external standard method. QuEChERs was used as the pretreatment method to optimize the combination and the amount of adsorbents, collision energy and residence time. The results showed that there was a good linear relationship between the content of 13 pyrethroids in the range of 10-200μg/L, and the correlation coefficient R2 was greater than 0.995. The average recovery was 75.4-87.6% and the relative standard deviation (RSD) was 1.9-7.7%. The method was simple and rapid. The sensitivity, accuracy and precision of the method met the technical requirements for the determination of pyrethroid pesticides.