摘要
目的:建立全自动QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe)前处理技术结合超高效液相色谱-串联质谱法同时检测茶叶中41种农药残留的方法。方法:茶叶样品粉末加水浸泡30 min后,经乙腈超声提取30 min,再经无水硫酸镁除水和乙二胺-N-丙基硅烷化硅胶(PSA)、石墨化炭黑(GCB)净化,采用超高效液相色谱-串联质谱仪检测。结果:41种农药的出峰时间介于1.57~6.88 min,且在相应质量浓度范围内相关系数(R2)介于0.99646~0.99938,呈现出良好的线性关系。在3种加标水平下,41种农药的平均回收率介于80.0%~108.7%,相对标准偏差(n=6)介于0.5%~8.6%;检出限为0.00012~0.00403 mg/kg,定量下限为0.000127~0.01344 mg/kg。结论:方法准确度高、灵敏度好、成本低、简便快速,适用于高效分析茶叶样品中41种农药痕量残留的同时检测。
Objective:To establish a method for simultaneous determination of 41 pesticide residues in tea by automatic QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)pretreatment combined with ultra-performance liquid chroma⁃tography-tandem mass spectrometry(UPLC-MS/MS).Methods:The tea sample powder was soaked in water for 30min,then extracted by ultrasonic extraction of acetonitrile for 30 min.After that,the extract was dehydrated by anhydrous mag⁃nesium sulfate and purified by PSA and GCB,and then detected by UPLC-MS/MS.Results:The peak time of the 41 pesti⁃cides ranged from 1.57 to 6.88 min,and The 41 pesticides showed good linearity in the corresponding concentration range,and the correlation coefficients(R2)ranged from 0.99646 to 0.99938.The recoveries for 41 pesticides at three spiked levels ranged from 80.0%to 108.7%,and the relative standard deviation(n=6)was from 0.5%to 8.6%.The limits of detection(LODs)and the limits of quantitation(LOQs)were in the range of 0.00012~0.00403 mg/kg and 0.000127~0.01344 mg/kg,respectively.Conclusion:The method is accurate,sensitive,simple,rapid and suitable for the simultaneous determina⁃tion of 41 pesticide residues in tea samples.
作者
吴丽荣
王春
王征
黄芊
石焱芳
Wu Li-rong;Wang Chun;Wang Zheng;Huang Qian;Shi Yan-fang(Quanzhou Medical College,Quanzhou,Fujian 362000,China;Fujian Inspection and Research Institute for Product Quality,Fuzhou,Fujian 350002,China)
出处
《福建分析测试》
CAS
2023年第4期11-16,共6页
Fujian Analysis & Testing
基金
泉州市科技局项目(2021N132S)
福建省市场监督管理局科技项目(FJMS2021001)。
关键词
茶叶
农药残留
全自动
超高效液相色谱-串联质谱法
Tea
pesticide residues
Automatic
ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
