摘要
目的建立气相色谱-串联质谱法(gaschromatography tandem mass spectrometer,GC-MS/MS)测定普洱茶中192种农药(包括同分异构体)残留的分析方法。方法普洱晒青毛茶样品用乙腈过夜浸泡后振摇提取,浓缩后经Clearnet TPT固相萃取柱净化,样品采用气相色谱-串联质谱法选择MRM模式测定,以环氧七氯为内标物定量。通过检出限、定量限、加标回收率、线性范围验证方法的可行性。结果所有农药在0.025～1.6 mg/L范围内,线性关系r^2在0.995以上;方法的检出限和定量限范围分别为0.0003～0.25 mg/kg、0.0009～0.8 mg/kg;加标水平分别为0.025、0.05、0.1 mg/kg时,农药的平均回收率范围为64%～126%,相对标准偏差均小于9.8%。结论该方法灵敏度、准确度和精密度良好,符合多农药残留检测的技术要求。
Objective To establish a method for the determination of 192 kinds of pesticides residues in Pu’er tea by gas chromatography tandem mass spectrometry(GC-MS/MS).Methods The sample of Pu’er sun tea was soaked in acetonitrile overnight,shaken and extracted,concentrated and purified by Clearnet TPT solid phase extraction column.The samples were determined by gas chromatography-tandem mass spectrometry with multi-reaction monitoring(MRM)mode and quantified by epoxy heptachlor.The method was validated according to the limit of detention(LOD),limit of quantitative(LOQ),and the percentage of recovery and linearity range.Results The correlation coefficients(r^2)of all pesticides residues were more than 0.995 with the concentration range of0.025-1.6 mg/L.The LODs and LOQs of the method were 0.0003-0.25 mg/kg and 0.0009-0.8 mg/kg,respectively.The average recoveries of pesticides ranged from 64%to 126%,and the relative standard deviations were less than9.8%at spiked levels of 0.025,0.05 and 0.1 mg/kg.Conclusion This method is sensitive,accurate and precise,which can meet the technical requirements for multi-pesticide residue detection.
作者
满红平
吕生
毛静春
车涛
罗正刚
姜东华
周利
MAN Hong-Ping;LV Sheng;MAO Jing-Chun;CHE Tao;LUO Zheng-Gang;JIANG Dong-Hua;ZHOU Li(Pu’er Comprehensive Technical Testing Center,Pu’er 665000,China;The Research Institute,Chinese Academy of Agricultural Science,Zhejiang 310008,China)
出处
《食品安全质量检测学报》
CAS
2019年第9期2702-2722,共21页
Journal of Food Safety and Quality
基金
云南省科技厅重点研发计划(2018BC005-05)
普洱市科技项目(2017KJ004)~~
关键词
普洱茶
农药多残留
气相色谱-串联质谱法
多反应离子检测
Pu’er tea
multi-pesticide residue
gas chromatography tandem mass spectrometry
multi-reaction monitoring
作者简介
通讯作者:满红平,高级工程师,主要研究方向为食品安全检测。E-mail:278854127@qq.com
