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Position: Home > Articles > Rapid Determination of 35 Pesticides' Residues in Tea by GC-MS and LC-MSMS China Tea Processing 2019 (3) 48-58

GC-MS和LC-MSMS法快速测定茶叶中35种农药残留

作  者:
刘相真;叶美君;陆小磊
单  位:
中华全国供销合作总社杭州茶叶研究院
关键词:
GC-MS;LC-MSMS;基质分散固相萃取;茶叶;农药残留;最大残留限量
摘  要:
文章建立了超高效液相色谱-串联质谱联用仪(LC-MSMS)和气相色谱-质谱联用仪(GC-MS)快速测定茶叶中35种农药的方法。利用基质分散固相萃取法进行样品前处理,比较了乙腈、乙腈+100μL乙酸、正己烷作为提取溶剂,不同比例的氯化钠-硫酸镁体系,以及不同比例的PSA-石墨化碳体系对35种农药在茶叶中回收率的影响,最终选择采用10 mL乙腈提取,1 g氯化钠和4 g硫酸镁盐析,以及200 mg N-丙基乙二胺(PSA)和100 mg石墨化碳净化,提取液通过LC-MSMS和GC-MS进行测定。在该前处理条件下的结果表明,35种农药化合物在5.0~500.0μg/L的质量浓度范围内,标准工作曲线相关系数均大于0.99,且在0.05、0.1、0.5 mg/kg的质量分数添加水平下,回收率均在60%~120%之间,相对标准偏差小于10.0%,最小检出限均符合各国规定的检测限量要求。该方法操作简单快捷、分析灵敏准确,适用于茶叶中农药多残留的快速检测。
译  名:
Rapid Determination of 35 Pesticides' Residues in Tea by GC-MS and LC-MSMS
作  者:
LIU Xiang-zhen;YE Mei-jun;LU Xiao-lei;Hangzhou Tea Research Institute CHINA COOP;China National Center of Quality Supervision and Inspection of Tea;Zhejiang Key Laboratory of Transboundary Applied Technology for Tea Resourses;
关键词:
GC-MS;;LC-MSMS;;Matrix Solid-Phase Dispersion;;Tea;;Pesticide residue;;MRL
摘  要:
A multi-residue method was developed for the simultaneous rapid determination of 35 pesticides' residues in tea by ultra high performance liquid chromatography tandem mass spectrometry(LC-MSMS) and gas chromatography mass spectrometer(GC-MS). Sample pretreatment was carried out by the matrix solid-phase dispersion(MSPD). Different solvents for acetonitrile, acetonitrile with 100 μL acetic acid, n-hexane, and system of NaCl and MgSO4 with various ratios, and system of N-Isopropylethylenediamine(PSA) and graphitizable carbonwith various ratios were compared. The optimized pretreatment conditions were 10 m L acetonitrile extraction, 1 g sodium chloride and 4 g magnesium sulfate salting out, and 200 mg PSA and 100 mg graphitization carbon purification. The results under the optimized pretreatment conditions showed that the correlation coefficients of the standard working curves for35 pesticides were all above 0.99 when the mass concentrations were in the range of 5.0 ~500.0 μg/L. The recoveries were between 60%~120%, and the relative standard derivations(RSDs) were less than 10% at 0.05 mg/kg, 0.1 mg/kgand 0.5 mg/kg levels, respectively, which meet the requirement of national standard. This method is simple and quick to operate, sensitive and accurate in analysis, and is suitable for rapid determination of pesticide residues in tea.

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