气相色谱-串联质谱法同时测定三七中212种农药残留  

Simultaneous Determination of 212 Pesticide Residues in Panax Notoginseng by Gas Chromatography-Tandem Mass Spectrometry

作　　者：王一帆 吴易峰 徐敦明 陈达捷 郑文杰 季超 WANG Yi-fan;WU Yi-feng;XU Dun-ming;CHEN Da-jie;ZHENG Wen-jie;JI Chao(College of Food Science,Fujian Agriculture and Forestry University,Fuzhou 350002,China;Technical Center of Xiamen Customs,Xiamen 361026,China;College of Life Sciences,Tianjin Normal University,Tianjin 300382,China;State Key Laboratory for Conversation and Utilization of Yunnan Biological Resources,Yunnan Agricultural University,Kunming 650091,China)

机构地区：[1]福建农林大学食品科学学院,福建福州350002 [2]厦门海关技术中心,福建厦门361026 [3]天津师范大学生命科学学院,天津300382 [4]云南农业大学云南生物资源保护与利用国家重点实验室,云南昆明650091

出　　处：《分析测试学报》2023年第10期1251-1264,共14页Journal of Instrumental Analysis

基　　金：云南省科技厅科技计划项目(202102AE090042)。

摘　　要：建立了气相色谱-串联质谱(GC-MS/MS)同时测定三七中212种农药残留的方法。样品以乙腈-乙酸乙酯(体积比1∶3)提取,经FaPEx-BKT50固相萃取柱净化,待测物采用GC-MS/MS测定,以保留时间和特征离子对定性,外标法定量。结果表明,212种农药在10~200µg/L范围内线性关系良好,相关系数(r^(2))均大于0.999,检出限(S/N=3)为0.003~0.02 mg/kg,定量下限(S/N=10)为0.01~0.05 mg/kg。在空白样品中进行0.02、0.04、0.1 mg/kg 3个水平的加标回收实验,212种农药的平均回收率为60.0%~121%,相对标准偏差(RSD)为0.90%~31%。该方法简单、灵敏、稳定,可有效去除复杂基体的干扰,各项技术指标均满足国内外农药残留的限量要求,适用于中药材三七中痕量农药的残留测定。A method for the simultaneous determination of 212 pesticide residues in Panax notogin-seng by gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed.The samples were extracted by acetonitrile-ethyl acetate(1∶3,by volume),and cleaned up by a FaPEx-BKT50 solid phase extraction cartridge.The analytes were measured on GC-MS/MS,characterized by reten-tion time and characteristic ion pairs,and quantified by external standard method.The results showed that the analytes were linear in the range of 10-200µg/L,with linear correlation coefficients(r^(2))more than 0.999.The limits of detection(S/N=3)for the analytes were 0.003-0.02 mg/kg and the limits of quantitation(S/N=10)were 0.01-0.05 mg/kg.At the spiked levels of 0.02,0.04,0.1 mg/kg,the average recoveries of 212 analytes in blank sample were 60.0%-121%with relative standard deviations(RSDs)of 0.90%-31%.The method is simple,sensitive and stable,and all the technical parameters meet the requirements of the domestic and international standards for pesticide residue monitoring,and can be applied to the determination of trace pesticide residues in Panax notoginseng.

关 键 词：气相色谱-串联质谱法(GC-MS/MS) 三七 多农药残留 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]