氨基化多壁碳纳米管分散固相萃取-气相色谱串联质谱法测定大米中22种有机磷类农药残留  

Determination of 22 Organophosphorus Pesticide Residues in Rice by Aminated Multi-wall Carbon Nanotubes Dispersed Solid Phase Extraction with Gas Chromatography-Tandem Mass Spectrometry

作　　者：谭莉 范宏 张慧[1] 张俊姝 孟繁磊[1] 宋志峰[1] TAN Li;FAN Hong;ZHANG Hui;ZHANG Junshu;MENG Fanlei;SONG Zhifeng(Jilin Provincial Key Laboratory of Agro-Environment and Agro-Products Safety,Risk Assessment Lab of Agri-Products Quality and Safety(Changchun),Institute of Agricultural Quality Standard and Testing Technology,Jilin Academy of Agricultural Sciences,Changchun 130033,China;Agricultural Comprehensive Administrative Law Enforcement Unit of Meihekou City,Meihekou 135000,China)

机构地区：[1]吉林省农业科学院农业质量标准与检测技术研究所,吉林省农业环境与农产品安全重点实验室,农业农村部农产品质量安全风险评估实验室(长春),吉林长春130033 [2]梅河口市农业综合行政执法大队,吉林梅河口135000

出　　处：《食品科技》2023年第9期285-290,298,共7页Food Science and Technology

基　　金：吉林省科技发展计划项目(20210202110NC);国家农产品质量安全风险评估计划项目(14225060)。

摘　　要：文章建立了一种以氨基化多壁碳纳米管(Aminated multi-walled carbon nanotubes,MWCNTsNH_(2))为分散固相萃取吸附剂的前处理净化技术,采用气相色谱-三重四极杆串联质谱(Gas chromatography-triple quadrupole mass spectrometry,GC-MS/MS)同时测定大米中22种有机磷农药残留的方法。大米中残留的农药经酸化乙腈提取,MWCNTs-NH2净化后,采用GC-MS/MS测定,基质标准曲线外标法定量。22种农药在2~200μg/L范围内线性关系良好,相关系数(r)均大于0.999,方法检出限(Limit of detection,LODs)为0.002~0.005 mg/kg,定量限(Limit of quantitation,LOQs)为0.005~0.010 mg/kg。在0.010、0.020、0.100 mg/kg 3个加标水平的平均回收率为82.6%~106%,相对标准偏差(Relative standard deviation,RSD,n=6)均小于6.78%。该方法操作简单、快速、准确,适用于大米中农药多残留的高通量检测。A pre-treatment purification process using aminated multi-walled carbon nanotubes(MWCNTs-NH_(2))as dispersed solid phase extraction adsorbent was established.A method for the simultaneous determination of 22 organophosphorus pesticide residues in rice was developed by gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS).The pesticide residues in rice were extracted by acidified acetonitrile,purified by MWCNTs-NH 2,determined by GC-MS/MS,and quantified by matrix standard curve external standard method.The linear relationship of 22 pesticides was good in the range of 2–200μg/L,and the correlation coefficient(r)was greater than 0.999.The limits of detection(LODs)were 0.002–0.005 mg/kg,and the limits of quantification(LOQs)were 0.005–0.010 mg/kg.The average recoveries were 82.6%–106%,at 0.010,0.020 and 0.100 mg/kg,and the relative standard deviations(RSD,n=6)were all smaller 6.78%.The method is simple,rapid and accurate,and is suitable for the high throughput detection of pesticide residues in rice.

关 键 词：氨基化多壁碳纳米管 气相色谱-三重四极杆串联质谱 有机磷农药 大米 

分 类 号：TS207.53[轻工技术与工程—食品科学]