多壁碳纳米管分散固相萃取-液相色谱串联质谱法测定大米中26种氨基甲酸酯类农药及其代谢产物残留量  

Determination of 26 Carbamate Pesticides and Their Metabolites Residues in Rice by Multi-Walled Carbon Nanotubes Dispersion Solid Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry

作　　者：范宏 谭莉 张惠峰 张慧[1] 蔡红梅[1] 张俊姝 宋志峰[1] 孟繁磊[1] FAN Hong;TAN Li;ZHANG Huifeng;ZHANG Hui;CAI Hongmei;ZHANG Junshu;SONG Zhifeng;MENG Fanlei(Institute of Agricultural Quality Standard and Testing Technology,Jilin Academy of Agricultural Sciences/Jilin Provincial Key Laboratory of Agro-Environment and Agro-Products Safety,Changchun 130033,China;Agricultural Comprehensive Administrative Law Enforcement Unit of Meihekou,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,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10期276-283,共8页Food Science and Technology

基　　金：吉林省科技厅重点研发项目(20210202110NC);吉林省科技厅创新平台(基地)和人才专项(20230505056ZP)。

摘　　要：目的:建立多壁碳纳米管分散固相萃取-液相色谱串联质谱法测定大米中26种氨基甲酸酯类农药及其代谢产物残留量的分析方法。方法:大米样品水化后经酸化乙腈提取,多壁碳纳米管净化,C_(18)色谱柱分离,流动相采用2 mmol/L甲酸铵水和2 mmol/L甲酸铵甲醇进行梯度洗脱,电喷雾正离子(ESI^(+))模式电离,多反应监测模式检测,基质标准曲线外标法定量。结果:结果表明,26种农药在0.2-100 ng/mL范围内线性关系良好,相关系数均大于0.999,方法的检出限(S/N=3)为0.01-0.18μg/kg,定量限(S/N=10)为0.03-0.58μg/kg。在1、2μg/kg和20μg/kg 3个添加水平下,26种农药的回收率为87.4%-112.8%,相对标准偏差(n=6)为1.46%-7.22%。结论:该方法操作简便、灵敏度和精密度高、结果准确可靠,适用于大米中氨基甲酸酯类农药及其代谢产物残留量的检测。Objective:To establish a method for the determination of 26 carbamate pesticides and their metabolites residues in rice by multi-walled carbon nanotubes dispersion solid phase extraction coupled with liquid chromatography-tandem mass spectrometry.Methods:The rice samples were mixed with water,extracted by 1%acetic acid acetonitrile,purified by multi-walled carbon nanotubes,separated by C_(18) column,gradient elution was performed with 2 mmol/L ammonium formate water and 2 mmol/L ammonium formate methanol as mobile phases,ionized by electrospray positive ion(ESI^(+))mode,detected by multiple reaction monitoring(MRM)mode,and quantified by matrix standard curve external standard method.Results:The results showed that the linear relationships of 26 pesticides were good in the range of 0.2-100 ng/mL,and the correlation coefficients were all greater than 0.999.The limits of detection(S/N=3)ranged from 0.01μg/kg to 0.18μg/kg,and the limits of quantitation(S/N=10)ranged from 0.03μg/kg to 0.58μg/kg.The recoveries of 26 carbamate pesticides and their metabolites residues at three spiked levels of 1,2μg/kg and 20μg/kg ranged from 87.4%to 112.8%,and the relative standard deviations(n=6)ranged from 1.46%to 7.22%.Conclusion:The method is simple,sensitive,accurate and reliable,and it is suitable for the determination of carbamate pesticides and their metabolites residues in rice.

关 键 词：多壁碳纳米管 分散固相萃取 液相色谱串联质谱法 大米 氨基甲酸酯类农药及其代谢产物 

分 类 号：TS207.53[轻工技术与工程—食品科学]