多壁碳纳米管分散固相萃取-液相色谱串联质谱法测定鸡肉中26种农药残留  

Determination of 26 kinds of pesticide residues in chicken by multi-walled carbon nanotubes dispersive solid phase extraction coupled liquid chromatography-tandem mass spectrometry

作　　者：吕佳宁 丁葵英 郭礼强 许文娟 田国宁 LU Jianing;DING Kuiying;GUO Liqiang;XU Wenjuan;TIAN Guoning

机构地区：[1]潍坊医学院公共卫生与管理学院,山东潍坊261043 [2]潍坊海关,山东潍坊261041

出　　处：《肉类工业》2022年第5期39-45,共7页Meat Industry

基　　金：潍坊市科学技术发展计划(2020ZJ1323)。

摘　　要：建立了一种基于多壁碳纳米管(MWCNTs)为吸附剂快速、准确的净化技术,联合液相色谱-串联质谱法对鸡肉中26种农药残留进行快速准确的定量分析方法,以提高鸡肉中多农药残留的检测效率。比较了长多臂碳纳米(LMWCNTs)、短多壁碳纳米管(SMWCNTs)和传统的PSA混合C18的三种净化剂的净化效果,探讨了不同量的LMWCNTs吸附剂净化效果及对各农药的吸附率,优化了26种农药残留的质谱参数,采用基质外标法定量。结果表明:鸡肉中26种农药在0.005~0.1μg/mL范围内相关系数为0.9992~1.00,检出限(LODS)在0.032~3.3μg/kg之间,定量限在0.14~10μg/kg(LOQS)之间;在鸡肉空白基质中进行10μg/kg、20μg/kg和100μg/kg三个水平加标试验,其回收率在70.9%~106.7%之间,精密度(n=7)在1.3%~11.4%之间。该方法简便快捷、特异性强、可靠性好,回收率及精密度均可满足鸡肉中26种农药残留限量的要求。The multi-walled carbon nanotubes(MWCNTs)was taken as adsorbent,and a kind of rapid and accurate purification technology was established,and liquid chromatography-tandemmass spectrometry was combined,and 26 kinds of pesticide residues in chicken were rapidly and accurately quantitatively analyzed,and the detection efficiency of multi-pesticide residues in chicken could be improved.The purification effects oflong multi-arm carbon nanotubes(LMWCNTs),short multi-walled carbon nanotubes(SMWCNTs)and traditional PSA mixed with C18 were compared.The purification effects of different amounts of LMWCNTs adsorbents andtheir adsorption ratesfor various pesticides were discussed.The mass spectrometry parameters of 26 kinds of pesticide residues were optimized,and matrix external standard method was adopted to quantify.The results showed that the correlation coefficients of 26 kinds of pesticides in chicken were 0.9992~1.00 in the range of 0.005~0.1μg/mL,and the limits of detection(LODS)were 0.032~3.3μg/kg,and the limits of quantification(LOQS)were 0.14~10μg/kg.The standard addition tests at three levels of 10μg/kg,20μg/kg and 100μg/kgwere conducted in chicken blank matrix,and the recoveries were 70.9%~106.7%,and the precision(n=7)was 1.3%~11.4%.The method was simple and rapid,and it had strong specificity and reliability,and the recovery and precision could meet the requirements of the residue limits of 26 kinds of pesticides in chicken.

关 键 词：QUECHERS 多壁碳纳米管 鸡肉 液相色谱-串联质谱 26种农药 农药残留 

分 类 号：O657.63[理学—分析化学] TS251.55[理学—化学]