基于改性多壁碳纳米管净化的高效液相色谱-三重四极杆/复合线性离子阱质谱测定南美白对虾中66种农药残留  

Determination of 66 pesticide residues in Litopenaeus vannameiby high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry based on modifiedmulti-wall carbon nanotube purification

作　　者：周锐东 文宇鹏 霍文迪 张超英 刘欢[2] 孙慧武[2] 吴立冬[2] 李晋成[2] ZHOU Ruidong;WEN Yupeng;HUO Wendi;ZHANG Chaoying;LIU Huan;SUN Huiwu;WU Lidong;LI Jincheng(College of Fisheries and Life Science,Shanghai Ocean University,Shanghai 201306,China;Key Laboratory of Control of Quality and Safety for Aquatic Products,Ministry of Agriculture and Rural Affairs,Chinese Academy of Fishery Sciences,Beijing 100141,China;School of New Materials and Chemical Engineering,Beijing Institute of Petrochemical Technology,Beijing 102617,China)

机构地区：[1]上海海洋大学水产与生命学院,上海201306 [2]中国水产科学研究院农业农村部水产品质量安全控制重点实验室,北京100141 [3]北京石油化工学院新材料与化工学院,北京102617

出　　处：《色谱》2024年第12期1136-1144,共9页Chinese Journal of Chromatography

基　　金：中国水产科学研究院基本科研业务基金(2024A001);中国水产科学研究院科技创新项目(2020TD75);现代农业产业技术体系建设专项资金(CARS-48)~~。

摘　　要：针对水产品农药残留分析过程中基质干扰强的现状,本研究利用多壁碳纳米管(MWCNTs)和海藻酸钠(SAL)制备了一种MWCNTs-SAL复合净化材料,建立了高效液相色谱-三重四极杆/复合线性离子阱质谱(HPLC-QTRAP-MS/MS)快速测定水产品中66种农药残留的分析方法。采用电喷雾装置将MWCNTs和SAL的复合溶液快速喷入CaCl2溶液中进行交联,制备MWCNTs-SAL复合材料。将乙腈作为提取溶剂,基于推杆式震荡型净化技术对提取液进行净化。采用C18RRHD色谱柱(150 mm×3.0 mm, 1.8μm)对目标化合物进行分离,在多反应监测(MRM)模式下采集质谱数据,使用基质匹配混合标准溶液进行定量分析。实验比较了MWCNTs-SAL填料与商品化填料对南美白对虾提取液的净化效果,并考察了MWCNTs-SAL用量对目标化合物净化效果的影响。实验结果表明,66种农药在0.5~50μg/L内线性关系良好,相关系数均>0.99,检出限和定量限分别为0.5~1μg/kg和1~2μg/kg;在低、中、高3个加标水平下,66种目标化合物的回收率为64.1%~107.3%,日内和日间精密度均小于20.4%。该方法经济快速,简便高效,具有较高的灵敏度和重复性,是水产品中农药残留分析的可行方法。The complex composition of aquatic products,with high levels of protein and fat,significantly impacts the accuracy of liquid chromatography-mass spectrometry analysis for pesticide residue detection.Hence,developing effective purification materials is essential to mitigate these matrix interferences.To address strong matrix interference in pesticide residue analysis,a composite material,multi-walled carbon nanotubes(MWCNTs)-sodium alginate(SAL)(MWCNTs-SAL),was developed and used as purification material in a push-rod oscillation purification column to establish a rapid method for analyzing 66 pesticide residues in Litopenaeus vannamei.The composite solution of MWCNTs and SAL was quickly sprayed into CaCl 2 solution by electrospray device for crosslinking,and MWCNTs-SAL materials were prepared.The results of scanning electron microscopy image proved the successful preparation of the MWCNTs-SAL.Acetonitrile,as the extraction solvent,was modified with acetic acid to augment the extraction efficiency of acidic pesticides,and anhydrous sodium sulfate was utilized to remove water from the matrix.Push-rod oscillation purification technology was used for purification of the post-centrifugation extract.The target compounds were separated using C 18 RRHD column(150 mm×3.0 mm,1.8μm)and the mobile phases were consisted of 0.2%formic acid aqueous solution(containing 5 mmol/L ammonium acetate)and 0.2%formic acid methanol.The high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry(HPLC-QTRAP-MS/MS)was used for separation and determination,and the data was collected through the multiple reaction monitoring(MRM)mode.Due to the different properties of the target compounds,positive and negative ion acquisition scan modes were employed for mass spectrometry analysis.The quantitative analyses of the 66 pesticides were achieved by matrix-matched standard curves.The purification effects of MWCNTs-SAL and commercial sorbents on the extraction of the 66 pesticides were compared.The pretreatment parame

关 键 词：多壁碳纳米管 高效液相色谱-三重四极杆/复合线性离子阱质谱 水产品 农药残留 

分 类 号：O658[理学—分析化学]