磁性“一步法”-液相色谱-串联质谱法测定水产品中28种有机磷农药残留  

Determination of 28 Kinds of Organophosphorus Pesticide Residues in Aquatic Products by Magnetic"One-step"Method Combined with Liquid Chromatography-Tandem Mass Spectrometry

作　　者：金慧玲 刘真真[2] 范晓民 葛梦圆 王娇[2] 王新全 丁立建[1,3] 齐沛沛[1,2] JIN Hui-Ling;LIU Zhen-Zhen;FAN Xiao-Min;GE Meng-Yuan;WANG Jiao;WANG Xin-Quan;DING Li-Jin;QI Pei-Pei(State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products,School of Food Science and Engineering,Ningbo University,Ningbo 315211 China;State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products,Institute of Agro-product Safety and Nutrition,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China;Li Dak Sum Yip Yio Chin Kenneth Li Marine Biopharmaceutical Research Center,Health Science Center,Ningbo University,Ningbo 315211 China)

机构地区：[1]宁波大学食品科学与工程学院,省部共建农产品质量安全危害因子与风险防控国家重点实验室,宁波315211 [2]浙江省农业科学院农产品质量安全与营养研究所,省部共建农产品质量安全危害因子与风险防控国家重点实验室,杭州310021 [3]宁波大学医学部李达三海洋生物医药研究中心,宁波315211

出　　处：《分析化学》2024年第3期419-428,共10页Chinese Journal of Analytical Chemistry

基　　金：浙江省重点研发项目(Nos.2023C02038,2020C02023)资助。

摘　　要：基于磁性纳米材料建立了磁性“一步法”前处理技术,结合液相色谱-串联质谱(LC-MS/MS)方法,实现了水产品中28种有机磷农药残留的精准定量分析。针对水产品富含蛋白质、脂肪和脂肪酸的特点,选择磁性聚合物(聚二乙烯基苯-吡咯烷酮,Fe_(3)O_(4)-PLS)为净化剂,通过疏水作用、氢键和π-π键等相互协同作用高效吸附基质干扰组分,净化样品。优化了萃取溶剂类型及用量、盐析与除水剂、Fe_(3)O_(4)-PLS和C_(18)用量等实验条件。在最佳样品前处理条件下,28种有机磷农药的方法检出限(MLOD)为0.03~0.85μg/kg,方法定量限(MLOQ)为0.50~2.00μg/kg;不同添加浓度水平下目标物的平均回收率为60.1%~119.0%,相对标准偏差(RSDs)为0.8%~19.0%,方法的灵敏度和准确度高。与QuEChERS方法对比,本方法在萃取溶剂、盐析与除水剂和净化剂用量以及分析效率等方面均展现出明显的优势。采用本方法检测不同种类水产品中有机磷农药残留,结果表明,本方法具有良好的实用性,可为水产品中有机磷农药残留的快速分析提供新的方法依据。A magnetic"one-step"pretreatment technique was established based on magnetic functional materials and combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS)to achieve accurate quantitative analysis of 28 kinds of organophosphorus pesticide residues in aquatic products.Aquatic products had complex matrices that composed of a large amount of fats,fatty acids,and proteins,therefore,the amphiphilic magnetic functional material Fe_(3)O_(4)-PLS was selected as the clean-up adsorbent,which could effectively remove interfering components from aquatic products matrix through hydrophobic interactions,hydrogen bonds,and-t interactions.The main factors affecting accurate quantitative analysis in the extraction and purification procedure,such as the type of extraction solution,the dosage of salting out and dehydrating reagents,Fe_(3)O_(4)-PLS and C_(18) were systematically investigated respectively.Ultimately,the sample was extracted by 1.5 mL water and 3.5 mL acetonitrile with 2%acetic acid,then 2 g NaCl and anhydrous MgSO_(4)(1:4,m/m),40 mg Fe_(3)O_(4)-PLS and 10 mg C_(18) were added into the above centrifuge tube.Under the optimum conditions,the method limits of detection(MLOD)of 28 kinds of organophosphorus pesticides were 0.03-0.85μg/kg,and the method limits of quantitative(MLOQ)were 0.50-2.00μg/kg.Under different spiked concentration levels,the recoveries of target analytes ranged from 60.1%to 119.0%and RSDs were 0.8%-19.0%,which indicated that the magnetic"one-step"method had satisfactory sensitivity and recoveries.Compared to the QuEChERS method with non-magnetic material as cleanup adsorbent,the present method had obvious advantages in operation convenience,efficiency operation and the dosage of extraction solution,salting out and dehydrating reagents and purification adsorbents.In addition,the applicability of the developed method for analysis of organophosphorus pesticide residues in different kinds of aquatic products was validated.It was found to be suitable for the analysis of organophosphorus

关 键 词：Fe_(3)O_(4)-PLS 磁性“一步法” 液相色谱-串联质谱 水产品 有机磷农药 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]