分析化学2024，Vol.52Issue(3)：419-428,中插50-中插60,21.DOI:10.19756/j.issn.0253-3820.231313
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
摘要
Abstract
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 Fe3O4-PLS was selected as the clean-up adsorbent,which could effectively remove interfering components from aquatic products matrix through hydrophobic interactions,hydrogen bonds,and π-π 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,Fe3O4-PLS and C18 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 MgSO4(1∶4,m/m),40 mg Fe3O4-PLS and 10 mg C18 were added into the above centrifuge tube.Under the optimum conditions,the method limits of detection(MLOD)of 28 kinds of organophosphorus pesticides were 0.03-0.85 μg/kg,and the method limits of quantitative(MLOQ)were 0.50-2.00 μg/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 pesticide residues in different types of aquatic products.关键词
Fe3O4-PLS/磁性"一步法"/液相色谱-串联质谱/水产品/有机磷农药Key words
Fe3O4-PLS/Magnetic"one-step"method/Liquid chromatography-tandem mass spectrometry/Aquatic products/Organophosphorus pesticide引用本文复制引用
金慧玲,刘真真,范晓民,葛梦圆,王娇,王新全,丁立建,齐沛沛..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[J].分析化学,2024,52(3):419-428,中插50-中插60,21.基金项目
浙江省重点研发项目(Nos.2023C02038,2020C02023)资助. Suppoted by the Key Research and Development Program of Zhejiang Province,China(Nos.2023C02038,2020C02023). （Nos.2023C02038,2020C02023）
