高效液相色谱-串联质谱同位素内标法测定水产品中19种磺胺类药物及其2种增效剂  

Determination of 19 Sulfonamides and 2 Sulfonamide Synergist Residues in Aquatic Products by HPLC-MS/MS

作　　者：吴燕 孙晓杰[2] 邢丽红[2] 穆阿丽 初晓娜 林存壮 王绅 付红蕾 李兆新[2] WU Yan;SUN Xiaojie;XING Lihong;MU Ali;CHU Xiaona;LIN Cunzhuang;WANG Shen;FU Honglei;LI Zhaoxin(Qingdao Agricultural Products Quality and Safety Center,Qingdao 266100;Yellow Sea fisheries Research Insttute,Qingdao 266100)

机构地区：[1]青岛市农产品质量安全中心,山东青岛266000 [2]中国水产科学研究院黄海水产研究所,山东青岛266100

出　　处：《分析科学学报》2024年第6期662-668,共7页Journal of Analytical Science

基　　金：山东省自然科学基金项目(ZR2023MD109);中国水产科学研究院黄海水产研究所基本科研业务费项目(20603022024004);中国水产科学研究院基本科研业务费项目(2023TD76);国家重点研发计划“蓝色粮仓科技创新”重点专项(2019YFD0901701);农业农村部标准制修订项目(2016-58)。

摘　　要：建立了一种基于固相萃取技术,采用同位素内标法同时测定水产品中19种磺胺类药物及其2种增效剂残留的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。分别考察了不同提取条件、净化条件和色谱条件对实验结果的影响。样品经乙腈提取,MCX固相萃取柱净化,采用电喷雾离子源正离子模式多反应监测(MRM)进行定性定量分析。结果表明,21种磺胺类药物的检出限为1.0μg/kg,定量限为2.0μg/kg,相对标准偏差(n=6)为2.45%~13.9%,考察了鲤鱼、对虾、海参、甲鱼等4种基质条件下的加标回收实验,加标回收率介于67.8%~115%之间。该方法具有适用范围广、灵敏度高、重复性好等特点,可广泛应用于水产品中多种磺胺类药物及其增效剂的残留测定。A high-performance liquid chromatography-tandem mass spectrometry method(HPLC-MS/MS)with solid phase extraction was established for the simultaneous determination of 19 sulfonamides residues and 2 synergists in fisheries products using isotope internal standard for quantification.The effects of different pre-treatment conditions,purification conditions,and chromatographic conditions on the experimental results were investigated.The samples were extracted with acetonitrile,purified by MCX solid-phase extraction column and determined by LC-MS/MS selective multiple reaction monitoring with positive ion mode for qualitative and quantitative analysis.The results showed that the detection limits and quantification limits of 21 sulfonamides were 1.0μg/kg and 2.0μg/kg,respectively.The relative standard deviations were between 2.45%-13.9%(n=6)and the recoveries were between 67.8%-115%.This method was validated by using four substrates,including carp,shrimp,sea cucumber,and turtle.It has the characteristics of wide applicability,high sensitivity,and good repeatability,and can be applied to the residual determination of various sulfonamide and their synergist in aquatic products.

关 键 词：高效液相色谱-串联质谱法 水产品 磺胺类药物 增效剂 

分 类 号：O657.63[理学—分析化学]