扇贝组织中不同形态氨基脲测定方法研究  

Determination method of the semicarbazide existing form in scallop

作　　者：邢丽红[1,2,3] 孙伟红 朱盼盼[1,2,3] 孙晓杰 李兆新 XING Li-hong;SUN Wei-hong;ZHU Pan-pan;SUN Xiao-jie;LI Zhao-xin(Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality,Ministry of Agriculture and Rural Affairs,China,Yellow Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Qingdao 266071,China;Pilot National Laboratory for Marine Science and Technology,Qingdao 266003,China;Collaborative Innovation Center of Seafood Deep Processing,Dalian Polytechnic University,Dalian 116034,China)

机构地区：[1]中国水产科学研究院,黄海水产研究所,农业农村部水产品质量安全检测与评价重点实验室,山东青岛266071 [2]青岛海洋科学与技术试点国家实验室,山东青岛266033 [3]大连工业大学,海洋食品精深加工关键技术省部共建协同创新中心,辽宁大连116034

出　　处：《海洋科学》2022年第6期70-79,共10页Marine Sciences

基　　金：国家自然科学基金项目(41806148);浙江省近岸水域生物资源开发与保护重点实验室、温州市海洋生物遗传育种重点实验室联合开放基金(J2021003);中国水产科学研究院基本科研业务费(2020TD71)。

摘　　要：为明确环境新型污染物--氨基脲(semicarbazide,SEM)在贝类体内的存在形态,本文建立了一种SEM在扇贝中形态测定的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry,LC-MS/MS)分析方法。扇贝中SEM总量测定方法为:样品用盐酸水解,以2-硝基苯甲醛为衍生剂衍生,乙酸乙酯提取,超滤离心净化,进LC-MS/MS分析。结合态SEM测定方法为:样品分别采用50%甲醇水溶液、75%甲醇水溶液、甲醇和水洗涤后,按照SEM总量测定方法处理,采用甲醇和2 mmol/L乙酸铵作为流动相进行梯度洗脱,电喷雾离子源正离子(electrosprary ionization,ESI+)选择反应监测模式对SEM进行定性和定量测定。本方法在1~20μg/L范围内线性关系良好,相关系数大于0.999。SEM在1.00、5.00、10.0μg/kg添加水平的回收率在84.2%~118%,相对标准偏差均<15%。本方法扇贝中SEM的定量限为1.0μg/kg,本方法灵敏、准确、操作简便,适用于扇贝中SEM存在形态的测定。In order to clarify the existing form of a new environmental pollutant semicarbazide(SEM)in shellfish,a liquid chromatography–tandem mass spectrometry(LC–MS/MS)method was developed to determine the existing form of the environmental pollutant semicarbazide(SEM)in scallop.The total SEM in scallop was determined as follows:After hydrolysis by hydrochloric acid,the sample was derivatized by 2-nitrobenzaldehyde overnight for 16 hours.Then,SEM was extracted with ethyl acetate,purified by ultrafiltration,and analyzed using LC–MS/MS.The tissue-bound SEM was separately washed with methanol/water(50:50;v/v),followed by methanol/water(75:25;v/v),methanol,and water.Then,the sample was determined as the method of the total SEM.The SEM residue in the extract was separated on a reversed phase using a gradient elution program of methanol and 2 mmol/L ammo-nium acetate.Using LC–MS/MS(electrospray ionization,ESI+)with selected reaction monitoring,identification of the major components of the SEM residue was performed based on the fragment intensities.The calibration curve showed good linearity from 0.5–20μg/L,with a correlation coefficient over 0.999.The recoveries ranged from 84.2%to 118%for the SEM residues,with 3 spiked levels at 1.00,5.00,and 10.0μg/kg.The relative standard de-viations were less than 15%,and the limit of quantitation for the SEM in scallop tissue was 1.0μg/kg.The proposed method is sensitive,accurate,and easy to operate,which is suitable for determining the existing form of SEM in scallop.

关 键 词：氨基脲 液相色谱-串联质谱法 扇贝 存在形态 

分 类 号：S912[农业科学—水产科学]