鱼露中砷形态分析  

Speciation analysis of arsenic in fish sauce

作　　者：陈镇 陈绍占 姚晓慧 刘洋[1,3] 刘丽萍 CHEN Zhen;CHEN Shaozhan;YAO Xiaohui;LIU Yang;LIU Liping(Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing Center for Disease Prevention and Control,Beijing 100013,China;Pinggu Center for Disease Prevention and Control,Beijing 101200,China;Beijing Center for Preventive Medicine Research,Beijing 100013,China)

机构地区：[1]北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室,北京100013 [2]北京市平谷区疾病预防控制中心,北京101200 [3]北京市预防医学研究中心,北京100013

出　　处：《分析试验室》2022年第5期576-582,共7页Chinese Journal of Analysis Laboratory

摘　　要：采用高效液相色谱-电感耦合等离子体质谱(HPLC-ICP/MS)联用技术对鱼露样品中砷形态进行分析。鱼露样品采用含0.45%H_(2)O_(2)的1%HNO_(3)溶液90℃热浸提3 h,8000 r/min离心过滤后,采用Hamilton PRP-X100阴离子交换柱(250 mm×4.1 mm,10μm),以(NH_(4))_(2)HPO_(4)溶液为流动相,梯度洗脱,HPLC-ICP/MS法进行分析。结果显示,在前处理过程中添加H_(2)O_(2)可准确测定鱼露样品中一甲基砷(MMA)和无机砷(iAs)的含量;同时发现氧化后砷甜菜碱(AsB)高的鱼露基质样品中少量的AsB会转化为未知砷形态,影响二甲基砷(DMA)的准确测定。The speciation of arsenic in fish sauce samples was analysized by high-performance liquid chromatography inductively coupled plasma mass spectrometry(HPLC-ICP/MS).The fish sauce sample was hot extracted with 1%nitric acid solution containing 0.45%hydrogen peroxide at 90℃for 3 h,centrifuged at 8000 r/min,and then analysized by HPLC-ICP/MS using Hamilton PRP-X100 anion exchange column(250 mm×4.1 mm,10μm)and diammonium hydrogen phosphate solution as mobile phase for gradient elution.Adding hydrogen peroxide in the pretreatment process could accurately determine the contents of methylarsenic and inorganic arsenic in fish sauce samples.At the same time,it was found that a small amount of arsenicbetaine in fish sauce matrix samples with high arsenicbetaine after oxidation would be transformed into unknown arsenic form,which would affect the accurate determination of dimethyl arsenic.

关 键 词：液相色谱电感耦合等离子体质谱(HPLC-ICP/MS) 砷形态 鱼露 

分 类 号：R155[医药卫生—营养与食品卫生学]