氧化还原一步法测定饲料中总硒含量  

Determination of total selenium in feed via one-step redox reaction

作　　者：曹进平 程远之 刘鑫 汪以真[1] 王凤芹[1] CAO Jin-ping;CHENG Yuan-zhi;LIU Xin;WANG Yi-zhen;WANG Feng-qin

机构地区：[1]浙江大学动物科学学院生物饲料安全与污染防控国家工程实验室农业农村部(华东)动物营养与饲料重点实验室浙江省饲料与动物营养重点实验室教育部动物分子营养重点实验室,浙江杭州310058

出　　处：《饲料研究》2021年第15期96-100,共5页Feed Research

基　　金：浙江省基础公益研究计划(项目编号:LGC20C170001);现代农业生猪产业体系(项目编号:CARS-35)。

摘　　要：试验旨在建立过氧化氢-盐酸氧化还原一步法消解饲料样品,利用高效液相质谱-电感耦合等离子体质谱联用仪(HPLC-ICP-MS)测定饲料中总硒含量的方法。饲料样品中加入过氧化氢和盐酸在水浴1 h,进行氧化还原一步消解,SeO_(3)^(2-)定容,采用HPLC-ICP-MS测定硒的含量。样品经C18色谱柱分离,磷酸二氢钾水溶液-七氟丁酸和甲醇体系等度洗脱,ICP-MS在KED模式分析^(78)Se,外标法定量测定样品中的总硒。结果表明:试验所建立的方法的线性方程中R^(2)大于0.9900,硒的检出限为0.17μg/g,定量限为0.57μg/g,且峰面积与保留时间的相对标准偏差均低于3%。采用该方法测得2批富硒多糖饲料样品中总硒的含量分别为1118.00、1402.06μg/g,富硒酵母中总硒的含量为941.13μg/g,预混合饲料中总硒的含量为0.95μg/g。除预混合饲料外,采用该方法测定不同饲料样品的相对标准偏差均小于10%。与传统测定总硒采用HNO3-HClO4混合酸体系消解样品,再用盐酸进一步还原的前处理过程相比,该方法具有操作简单、样品转移少、反应快速、回收率高、安全环保、适用性强等特点。The purpose of the experiment was to establish a one-step redox reaction method by using hydrogen peroxide and hydrochloric acid to pretreat feed samples,and high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS)was adopted to determine the^(78)Se of samples.Hydrogen peroxide and hydrochloric acid were added in feed samples under water bath for 1 h to perform one-step redox digestion.The obtained SeO_(3)^(2-)volume was used to determine the content of selenium directly by HPLC-ICP-MS.The samples were separated by C18,the potassium dihydrogen phosphate aqueous solution-sevoflurane butyric acid and methanol system was isocratic elution.ICP-MS was used to analyze^(78)Se in KED mode,and the external standard method was used to quantify.The results showed that R2 of the linear equation was greater than 0.9900,the detection limit of selenium was 0.17μg/g and the quantification limit was 0.57μg/g,and the relative standard deviations of peak area and retention time were all less than 3%.The content of total selenium in the two batches of selenium-enriched polysaccharide feed samples was 1118.00,1402.06μg/g,the content of total selenium in selenium-enriched yeast was 941.13μg/g,and the content of total selenium in premixed feed was 0.95μg/g measured by the method.Except for the premixed feeds,the relative standard deviations of different feed samples determined by the method were less than 10%.Compared with the traditional pretreatment process of determining^(78)Se using HNO3-HClO4 system to digest samples,the method has the advantages of simple operation,less sample transfer,fast reaction,high recovery rate and well applicability.

关 键 词：氧化还原一步法 富硒饲料 HPLC-ICP-MS 总硒 

分 类 号：S816.17[农业科学—饲料科学]