LC-ICP-MS法同时测定富硒大米中有机硒和无机砷  

Simultaneous determination of organic selenium and inorganic arsenic in selenium rich rice by LC-ICP-MS method

作　　者：苏莹 林津 冯灏 李越 郭青青 周陶鸿 SU Ying;LIN Jin;FENG Hao;LI Yue;GUO Qing-qing;ZHOU Tao-hong(Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal Derived Food for State Market Regulation/Hubei Engineering Technology Research Center for Food Quality and Safety Testing/Hubei Shizhen Laboratory,Hubei Provincial Institute for Food Supervision and Test,Wuhan 430075,China)

机构地区：[1]湖北省食品质量安全监督检验研究院/国家市场监管重点实验室/动物源性食品中重点化学危害物检测技术/湖北省食品质量安全检测工程技术研究中心/湖北时珍实验室,武汉430075

出　　处：《湖北农业科学》2024年第9期191-195,共5页Hubei Agricultural Sciences

基　　金：湖北省重点研发计划项目(2022BBA0077);湖北省市场监督管理局科技计划专项(Hbscjg-KJ2023005)。

摘　　要：采用液相色谱-电感耦合等离子体质谱(LC-ICP-MS)技术,建立富硒大米中有机硒和无机砷同时检测的方法,用于检测湖北省市售富硒大米中有机硒和无机砷的含量。富硒大米前处理方法选用15 mg蛋白酶E和15 mg蛋白酶K混合提取,色谱条件采用Aglient ZORBAX SB-Aq色谱柱,流动相为20 mmol/L柠檬酸溶液+5 mmol/L己烷磺酸钠溶液+1%甲醇溶液(pH=4.0),1 mL/min流速进样,质谱采用HEHe模式,可在5 min内完全分离出3种有机硒和2种无机砷。3种有机硒和2种无机砷在1~50μg/L范围内具有良好的线性关系,相关系数(R2)均大于0.9990,As(Ⅴ)、As(Ⅲ)、SeCys2、MeSeCys、SeMet的检出限分别为0.10、0.12、0.18、0.15、0.15μg/L,满足检测要求。无机砷的回收率为96.2%~101.3%,相对标准偏差为2.5%~3.9%,有机硒的回收率为72.4%~100.6%,相对标准偏差为2.1%~4.1%。该方法操作简便、快速、灵敏度高,可用于富硒大米中有机硒和无机砷的同时检测。Using liquid chromatography inductively coupled plasma mass spectrometry(LC-ICP-MS)technology,a method for simul-taneous detection of organic selenium and inorganic arsenic in selenium-rich rice had been established,which was used to detect the content of organic selenium and inorganic arsenic in selenium-rich rice sold in Hubei Province.The pre-treatment method for seleni-um rich rice involved the mixed extraction by using of 15 mg proteinase E and 15 mg proteinase K,the chromatographic conditions were performed using an AgClient ZORBAX SB Aq column,and the mobile phase consistd of a 20 mmol/L citric acid solution,a 5 mmol/L sodium hexane sulfonate solution,and a 1%methanol solution(pH=4.0).Sample in jection was conducted at a flow rate of 1 mL/min,mass spectrometry used HEHe mode,and three types of organic selenium and two types of inorganic arsenic were separated completely within 5 minutes.The three types of organic selenium and two types of inorganic arsenic showed a good linear relationship ranging from 1 to 50μg/L,with correlation coefficients(R2)greater than 0.9990;the detection limits of As(Ⅴ),As(Ⅲ),SeCys2,MeSeCys,and SeMet were 0.10,0.12,0.18,0.15,and 0.15μg/L,respectively,which met the detection requirements.The recovery rate of inorganic arsenic was 96.2%~101.3%,with a relative standard deviation of 2.5%~3.9%;the recovery rate of organic selenium was 72.4%~100.6%,with a relative standard deviation of 2.1%~4.1%.This method was easy to operate,fast,and highly sensitive,and could be used for simultaneous detection of organic selenium and inorganic arsenic in selenium rich rice.

关 键 词：富硒大米 有机硒 无机砷 LC-ICP-MS法 

分 类 号：TS207.3[轻工技术与工程—食品科学]