湖北农业科学 ›› 2024, Vol. 63 ›› Issue (9): 191-195.doi: 10.14088/j.cnki.issn0439-8114.2024.09.032

• 检测分析 • 上一篇    下一篇

LC-ICP-MS法同时测定富硒大米中有机硒和无机砷

苏莹, 林津, 冯灏, 李越, 郭青青, 周陶鸿   

  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
  • 收稿日期:2023-10-13 出版日期:2024-09-25 发布日期:2024-09-30
  • 通讯作者: 林 津(1988-),女,湖北武汉人,高级工程师,硕士,主要从事食品质量与安全研究,(电子信箱)524153439@qq.com。
  • 作者简介:苏 莹(1997-),女,湖北荆门人,助理工程师,硕士,主要从事食品质量与安全研究,(电话)13774067369(电子信箱)513278616@qq.com。
  • 基金资助:
    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)

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

SU Ying, LIN Jin, FENG Hao, LI Yue, GUO Qing-qing, ZHOU Tao-hong   

  1. 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
  • Received:2023-10-13 Published:2024-09-25 Online:2024-09-30

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1~50 μg/L范围内具有良好的线性关系,相关系数(R2)均大于0.999 0,As(Ⅴ)、As(Ⅲ)、SeCys2、MeSeCys、SeMet的检出限分别为0.10、0.12、0.18、0.15、0.15 μg/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。

关键词: 富硒大米, 有机硒, 无机砷, LC-ICP-MS法

Abstract: Using liquid chromatography inductively coupled plasma mass spectrometry (LC-ICP-MS) technology,a method for simultaneous 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 selenium 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 50 μg/L, with correlation coefficients (R2) greater than 0.999 0;the detection limits of As (Ⅴ), As (Ⅲ), SeCys2, MeSeCys, and SeMet were 0.10, 0.12, 0.18, 0.15, and 0.15 μg/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.

Key words: selenium rich rice, organic selenium, inorganic arsenic, LC-ICP-MS method

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