Division of Chemical Metrology and Analytical Science, National Institute of Metrology, No. 18 Beisanhuan Donglu, Chaoyang Dist., Beijing 100029, China; Key Laboratory of Chemical Metrology and Applications on Nutrition and Health for State Market Regulation, No. 18 Beisanhuan Donglu, Chaoyang Dist., Beijing 100029, China.
Division of Chemical Metrology and Analytical Science, National Institute of Metrology, No. 18 Beisanhuan Donglu, Chaoyang Dist., Beijing 100029, China; Key Laboratory of Chemical Metrology and Applications on Nutrition and Health for State Market Regulation, No. 18 Beisanhuan Donglu, Chaoyang Dist., Beijing 100029, China.
J Chromatogr A. 2022 Jul 5;1674:463134. doi: 10.1016/j.chroma.2022.463134. Epub 2022 May 12.
An enzyme-assisted extraction and an ion pairing reversed phase chromatography (IP-RPC) coupled to inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) method were established for the simultaneous analysis of five selenium species in rice: selenious acid (SeIV), selenic acid (SeVI), selenocystine (SeCys), methylselenocysteine (SeMeCys) and selenomethionine (SeMet). Optimal extraction efficiencies were obtained by using 15 mg protease XIV, water bath temperature of 45°C, pH of 6.5 and incubation of six hours. The total extracted Se species account for 92.5-109.3 % of the total Se in rice. The instrumental limits of detection for five selenium species ranged from 0.04 to 0.12 ng Se g. Spike recovery experiments performed on rice samples were in the range of 96.1-102.9 % for all analytes except for SeCys (66.1-77.1 %). A consistency of Se elemental response was observed among Se species analyzed in this study as the ratio of linear equation slope ranged from 1.020 to 1.036 (SeIV as reference) in rice matrix. The developed compound-independent calibration method was applied to detect Se species in eleven rice samples from China. Both selenium-enriched rice and regular rice were predominated with SeMet, accounting for ∼89.4 % of total selenium.
建立了一种酶辅助提取和离子对反相色谱(IP-RPC)与电感耦合等离子体质谱串联质谱(ICP-MS/MS)联用的方法,用于同时分析大米中的五种硒形态:亚硒酸(SeIV)、硒酸(SeVI)、硒代半胱氨酸(SeCys)、甲基硒代半胱氨酸(SeMeCys)和硒代蛋氨酸(SeMet)。通过使用 15mg 蛋白酶 XIV、45°C 水浴温度、pH 值为 6.5 和孵育 6 小时,可获得最佳的提取效率。总提取的硒形态占大米中总硒的 92.5-109.3%。五种硒形态的仪器检出限范围为 0.04-0.12ng Se g。在大米样品中进行的加标回收实验,所有分析物的回收率均在 96.1-102.9%之间,除了 SeCys(66.1-77.1%)。在本研究中分析的硒形态中观察到硒元素响应的一致性,因为在大米基质中线性方程斜率的比值范围为 1.020-1.036(以 SeIV 为参考)。开发的无化合物依赖的校准方法应用于检测来自中国的 11 个大米样品中的硒形态。富硒大米和普通大米均以 SeMet 为主,占总硒的约 89.4%。