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建立了高效液相色谱-动态反应池-电感耦合等离子体质谱(HPLC-DRC-ICP-MS)联用测定硒代胱氨酸(SeCys2)、甲基硒代半光氨酸(MeSeCys)、亚硒酸盐(SeIV)、硒代蛋氨酸(SeMet)和硒酸盐(SeVI)的方法。样品通过胃蛋白酶提取,采用Hamilton PRP X-100色谱柱(250 mm×4.6 mm,10μm),使用5 mmol/L的柠檬酸溶液(pH 4.7)作为流动相,在10 min内可以完全分离5种硒形态。在80Se质量数下,采用甲烷作为DRC反应气,可有效消除40Ar40Ar+对80Se的干扰,提高检测灵敏度。电感耦合等离子体质谱(ICP-MS)检测,各硒形态的线性相关系数均大于0.9990,Se(IV)、Se(VI)、SeMet、SeCys2、MeSeCys的定量限分别为5,10,10,5,5μg/kg,5种硒形态的加标回收率在80.1%～99.2%之间,可满足蔬菜中硒形态定量分析。
A high performance liquid chromatography-dynamic response cell-inductively coupled plasma mass spectrometry (HPLC-DRC-ICP-MS) was developed for the determination of SeCys2, MeSeCys, Selenate (SeIV), selenomethionine (SeMet) and selenate (SeVI). The samples were isolated by pepsin and completely separated in 10 min using Hamilton PRP X-100 column (250 mm × 4.6 mm, 10 μm) and 5 mmol / L citric acid solution (pH 4.7) as the mobile phase Selenium form. Under the mass of 80Se, using methane as the DRC reagent gas can effectively eliminate the interference of 40Ar40Ar + to 80Se and improve the detection sensitivity. The linear correlation coefficients of Selenium and Se (IV), Se (VI), SeMet, SeCys2 and MeSeCys were 5, 10, 10 and 5 respectively by inductively coupled plasma mass spectrometry (ICP-MS) , 5μg / kg. The spiked recoveries of five selenium forms ranged from 80.1% to 99.2%, which could meet the quantitative analysis of selenium in vegetables.