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建立了超声辅助酶法提取-高效液相色谱-电感耦合等离子体质谱联用同时测定食品中无机硒和硒氨基酸等6种硒形态的新方法。对影响硒形态分离及提取的诸因素如提取方式、流动相pH、浓度、甲醇含量、流速和柱温等进行详细考察和优化,同时利用碰撞反应池,有效地消除了复合离子的干扰,提高了检测灵敏度。该方法在9.50 min内使亚硒酸盐(Se(IV))、硒酸盐(Se(VI))、硒胱氨酸(SeCys_2)、硒蛋氨酸(SeMet)、甲基硒代半胱氨酸(MeSeCys)和硒代乙硫氨酸(SeEt)等6种目标分析物完全达到基线分离,各物质的检出限为(0.012~0.60)μg Se/L,线性范围达3~4个数量级,相对标准偏差(RSDs,n=7)为4.0%~8.2%;将该方法应用于食品中硒形态的分析,其加标回收率为81.6%~108.6%。方法具有操作简单方便、快速高效、灵敏度高和环境友好等优点,可满足食品中硒形态定量分析
A new method of simultaneous determination of six selenium forms, including inorganic selenium and selenoamino acid, in food by ultrasound-assisted enzymatic extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry was established. The influencing factors of selenium separation and extraction such as extraction method, mobile phase pH, concentration, methanol content, flow rate and column temperature were investigated in detail and optimized. At the same time, the collision reaction tank was used to effectively eliminate the interference of complex ions and improve The detection sensitivity. In this method, selenite (Se (IV)), selenate (Se (VI)), SeCys_2, SeMet, methylselenocysteine (MeSeCys) and selenothioethionine (SeEt). The detection limits of each substance were (0.012 ~ 0.60) μg Se / L, and the linear range was 3 ~ 4 orders of magnitude. The relative standard deviations (RSDs, n = 7) ranged from 4.0% to 8.2%. The method was applied to the analysis of selenium in foodstuff with the spiked recoveries of 81.6% -108.6%. The method has the advantages of simple and convenient operation, fast and high efficiency, high sensitivity and environmental friendliness, and can meet the quantitative analysis of selenium in food