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本文研究建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用检测转基因大豆中的硒酸盐(Se VI)、亚硒酸盐(Se IV)、硒代蛋氨酸(selenomethionine,Se Met)、硒代胱氨酸(selenocystine,Se Cys2)和硒代乙硫氨酸(selenoethionine,Se Et)的方法。探讨了色谱柱、流动相及其酸度对分离效果的影响,使用10 mmol/L的柠檬酸溶液(p H值4.5)作流动相,Hamilton PRP X-100色谱柱分离,碰撞反应池技术消除40Ar40Ar+和40Ar2H2+等多原子离子干扰,ICP-MS检测82Se同位素,在21 min内可完全分离检测5种硒形态。探讨了不同提取方法的提取效果,优化了提取条件,采用蛋白酶提取,针对美国进口的转基因大豆样品进行加标回收实验,结果表明采用蛋白酶提取,Se IV和Se VI的回收率在100%左右,Se Met的回收率在92.6%~109.3%之间,Se Cys2和Se Et的回收率为81.2%~95.9%。该方法可完全满足转基因大豆中的硒形态定量分析鉴定。
In this paper, a high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was developed to detect selenomethionine (Se IV), selenomethionine , Se Met), selenocystine (Se Cys2) and selenoethionine (Se Et). The effect of column, mobile phase and acidity on the separation was discussed. The mobile phase was eluted with 10 mmol / L citric acid solution (pH 4.5) as the mobile phase. The collision cell technology was used to eliminate 40Ar40Ar + And 40Ar2H2 + and other polyatomic ions, ICP-MS detection 82 Se isotope, within 21 min can be completely separated and detected five kinds of selenium form. The extraction efficiency of different extraction methods was explored. The extraction conditions were optimized. Protease extraction was used to recover the transgenic soybeans imported from the United States. The results showed that the recoveries of Se IV and Se VI were about 100% Se Met recoveries ranged from 92.6% to 109.3%, Se Cys2 and Se Et recoveries ranged from 81.2% to 95.9%. This method can fully meet the quantitative analysis of selenium in transgenic soybean identification.