Development of chiral HPLC for selenoamino acids with ICP-MS detection:application to selenium nutritional supplements.
Development of chiral HPLC for selenoamino acids with ICP-MS detection:application to selenium nutritional supplements.
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DOI：
10.1039/a907847i
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发表时间：
2000
期刊：
影响因子：
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通讯作者：
K. Sutton;C. A. Ponce de León;K. L. Ackley;R. Sutton;A. Stalcup;J. Caruso
中科院分区：
文献类型：
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作者：
K. Sutton;C. A. Ponce de León;K. L. Ackley;R. Sutton;A. Stalcup;J. Caruso
用紫外光谱和电感耦合等离子体质谱联用技术对D，L-硒半胱氨酸、D，L-硒蛋氨酸和D，L-硒蛋氨酸三种未衍生化的硒氨基酸进行了对映体分离。色谱柱为手性冠醚固定相，流动相为0.10M HCO4。紫外光检测的绝对检出限为34.5-47.1 ng，而等离子体检测器的绝对检出限为40-400倍。两种检测器的分离度都很好，检测器对分辨率的影响很小。使用手性色谱柱对10种市售硒补充剂进行了分析，以鉴定和定量两种检测模式下存在的硒物种。用电感耦合等离子体质谱检测可以很容易地确定硒的形态，而紫外检测由于样品基质的干扰和灵敏度不足而不可行。用阴离子交换层析对手性柱未保留的硒物种进行鉴定。样品中的总量也用常规消化和酶消化-电感耦合等离子体质谱检测来测量。
The enantiomeric separation of three underivatized seleno-amino acids, D,L-selenocystine, and D,L-selenomethionine, and D,L-selenomethionine, with UV and ICP-MS detection is described. An HPLC column with a chiral crown ether stationary phase and a mobile phase of 0.10 M HCIO4 was used. Absolute detection limits obtained with UV detection ranged from 34.5 to 47.1 ng whereas those obtained with the plasma detector were ca. 40-400 times better. The separations with either detector were good, with the little detector effect on the resolution. Ten commercially available dietary selenium supplements were analyzed using the chiral column to identify and quantify the selenium species present with both detection modes. Selenium species were easily identified using ICP-MS detection, whereas UV detection was not viable because of interferences from the sample matrix and inadequate sensitivity. Selenium species that were unretained using the chiral column were identified using anion exchange chromatography. Total amounts in the samples were also measured using a conventional digestion and enzymatic digestion with ICP-MS detection.