| 富硒堇叶碎米荠中硒化合物的形态分析与鉴定 |
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| 基金项目:国家自然科学基金面上项目（32172197）；食品科学与技术国家重点实验室自主科研课题（SKLF－ZZA－202106） |
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| 中文摘要:该文以富硒堇叶碎米荠为研究对象，通过酶解法提取其中的硒化合物，采用高效液相色谱－电感耦合等离子质谱（HPLC－ICP－MS）定量分析已知的硒化合物；对于未知的硒化合物，将酶解液经3 kDa超滤离心管浓缩除杂、冻干后，用初始流动相复溶，选取Kinetex F5超高效液相五氟苯基柱（100 mm × 2.1 mm，2.6 μm），以0.1%（体积分数）甲酸－水溶液和0.1%（体积分数）甲酸－乙腈溶液为流动相进行梯度洗脱，通过超高效液相色谱－电喷雾电离源高分辨串联质谱（UPLC－ESI－Triple TOF MS），利用硒独特的同位素模式、一级质谱（TOF MS）和二级质谱（TOF MS/MS）进行筛选与鉴定。结果表明：HPLC－ICP－MS定量分析了堇叶碎米荠中的5种硒化合物，分别为硒代胱氨酸（SeCys2）、甲基硒代半胱氨酸（MeSeCys）、硒代蛋氨酸（SeMet）、四价硒［Se（Ⅳ）］、六价硒［Se（Ⅵ）］；UPLC－ESI－Triple TOF MS鉴定了其他15种硒化合物，包括7种已报道和8种未报道的硒化合物，并提出了C4H7NO2Se、C5H8O2Se和C7H9NO2Se 3种未报道硒化合物的结构。 |
| 中文关键词:富硒堇叶碎米荠 硒化合物 HPLC－ICP－MS UPLC－ESI－Triple TOF MS 鉴定 |
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| Detection and Identification of Selenium Compounds in Selenium-enriched Cardamine Violifolia |
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| Abstract:In this article，selenium（Se） compounds were extracted from Se-enriched Cardamine Violifolia（C. Violifolia） by enzymolysis method，and the known Se species were determined by high performance liquid chromatography－inductively coupled plasma mass spectrometry（HPLC－ICP－MS）．As for the identification of unkown Se compounds，the enzymatic hydrolysate was firstly concentrated by removing impurities with a 3 kDa ultrafiltration centrifuge tube，then freeze－dried，and finally suspended in the initial mobile phase．A Kinetex F5 column（100 mm × 2.1 mm，2.6 μm） was selected for gradient elution．Mobile phases A and B were water and acetonitrile both prepared with 0.1%（volume fraction） formic acid．The unknown Se compounds were screened and identified by ultrahigh performance liquid chromatography－electrospray ionization high resolution tandem mass spectrometry（UPLC－ESI－Triple TOF MS）using unique isotope patterns，TOF MS and TOF MS/MS．The results showed that five Se species in C. Violifolia were determined by HPLC－ICP－MS，namely selenocysteine（SeCys2），methylselenocysteine（MeSeCys），selenomethionine（SeMet），selenite［Se（Ⅳ）］ and selenate［Se（Ⅵ）］．15 other Se compounds，including 7 reported and 8 unreported Se compounds，were identified by UPLC－ESI－Triple TOF MS．The structural formula of three unreported Se compounds，C4H7NO2Se，C5H8O2Se and C7H9NO2Se were proposed. |
| Key Words:selenium-enriched Cardamine Violifolia selenium compounds HPLC－ICP－MS UPLC－ESI－Triple TOF MS identification |
| 引用本文：叶梅,虞锐鹏,丛欣,陈尚卫,朱松.富硒堇叶碎米荠中硒化合物的形态分析与鉴定[J].分析测试学报,2022,41(1):100-107. |
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