采用加压和微波辅助酶解后高效液相色谱-电感耦合等离子体质谱法测定富硒土壤中收获的食物中的硒形态。

Selenium species determination in foods harvested in Seleniferous soils by HPLC-ICP-MS after enzymatic hydrolysis assisted by pressurization and microwave energy.

机构信息

Grupo Química Analítica Aplicada (QANAP), University of A Coruña, Department of Chemistry, Faculty of Sciences, Centro de Investigaciones Científicas Avanzadas (CICA), University Institute of Research in Environmental Studies (IUMA), Campus de A Coruña, s/n, A Coruña 15071, Spain.

出版信息

Food Res Int. 2018 Sep;111:621-630. doi: 10.1016/j.foodres.2018.06.003. Epub 2018 Jun 5.

DOI:10.1016/j.foodres.2018.06.003

PMID:30007726

Abstract

Fast, green, automated, highly efficient and accurate methodology for extracting selenium species in foods samples (Brazil nut, golden berries and heart of palm) harvested in seleniferous soils by using pressurized-assisted enzymatic hydrolysis (PAEH) and microwave-assisted enzymatic hydrolysis (MAEH) were optimized. After foods defatting or drying, selenium species were released using protease XIV and enzyme activator in 7 and 12 min for PAEH and MAEHmethods, respectively. Inductively coupled plasma - mass spectrometry (ICP-MS) and high performance liquid chromatography (HPLC) coupled with ICP-MS detection were used to assess total selenium and selenium species contents in the enzymatic extracts. Analytical performances, such as limits of quantification (0.032-0.599 μg g and 0.014-0.240 μg g for PAEH and MAEH, respectively), repeatability (11-14.5%) and accuracy of the over-all procedures were established. Selenomethionine (SeMet) were detected in all analyzed samples and selenocystine (SeCys) in Brazil nut; however, SeMet and SeCys levels were only quantified in Brazil nut. Inorganic selenium species were not detected in any sample. The presence of SeMet and SeCys and the absence of oxidized selenium methionine (SeOMet) in the enzymatic extracts were confirmed by Orbitrap mass spectrometry.

摘要

优化了一种快速、绿色、自动化、高效、准确的方法，用于从富硒土壤中收获的食物样品（巴西坚果、金果和棕榈心）中提取硒形态，方法是使用加压辅助酶解（PAEH）和微波辅助酶解（MAEH）。在对食物进行脱脂或干燥后，使用蛋白酶 XIV 和酶激活剂，分别在 7 和 12 分钟内释放 PAEH 和 MAEH 方法中的硒形态。电感耦合等离子体质谱（ICP-MS）和高效液相色谱（HPLC）与 ICP-MS 检测联用，用于评估酶提取物中的总硒和硒形态含量。建立了分析性能，如定量限（PAEH 和 MAEH 分别为 0.032-0.599μg/g 和 0.014-0.240μg/g）、重复性（11-14.5%）和整个过程的准确性。在所有分析的样品中都检测到了硒代蛋氨酸（SeMet），在巴西坚果中检测到了硒代半胱氨酸（SeCys）；然而，仅在巴西坚果中定量了 SeMet 和 SeCys 水平。在任何样品中均未检测到无机硒形态。酶提取物中存在 SeMet 和 SeCys，且不存在氧化硒蛋氨酸（SeOMet），这一点通过轨道阱质谱得到了确认。