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采用微波辅助提取和固相萃取后电感耦合等离子体发射光谱法测定营养补充剂中的钴形态。

Determination of cobalt species in nutritional supplements using ICP-OES after microwave-assisted extraction and solid-phase extraction.

机构信息

Warsaw University of Technology, Faculty of Chemistry, Chair of Analytical Chemistry, Noakowskiego 3, 00-664 Warsaw, Poland.

Warsaw University of Technology, Faculty of Chemistry, Chair of Analytical Chemistry, Noakowskiego 3, 00-664 Warsaw, Poland.

出版信息

J Pharm Biomed Anal. 2018 Jun 5;155:135-140. doi: 10.1016/j.jpba.2018.03.058. Epub 2018 Mar 31.

Abstract

Cobalt content (as vitamin B and inorganic cobalt) in two nutritional supplements, namely Spirulina platensis and Saccharomyces cerevisiae known as a "superfood", has been determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Several sample pre-treatment protocols have been applied and compared. Microwave-assisted acid digestion efficiently decomposed all cobalt-containing compounds, thus allowed obtaining total cobalt content in supplements examined. Vitamin B was extracted from the samples with acetate buffer and potassium cyanide solution exposed to mild microwave radiation for 30 min, and cyanocobalamin was separated from the extract by on-column solid phase extraction using C-18 modified silica bed. About 100% of cobalt species was extracted using the triple microwave-assisted extraction procedure. Total cobalt content was 20-fold greater in Spirulina tablets than the declared cobalamin content (as Co). The ICP-OES method precision was about 3% and detection limit was 1.9 and 2.7 ng Co mL for inorganic cobalt or cyanocobalamin, respectively.

摘要

采用电感耦合等离子体发射光谱法(ICP-OES)测定了两种营养补充剂——螺旋藻和酿酒酵母(被称为“超级食物”)中的钴含量(作为维生素 B 和无机钴)。应用并比较了几种样品预处理方案。微波辅助酸消解能有效地分解所有含钴化合物,从而能够获得所检测补充剂中的总钴含量。采用醋酸盐缓冲液和氰化钾溶液从样品中提取维生素 B,并在温和的微波辐射下暴露 30 分钟,然后使用 C-18 改性硅胶床在柱上进行固相萃取,将氰钴胺素从提取物中分离出来。使用三重微波辅助提取程序,可提取约 100%的钴形态。螺旋藻片中的钴总含量比所宣称的维生素 B12 含量(以 Co 计)高 20 倍。ICP-OES 法的精密度约为 3%,检测限分别为无机钴或氰钴胺素的 1.9 和 2.7ng Co/mL。

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