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采用固相微萃取和原子发射检测气相色谱法测定牛奶和牛奶副产品中的二甲基硒和二甲基二硒。

Determination of dimethylselenide and dimethyldiselenide in milk and milk by-products by solid-phase microextraction and gas chromatography with atomic emission detection.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia, Spain.

出版信息

Talanta. 2010 Mar 15;80(5):1856-61. doi: 10.1016/j.talanta.2009.10.034. Epub 2009 Oct 24.

DOI:10.1016/j.talanta.2009.10.034
PMID:20152423
Abstract

A method based on solid-phase microextraction (SPME) followed by gas chromatography with microwave-induced plasma atomic emission detection for determining dimethylselenide (DMSe) and dimethyldiselenide (DMDSe) in milk and milk by-products is proposed. Parameters affecting the SPME, such as sample volume or mass, ionic strength, adsorption and desorption times and temperatures were optimized in the headspace mode. The matrix effect was evaluated for the different samples studied, concluding that standard additions calibration was required for quantification purposes. The detection limits ranged from 70 to 110 pg mL(-1) for DMSe and from 80 to 400 pg mL(-1) for DMDSe, depending on the sample under analysis. None of the twenty-three samples analyzed contained the studied compounds at concentrations above the corresponding detection limits.

摘要

提出了一种基于固相微萃取(SPME)结合微波诱导等离子体原子发射检测的方法,用于测定牛奶和奶制品中的二甲基硒(DMSe)和二甲基二硒(DMDSe)。优化了顶空模式下影响 SPME 的参数,如样品体积或质量、离子强度、吸附和解吸时间和温度。评估了不同样品的基质效应,得出需要进行标准添加校准以进行定量的结论。检测限范围为 70 至 110 pg mL(-1),用于 DMSe,80 至 400 pg mL(-1),用于 DMDSe,具体取决于分析的样品。在所分析的二十三个样品中,没有一个样品中含有浓度高于相应检测限的研究化合物。

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