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用于反式脂肪酸气相色谱分析的氰丙基固定相选择性优化

Optimization of the selectivity of a cyanopropyl stationary phase for the gas chromatographic analysis of trans fatty acids.

作者信息

Martin Clayton Antunes, de Oliveira Claudio Celestino, Visentainer Jesuí Vergílio, Matsushita Makoto, de Souza Nilson Evelázio

机构信息

Departamento de Química, Universidade Estadual de Maringá, Avenida Colombo 5790, Maringá, PR 87020-900, Brazil.

出版信息

J Chromatogr A. 2008 Jun 13;1194(1):111-7. doi: 10.1016/j.chroma.2008.04.033. Epub 2008 Apr 22.

Abstract

The quantification of monounsaturated and polyunsaturated trans fatty acids in partially hydrogenated fats by gas-liquid chromatography on a CP-Select CB-FAME capillary column was optimized using equivalent chain length values of fatty acids methyl esters that could coelute in the temperature range from 155 to 200 degrees C. The most appropriate temperature for the simultaneous determination of these trans isomers is around 197 degrees C. It is proposed a system to discriminate trans from cis octadecenoic fatty acid methyl esters based on the angular coefficient values of the equivalent chain length curves. The limits of detection and quantification were 0.28 and 0.93 mg g(-1). Quantification was performed in the range from 0.93 to 280 mg g(-1). Quantification accuracy was estimated by spike recovery of elaidic and trans-13-octadecenoic acids in hydrogenated fat samples. The obtained levels were from 97.60 to 103.28% for elaidic acid and from 98.12 to 99.27% for trans-13-octadecenoic acid. These results indicate that the accuracy of the methodology proposed for the quantification of monounsaturated and polyunsaturated trans fatty acids in hydrogenated fats is adequate.

摘要

通过在CP-Select CB-FAME毛细管柱上进行气液色谱法,利用在155至200摄氏度温度范围内可能共洗脱的脂肪酸甲酯的等效链长值,对部分氢化脂肪中的单不饱和和多不饱和反式脂肪酸进行了定量分析优化。同时测定这些反式异构体的最合适温度约为197摄氏度。提出了一种基于等效链长曲线的角系数值来区分反式和顺式十八碳烯酸甲酯的系统。检测限和定量限分别为0.28和0.93 mg g(-1)。在0.93至280 mg g(-1)范围内进行定量。通过在氢化脂肪样品中添加反油酸和反式-13-十八碳烯酸进行加标回收来评估定量准确性。反油酸的回收率为97.60%至103.28%,反式-13-十八碳烯酸的回收率为98.12%至99.27%。这些结果表明,所提出的用于定量氢化脂肪中单不饱和和多不饱和反式脂肪酸的方法的准确性是足够的。

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