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牛奶样品中气相色谱未分离共轭亚油酸异构体三重峰的化学计量学去卷积

Chemometric deconvolution of gas chromatographic unresolved conjugated linoleic acid isomers triplet in milk samples.

作者信息

Blasko Jaroslav, Kubinec Róbert, Ostrovský Ivan, Pavlíková Eva, Krupcík Ján, Soják Ladislav

机构信息

Institute of Chemistry, Faculty of Natural Sciences, Comenius University, Mlynská dolina CH-2, 842 15 Bratislava, Slovakia.

出版信息

J Chromatogr A. 2009 Apr 3;1216(14):2757-61. doi: 10.1016/j.chroma.2008.11.019. Epub 2008 Nov 14.

DOI:10.1016/j.chroma.2008.11.019
PMID:19056089
Abstract

A generally known problem of GC separation of trans-7;cis-9; cis-9,trans-11; and trans-8,cis-10 CLA (conjugated linoleic acid) isomers was studied by GC-MS on 100m capillary column coated with cyanopropyl silicone phase at isothermal column temperatures in a range of 140-170 degrees C. The resolution of these CLA isomers obtained at given conditions was not high enough for direct quantitative analysis, but it was, however, sufficient for the determination of their peak areas by commercial deconvolution software. Resolution factors of overlapped CLA isomers determined by the separation of a model CLA mixture prepared by mixing of a commercial CLA mixture and CLA isomer fraction obtained by the HPLC semi-preparative separation of milk fatty acids methyl esters were used to validate the deconvolution procedure. Developed deconvolution procedure allowed the determination of the content of studied CLA isomers in ewes' and cows' milk samples, where dominant isomer cis-9,trans-11 is eluted between two small isomers trans-7,cis-9 and trans-8,cis-10 (in the ratio up to 1:100).

摘要

通过气相色谱-质谱联用仪(GC-MS)在涂有氰丙基硅氧烷固定相的100米毛细管柱上,于140 - 170摄氏度的等温柱温下,研究了反式-7;顺式-9;顺式-9,反式-11;以及反式-8,顺式-10共轭亚油酸(CLA)异构体的气相色谱分离中一个广为人知的问题。在给定条件下获得的这些CLA异构体的分离度对于直接定量分析而言不够高,但对于使用商业去卷积软件测定其峰面积来说却是足够的。由商业CLA混合物与通过牛奶脂肪酸甲酯的高效液相色谱半制备分离得到的CLA异构体馏分混合制备的CLA模型混合物的分离所确定的重叠CLA异构体的分离因子,被用于验证去卷积程序。所开发的去卷积程序能够测定母羊和牛奶样品中所研究的CLA异构体的含量,其中占主导的异构体顺式-9,反式-11在两个较小的异构体反式-7,顺式-9和反式-8,顺式-10之间洗脱(比例高达1:100)。

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