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三种用于分析苜蓿中华根瘤菌脂肪酸的气相色谱/质谱联用方法的比较:一种微量单瓶法的开发

Comparison of three GC/MS methodologies for the analysis of fatty acids in Sinorhizobium meliloti: development of a micro-scale, one-vial method.

作者信息

Basconcillo Libia Saborido, McCarry Brian E

机构信息

Department of Chemistry, McMaster University, West Hamilton, Ontario, Canada.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Aug 1;871(1):22-31. doi: 10.1016/j.jchromb.2008.06.041. Epub 2008 Jul 1.

DOI:10.1016/j.jchromb.2008.06.041
PMID:18635405
Abstract

Three protocols for fatty acid analysis in Sinorhizobium meliloti were improved by the addition of a number of standards/controls and a silylation step which allowed the determination of recoveries, extents of conversion of lipids to fatty acid methyl esters (FAMEs) and extents of side reactions. Basic hydrolysis followed by acid-catalyzed methylation and transmethylation with sodium methoxide, were the best for the analysis of 3-hydroxy- and cyclopropane fatty acids, respectively. A micro-scale, one-vial method that employed sodium methoxide/methanol was equally efficient and on a 1000-fold smaller scale than standard methods. Because this method avoids aqueous extractions, 3-hydroxybutanoic acid was detected as its trimethylsilyloxy methyl ester along with FAMEs.

摘要

通过添加多种标准品/对照品以及一个硅烷化步骤,改进了三种用于苜蓿中华根瘤菌脂肪酸分析的方案,该硅烷化步骤可用于测定回收率、脂质转化为脂肪酸甲酯(FAME)的程度以及副反应的程度。碱性水解后进行酸催化甲基化以及用甲醇钠进行转甲基化,分别是分析3-羟基脂肪酸和环丙烷脂肪酸的最佳方法。一种采用甲醇钠/甲醇的微量单瓶法同样高效,且规模比标准方法小1000倍。由于该方法避免了水相萃取,3-羟基丁酸与其脂肪酸甲酯一起被检测为其三甲基硅氧基甲酯。

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