Gas-liquid chromatography and mass spectral analysis of mono-, di- and tricarboxylates as their tert.-butyldimethylsilyl derivatives.
Gas-liquid chromatography and mass spectral analysis of mono-, di- and tricarboxylates as their tert.-butyldimethylsilyl derivatives.
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单、二和三羧酸盐及其叔丁基二甲基甲硅烷基衍生物的气相色谱和质谱分析。
DOI：
10.1016/s0021-9673(01)86899-0
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发表时间：
1986
期刊：
影响因子：
--
通讯作者：
Madson,MA
中科院分区：
文献类型：
--
作者：
Mawhinney,TP;Robinett,RS;Atalay,A;Madson,MA
描述了一种气液色谱（GLC）程序，该程序允许在一次GLC分析中对20种饱和单羧酸盐、16种二羧酸盐（烷烃二酸盐和烷烃二酸盐）以及柠檬酸三羧酸盐和乌头酸盐进行基线分离和定量。羧酸，作为它们的衍生物。-丁基二甲基硅基化衍生物，在SPB-1（键合）毛细管柱上很容易分离。在OV-17（键合）毛细管柱和SP-2250填充柱上对这些羧酸盐，以及15种不饱和羧酸盐的分离数据也给出了。Thetert。游离或铵盐形式的羧酸-丁基二甲基硅基化在n -甲基- n -（叔丁基二甲基硅基）-三氟乙酰胺的单一衍生化步骤中完成。给出了所有一羧酸、二羧酸和三羧酸的保留数据和反应。警报的质谱分析。提出了-丁基二甲基硅基化羧酸，每种羧酸都具有显著的特征[M - 57]片段离子。
A gas-liquid chromatographic (GLC) procedure is described which permits the baseline separation and quantitation of twenty saturated monocarboxylates, sixteen dicarboxylates (both alkanedioic and alkenedioic), and the tricarboxylates citrate and aconitate in a single GLC analysis. The carboxylic acids, as theirtert.-butyldimethylsilylated derivatives, are readily separable on a SPB-1 (bonded) capillary column. Separation data on an OV-17 (bonded) capillary column and a SP-2250 packed column of these carboxylates, in addition to fifteen unsaturated carboxylates, are also given. Thetert.-butyldimethylsilylation of carboxylic acids in their free or ammonium salt forms is accomplished in a single derivatization step with N-methyl-N-(tert.-butyldimethylsilyl)-trifuloroacetamide. Retentiond ata and responses for all mono-, di- and tricarboxylic acids are given. Mass spectral analysis of allert.-butyldimethylsilylated carboxylic acids is presented and each displays a prominent and characteristic [M — 57] fragment ion.