Mueller H W, Binz K
J Chromatogr. 1982 Mar 12;228:75-93. doi: 10.1016/s0378-4347(00)80421-1.
The combination of a consecutive double capillary column gas chromatographic system (Deans type) with a fully automatic injection device was developed to determine quantitatively the fatty acid fraction of serum extracts, without prior removal of the other lipids. A major difficulty arose through ghosting (memory), via reaction of methylating reagents with lipid deposits, mainly in the injection port. Use of diazomethane circumvented this, as the reagent was easily removed prior to analysis. The combination methyl iodide--potassium carbonate, convenient handling of which requires coinjection of methyl iodide, proved to be less than completely dependable. Dimethylformamide dimethylacetal is completely out of the question as a coinjectant. Lipid deposits in the injection port produced peak area drifts which could, however, be counteracted. The apparatus is capable of analyzing samples completely unattended for at least 20 hours (80 samples). It has been operated non-stop, day and night, for between 4 and 7 days with occasional reloading and servicing.
开发了一种连续双毛细管柱气相色谱系统(迪恩斯型)与全自动进样装置的组合,用于在不预先去除其他脂质的情况下定量测定血清提取物中的脂肪酸部分。主要问题是由于甲基化试剂与脂质沉积物发生反应,主要在进样口中,产生了拖尾(记忆效应)。使用重氮甲烷可避免此问题,因为该试剂在分析前易于去除。甲基碘 - 碳酸钾组合,其方便处理需要共注入甲基碘,但事实证明可靠性不完全。二甲基甲酰胺二甲基缩醛作为共注入剂完全不可行。进样口中的脂质沉积物会产生峰面积漂移,但可以抵消。该仪器能够在至少20小时内无人值守地分析样品(80个样品)。它日夜不停地运行了4至7天,偶尔进行重新加载和维护。