Huang Z H, Gage D A, Bieber L L, Sweeley C C
MSU-NIH Mass Spectrometry Facility, Department of Biochemistry, Michigan State University, East Lansing 48824-1319.
Anal Biochem. 1991 Nov 15;199(1):98-105. doi: 10.1016/0003-2697(91)90275-x.
A novel approach to the analysis of acylcarnitines has been developed. It involves a direct esterification using propyl chloroformate in aqueous propanol followed by ion-pair extraction with potassium iodide into chloroform and subsequent on-column N-demethylation of the resulting acylcarnitine propyl ester iodides. The products, acyl N-demethylcarnitine propyl esters, are volatile and are easily analyzed by gas chromatography-chemical ionization mass spectrometry. For medium-chain-length (C4-C12) acylcarnitine standards, detection limits are demonstrated to be well below 1 ng starting material using selected ion monitoring. Well-separated gas chromatographic peaks and structure-specific mass spectra are obtained with samples of synthetic and biological origin. Seven acylcarnitines have been characterized in the urine of a patient suffering from medium-chain acyl-CoA dehydrogenase deficiency.
已开发出一种分析酰基肉碱的新方法。该方法包括在丙醇水溶液中使用氯甲酸丙酯进行直接酯化，然后用碘化钾进行离子对萃取进入氯仿，随后对所得的酰基肉碱丙酯碘化物进行柱上N-去甲基化。产物酰基N-去甲基肉碱丙酯具有挥发性，可通过气相色谱-化学电离质谱轻松分析。对于中链长度（C4-C12）的酰基肉碱标准品，使用选择离子监测时，检测限证明远低于1 ng起始原料。从合成和生物来源的样品中获得了分离良好的气相色谱峰和结构特异性质谱图。在一名患有中链酰基辅酶A脱氢酶缺乏症的患者尿液中已鉴定出七种酰基肉碱。
