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一种结合色谱法灵敏且特异测定毛发脂质的系统方法。

A systematic method for the sensitive and specific determination of hair lipids in combination with chromatography.

作者信息

Masukawa Yoshinori, Tsujimura Hisashi, Imokawa Genji

机构信息

Tochigi Research Laboratories, Kao Corporation, 2606 Akabane, Ichikai-machi, Haga, Tochigi 321-3497, Japan.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Sep 5;823(2):131-42. doi: 10.1016/j.jchromb.2005.06.014.

Abstract

A systematic method for the sensitive, precise and accurate determination of hair lipids, including trace amounts of intrinsic endogenous cholesterol (CH), ceramide/N-palmitoyl-DL-dihydrosphingosine (CER/PDS), cholesterol sulfate (CS) and chemically bound 18-methyl eicosanoic acid (18-MEA), has been developed in combination with TLC/FID (flame ionization detection), LC/MS and GC/MS. TLC/FID was used for the simultaneous determination of squalene (SQ), wax esters (WEs), triglycerides (TGs) and free fatty acids (FFAs). Optimal conditions for LC/MS to determine CS and 18-MEA were developed using selected ion monitoring (SIM) under the negative ion mode of electrospray ionization. An alternative procedure for the determination of 18-MEA was also established using commercially available heneicosanoic acid (HEA). In GC/MS, the optimal selection of ions for SIM of trimethylsilylated CH and CER/PDS, and the use of on-column injection has enabled their simultaneous detection. This newly developed method has been used to characterize the hair lipid composition from the proximal root end to the distal tip of chemically untreated hair fibers from two different females, and specific changes of hair lipids probably due to its origin and individuals have been demonstrated for the first time. This method may be useful for clarifying the important roles of intrinsic endogenous 18-MEA, CS, CH and CERs in the function of the cell membrane complex of hair fibers.

摘要

结合薄层层析/火焰离子化检测(TLC/FID)、液相色谱/质谱联用(LC/MS)和气相色谱/质谱联用(GC/MS)技术,已开发出一种灵敏、精确且准确测定毛发脂质的系统方法,该方法可测定痕量的内源性胆固醇(CH)、神经酰胺/N - 棕榈酰 - DL - 二氢鞘氨醇(CER/PDS)、胆固醇硫酸酯(CS)以及化学结合的18 - 甲基二十烷酸(18 - MEA)。TLC/FID用于同时测定角鲨烯(SQ)、蜡酯(WEs)、甘油三酯(TGs)和游离脂肪酸(FFAs)。采用电喷雾电离负离子模式下的选择离子监测(SIM)技术,确定了LC/MS测定CS和18 - MEA的最佳条件。还建立了一种使用市售二十一烷酸(HEA)测定18 - MEA的替代方法。在GC/MS中,通过对三甲基硅烷化CH和CER/PDS进行SIM的离子最佳选择以及采用柱上进样,实现了它们的同时检测。这种新开发的方法已用于表征来自两名不同女性的未经过化学处理的毛发纤维从近端根部到远端末梢的毛发脂质组成,并首次证明了毛发脂质可能因其来源和个体不同而发生的特定变化。该方法可能有助于阐明内源性18 - MEA、CS、CH和神经酰胺在毛发纤维细胞膜复合体功能中的重要作用。

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