Wu Yan, Chen Guoqiang, Ji Chengdong, Hoptroff Michael, Jones Andrew, Collins Luisa Z, Janssen Hans-Gerd
Unilever R&D Shanghai, 66 Lin Xin Road, Linkong Economic Development Zone, Shanghai, 200335, China.
Analytical-Chemistry Group, Van't Hoff Institute for Molecular Sciences, University of Amsterdam, Science Park 904, 1098 XH, Amsterdam, The Netherlands.
Anal Bioanal Chem. 2016 Mar;408(9):2357-62. doi: 10.1007/s00216-016-9335-0. Epub 2016 Jan 29.
A sensitive and specific gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the measurement of the squalene content from root to tip, in both Chinese black virgin and bleached hair. Deuterated squalene was used as the internal standard. For quantification, selective ion monitoring (SIM) at m/z 410.0 and 347.0 were monitored for squalene and deuterated squalene, respectively. Different methods for the extraction of squalene from ex vivo human hair were compared including organic solvent extraction and acid/alkali hydrolysis. The best extraction efficiency was obtained by using a mixed solvent consisting of chloroform:methanol = 2:1 (v:v). The linear range of squalene ran from 1.0 to 50.0 μg mL(-1). The limit of detection (LOD) was 0.10 μg mL(-1) (corresponding to 0.005 mg g(-1) in human hair), which enabled quantification of squalene in human hair at very low level. The recovery of squalene was 96.4 ± 1.46% (n = 3). Using the above-mentioned mixed solvent extraction, squalene content in human hair was successfully quantified from root to tip. Meanwhile, a Raman imaging method was developed to visualize the squalene distribution in Chinese white virgin hair from cuticle to medulla.
开发并验证了一种灵敏且特异的气相色谱 - 质谱联用(GC - MS)方法,用于测定中国黑色原生发和漂发从发根到发梢的角鲨烯含量。氘代角鲨烯用作内标。定量时,分别对质荷比(m/z)为410.0的角鲨烯和m/z为347.0的氘代角鲨烯进行选择性离子监测(SIM)。比较了从离体人发中提取角鲨烯的不同方法,包括有机溶剂萃取和酸碱水解。使用氯仿:甲醇 = 2:1(v:v)的混合溶剂获得了最佳提取效率。角鲨烯的线性范围为1.0至50.0 μg mL⁻¹。检测限(LOD)为0.10 μg mL⁻¹(相当于人发中0.005 mg g⁻¹),这使得能够对人发中极低水平的角鲨烯进行定量。角鲨烯的回收率为96.4 ± 1.46%(n = 3)。使用上述混合溶剂萃取法,成功定量了人发从发根到发梢的角鲨烯含量。同时,开发了一种拉曼成像方法,以可视化中国白色原生发从角质层到髓质的角鲨烯分布。