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Electrophoresis. 2005 Oct;26(20):3952-9. doi: 10.1002/elps.200500080.
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电动色谱法对防晒剂3-(4-甲基亚苄基)-樟脑的对映体拆分:化妆品配方中的定量分析

Enantioselective separation of the sunscreen agent 3-(4-methylbenzylidene)-camphor by electrokinetic chromatography: Quantitative analysis in cosmetic formulations.

作者信息

Gómara Belén, García-Ruiz Carmen, Marina María Luisa

机构信息

Centro de Tecnología de los Alimentos y Servicios Biosanitarios, Universidad de Alcalá, Alcalá de Henares, Madrid, Spain.

出版信息

Electrophoresis. 2005 Oct;26(20):3952-9. doi: 10.1002/elps.200500080.

DOI:10.1002/elps.200500080
PMID:16217832
Abstract

3-(4-Methylbenzylidene)-camphor (MBC) is a chiral sunscreen agent used in cosmetic products. In this work, the enantioseparation of MBC has been performed by EKC and applied to the analysis of the MBC enantiomers in cosmetic creams. Different experimental conditions (type and concentration of the chiral selector, temperature, and sample solvent) have been optimized. Due to the neutral nature of this compound, anionic CD derivatives were investigated as chiral selectors. Carboxymethylated-beta-CD (CM-beta-CD) showed the highest chiral separation power, observing that a 15 mM concentration of this CD at a working temperature of 15 degrees C enabled to obtain the highest enantioresolution. However, under these conditions, tailing of peaks obtained for the enantiomers was observed. The addition of increasing concentrations of the neutral alpha-CD to CM-beta-CD at a 15 mM concentration in a 100 mM borate buffer at pH 9.0 improved the enantiomeric separation and decreased peak tailing. The use of DMF for the total dissolution of the cosmetic creams, and methanol:water (1:1 v/v) for appropriate dilution enabled to observe good shape and size for the peaks of the MBC enantiomers. After optimizing a method for the preconditioning of the capillary, the analytical characteristics of the chiral separation method for the analysis of MBC were investigated. Linearity, LODs and LOQs, precision (instrumental repeatability, method repeatability, intermediate precision), accuracy, and selectivity were evaluated. The method was applied to analyze MBC enantiomers contained in two commercial cosmetic creams containing racemic MBC and to study the skin absorption of this compound with time.

摘要

3-(4-甲基亚苄基)-樟脑(MBC)是一种用于化妆品的手性防晒剂。在本研究中,采用毛细管电泳法对MBC进行了对映体拆分,并将其应用于化妆品面霜中MBC对映体的分析。对不同的实验条件(手性选择剂的类型和浓度、温度以及样品溶剂)进行了优化。由于该化合物呈中性,因此研究了阴离子型环糊精衍生物作为手性选择剂。羧甲基化-β-环糊精(CM-β-CD)表现出最高的手性分离能力,发现在15℃的工作温度下,15 mM浓度的该环糊精能够获得最高的对映体分辨率。然而,在这些条件下,观察到对映体的峰出现拖尾现象。在pH 9.0的100 mM硼酸盐缓冲液中,向15 mM浓度的CM-β-CD中添加浓度不断增加的中性α-环糊精,改善了对映体分离效果并减少了峰拖尾。使用二甲基甲酰胺完全溶解化妆品面霜,并使用甲醇:水(1:1 v/v)进行适当稀释,使得MBC对映体的峰具有良好的峰形和大小。在优化了毛细管预处理方法后,研究了用于分析MBC的手性分离方法的分析特性。评估了线性、检测限和定量限、精密度(仪器重复性、方法重复性、中间精密度)、准确度和选择性。该方法应用于分析两种含有外消旋MBC的商业化妆品面霜中所含的MBC对映体,并研究该化合物随时间的皮肤吸收情况。