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应用于化妆品分析的超临界流体色谱法中的方法开发途径。

Method developments approaches in supercritical fluid chromatography applied to the analysis of cosmetics.

作者信息

Lesellier E, Mith D, Dubrulle I

机构信息

University Orléans, CNRS, ICOA (Institut de Chimie Organique et Analytique), UMR 7311, Pôle de Chimie, rue de Chartres, Orléans, F-45067 France.

University Orléans, CNRS, ICOA (Institut de Chimie Organique et Analytique), UMR 7311, Pôle de Chimie, rue de Chartres, Orléans, F-45067 France.

出版信息

J Chromatogr A. 2015 Dec 4;1423:158-68. doi: 10.1016/j.chroma.2015.10.053. Epub 2015 Oct 23.

Abstract

Analyses of complex samples of cosmetics, such as creams or lotions, are generally achieved by HPLC. These analyses are often multistep gradients, due to the presence of compounds with a large range of polarity. For instance, the bioactive compounds may be polar, while the matrix contains lipid components that are rather non-polar, thus cosmetic formulations are usually oil-water emulsions. Supercritical fluid chromatography (SFC) uses mobile phases composed of carbon dioxide and organic co-solvents, allowing for good solubility of both the active compounds and the matrix excipients. Moreover, the classical and well-known properties of these mobile phases yield fast analyses and ensure rapid method development. However, due to the large number of stationary phases available for SFC and to the varied additional parameters acting both on retention and separation factors (co-solvent nature and percentage, temperature, backpressure, flow rate, column dimensions and particle size), a simplified approach can be followed to ensure a fast method development. First, suited stationary phases should be carefully selected for an initial screening, and then the other operating parameters can be limited to the co-solvent nature and percentage, maintaining the oven temperature and back-pressure constant. To describe simple method development guidelines in SFC, three sample applications are discussed in this paper: UV-filters (sunscreens) in sunscreen cream, glyceryl caprylate in eye liner and caffeine in eye serum. Firstly, five stationary phases (ACQUITY UPC(2)) are screened with isocratic elution conditions (10% methanol in carbon dioxide). Complementary of the stationary phases is assessed based on our spider diagram classification which compares a large number of stationary phases based on five molecular interactions. Secondly, the one or two best stationary phases are retained for further optimization of mobile phase composition, with isocratic elution conditions or, when necessary, two-step gradient elution. The developed methods were then applied to real cosmetic samples to assess the method specificity, with regards to matrix interferences, and calibration curves were plotted to evaluate quantification. Besides, depending on the matrix and on the studied compounds, the importance of the detector type, UV or ELSD (evaporative light-scattering detection), and of the particle size of the stationary phase is discussed.

摘要

对诸如面霜或乳液等复杂化妆品样品的分析通常通过高效液相色谱法(HPLC)来完成。由于存在极性范围很广的化合物,这些分析往往采用多步梯度洗脱。例如,生物活性化合物可能是极性的,而基质中含有相当非极性的脂质成分,因此化妆品配方通常是油水乳液。超临界流体色谱法(SFC)使用由二氧化碳和有机共溶剂组成的流动相,使得活性化合物和基质辅料都具有良好的溶解性。此外,这些流动相的经典且广为人知的特性能够实现快速分析,并确保方法的快速开发。然而,由于超临界流体色谱法有大量可供选择的固定相,以及存在多种同时作用于保留因子和分离因子的附加参数(共溶剂性质和百分比、温度、背压、流速、色谱柱尺寸和粒径),可以采用一种简化方法来确保快速的方法开发。首先,应仔细选择合适的固定相进行初步筛选,然后将其他操作参数限制在共溶剂性质和百分比上,保持柱温箱温度和背压恒定。为了描述超临界流体色谱法中简单的方法开发指南,本文讨论了三个样品应用:防晒霜中的紫外线过滤剂(防晒剂)、眼线笔中的辛酸甘油酯和眼部精华液中的咖啡因。首先,在等度洗脱条件(二氧化碳中含10%甲醇)下筛选五种固定相(ACQUITY UPC(2))。基于我们的蜘蛛图分类法评估固定相的互补性,该分类法基于五种分子相互作用比较大量固定相。其次,保留一种或两种最佳固定相,用于进一步优化流动相组成,采用等度洗脱条件,或在必要时采用两步梯度洗脱。然后将所开发的方法应用于实际化妆品样品,以评估方法的特异性(考虑基质干扰情况),并绘制校准曲线以评估定量。此外,根据基质和所研究的化合物,讨论了检测器类型(紫外或蒸发光散射检测(ELSD))以及固定相粒径的重要性。

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