Department of Fragrance and Cosmetic Science, College of Pharmacy, Kaohsiung Medical University, Kaohsiung, Taiwan.
Electrophoresis. 2012 Oct;33(19-20):3079-86. doi: 10.1002/elps.201200213. Epub 2012 Sep 20.
A CD-modified CE method was established for quantitative determination of seven hydroxy acids in cosmetic products. This method involved chemometric experimental design aspects, including fractional factorial design and central composite design. Chemometric experimental design was used to enhance the method's separation capability and to explore the interactions between parameters. Compared to the traditional investigation that uses multiple parameters, the method that used chemometric experimental design was less time-consuming and lower in cost. In this study, the influences of three experimental variables (phosphate concentration, surfactant concentration, and methanol percentage) on the experimental response were investigated by applying a chromatographic resolution statistic function. The optimized conditions were as follows: a running buffer of 150 mM phosphate solution (pH 7) containing 0.5 mM CTAB, 3 mM γ-CD, and 25% methanol; 20 s sample injection at 0.5 psi; a separation voltage of -15 kV; temperature was set at 25°C; and UV detection at 200 nm. The seven hydroxy acids were well separated in less than 10 min. The LOD (S/N = 3) was 625 nM for both salicylic acid and mandelic acid. The correlation coefficient of the regression curve was greater than 0.998. The RSD and relative error values were all less than 9.21%. After optimization and validation, this simple and rapid analysis method was considered to be established and was successfully applied to several commercial cosmetic products.
建立了一种 CD 修饰的 CE 方法,用于定量测定化妆品中七种羟基酸。该方法涉及化学计量学实验设计方面,包括分因子设计和中心组合设计。化学计量学实验设计用于增强方法的分离能力,并探讨参数之间的相互作用。与使用多个参数的传统研究相比,使用化学计量学实验设计的方法耗时更少,成本更低。在本研究中,通过应用色谱分辨率统计函数,研究了三个实验变量(磷酸盐浓度、表面活性剂浓度和甲醇百分比)对实验响应的影响。优化条件如下:运行缓冲液为 150 mM 磷酸盐溶液(pH 7),含 0.5 mM CTAB、3 mM γ-CD 和 25%甲醇;20 s 以 0.5 psi 进样;分离电压为-15 kV;温度设定为 25°C;200nm 处 UV 检测。七种羟基酸在不到 10 分钟内得到很好的分离。水杨酸和扁桃酸的 LOD(S/N=3)均为 625 nM。回归曲线的相关系数大于 0.998。RSD 和相对误差值均小于 9.21%。经过优化和验证,认为该简单快速的分析方法已经建立,并成功应用于几种商业化妆品。