He Shali, Zhao Yifang, Zhu Zhiwei, Liu Huwei, Li Meixian, Shao Yuanhua, Zhuang Qiankun
Institute of Analytical Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing, PR China.
Talanta. 2006 Mar 15;69(1):166-71. doi: 10.1016/j.talanta.2005.09.018. Epub 2005 Oct 17.
The separation and determination of four parabens (methyl, ethyl, propyl, and butyl p-hydroxybenzoate) which are commonly used as preservatives in cosmetic products, by micellar electrokinetic capillary chromatography (MEKC) with and without large-volume sample stacking (LVSS) technique were compared. As an effective on-line concentration technique, LVSS was successfully combined with MEKC to determine neutral parabens in an acidic media. The effects of some typical parameters such as sample volume, buffer pH, temperature, and concentration of surfactant were examined. The detection limits for this LVSS-MEKC method were found to be 3.0 x 10(-7)M for each of the parabens based on the signal-to-noise ratio of 3, which were around 300 times lower than normal MEKC technique. The curves of peak response versus concentration were linear from 1.0 x 10(-6) to 5.0 x 10(-5)M with regression coefficients of 0.9987, 0.9960, 0.9925 and 0.9864, respectively. A simple and easy-manipulative sample preparation method was developed and validated by analyzing commercially available cosmetic samples. It was found that with current sample preparation process and instrumentation system, 0.5 g of sample is enough for the analysis of parabens preservatives in cosmetic product with satisfactory results.
比较了采用胶束电动毛细管色谱法(MEKC)并结合或不结合大体积样品堆积(LVSS)技术对化妆品中常用防腐剂四种对羟基苯甲酸酯(对羟基苯甲酸甲酯、乙酯、丙酯和丁酯)的分离和测定。作为一种有效的在线富集技术,LVSS成功地与MEKC联用,用于测定酸性介质中的中性对羟基苯甲酸酯。考察了进样体积、缓冲液pH值、温度和表面活性剂浓度等一些典型参数的影响。基于3的信噪比,该LVSS-MEKC方法对各对羟基苯甲酸酯的检测限为3.0×10⁻⁷M,比常规MEKC技术低约300倍。峰响应值与浓度的曲线在1.0×10⁻⁶至5.0×10⁻⁵M范围内呈线性,回归系数分别为0.9987、0.9960、0.9925和0.9864。通过分析市售化妆品样品,开发并验证了一种简单易操作的样品制备方法。结果发现,采用当前的样品制备工艺和仪器系统,0.5g样品足以分析化妆品中的对羟基苯甲酸酯防腐剂,结果令人满意。