利用化學計量實驗設計法結合毛細管電泳法進行化粧品中七種羥基酸之分析研究

Determination of hydroxy acids in cosmetics by chemometric experimental design and capillary electrophoresis

劉佩妤(Pei-Yu Liu)

指導教授 ： 陳彥伶

高雄醫學大學/藥學院/香粧品學系碩士班/碩士(2012年)

摘要

本研究建立一個環糊精修飾毛細管電泳法並結合化學計量實驗設計法，包括部分因子設計法及中心混成設計法，以偵測化粧品中常見之七種羥基酸的含量。相較於傳統的單一變因參數探討，化學計量實驗設計法可以增加分離效率，探討參數之間的交互作用，減少實驗時間與實驗成本之損耗。本研究首先利用兩水準部分因子設計法，經實驗後得到三個對實驗具有影響性的參數為磷酸鹽緩衝溶液濃度、界面活性劑濃度與有機溶劑比例，再以中心混成設計法搭配層析指數函數 (chromatographic exponential function, CEF) 與層析解析度統計函數 (chromatography resolution statistic function, CRS-1)評估出最佳條件。研究結果顯示，最佳分離條件所使用緩衝溶液為150 mM磷酸鹽緩衝溶液 (pH 7) 添加0.5 mM CTAB、3 mM γ-CD及25%甲醇，以0.5 psi壓力取樣20秒，分離電壓設定為-15 kV。水楊酸與杏仁酸的偵測極限為625 nM (S/N=3)。其檢量線之相關係數均大於0.998，RSD值與RE值均小於9.21%，代表此分析方法具有良好的直線性、準確度及精密度。此分析方法已成功應用於數種市售化粧品的定量檢測。

關鍵字

毛細管電泳 ； 羥基酸 ； 化學計量實驗設計法 ； 部分因子設計 ； 中心混成設計 ； 化粧品

並列摘要

A cyclodextrin-modified capillary electrophoresis (CDCE) method with chemometric experimental design, including fractional factorial design (fFD) and central composite design (CCD), was established for quantitative analysis of seven hydroxy acids (HAs) in cosmetic products. Chemometric experimental design was used to enhance the method’s separation capability and to explore the interactions between parameters. Compared to the traditional investigation of multiple parameters, it 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 response were investigated by chromatographic exponential function (CEF) and chromatography resolution statistic function (CRS-1). The optimized conditions were 150 mM phosphate solution (pH 7) containing 0.5 mM CTAB, 3 mM γ-CD and 25% methanol as running buffer, sample injection 20 second by 0.5 psi and -15 kV as separation voltage at 25℃ with UV wavelength 200 nm. The seven HAs were well separated in less than 10 min. The limit of detection (S/N=3) was 625 nM for both salicylic acid (S) and mandelic acid (MA). The correlation coefficient of regression curve was greater than 0.998 with high precision and accuracy. After optimization and validation, the simple and rapid analysis method was considered to be established and was successfully applied to several commercial cosmetic products.

並列關鍵字

Capillary electrophoresis ； Hydroxy acids ； Chemometric experimental design ； Fractional factorial design ； Central composite design ； Cosmetics

參考文獻

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