本論文建立一種毛細管電泳分析法的線上濃縮技術以監測化粧品中的防腐劑,包括butyl paraben (BP)、isobutyl paraben (IBP)、propyl paraben (PP)、salicylic acid (SA)、ethyl paraben (EP)、methyl paraben (MP)、benzoic acid (BA)、sorbic acid (SO)、dehydracetic acid (DHA) 及p-hydroxybenzoic acid (PHBA),並且利用化學計量統計實驗設計理論(chemometric experimental design) 尋找最佳化的分析條件。 以液相萃取法進行乳霜的樣品前處理後,壓力取樣 (10 psi, 90 s) 在反向電壓 (-20 kV) 下,利用含有80 mM sodium dodecyl sulfate及30%甲醇的磷酸鹽溶液 (50 mM, pH 3) 為緩衝溶液進行分離,本方法經確效後,檢量線範圍如下: BP及IBP為5-100 ug/mL,PP為2.5-250 ug/mL,SA及BA為0.05-10 ug/mL,EP為5-120 ug/mL,DHA為0.2-50 ug/mL,MP為0.5-70 ug/mL,SO為5-350 ug/mL,PHBA為0.02-450 ug/mL,有良好的線性關係;評估同日內及異日間分析的精確度及準確性。其相對標準偏差和相對誤差皆小於7.8%,且所有待測物的偵測極限在0.005-2 ug/mL,本分析方法可成功地應用於市售化粧品中防腐劑的檢測。
In this study, a capillary electrophoresis (CE) method combined with online sample stacking was established for determination of common preservatives in cosmetic samples, including butyl paraben (BP), isobutyl paraben (IBP), propyl paraben (PP), salicylic acid (SA), ethyl paraben (EP), methyl paraben (MP), benzoic acid (BA), sorbic acid (SO), dehydracetic acid (DHA) and p-hydroxybenzoic acid (PHBA). The method was developed by using chemometric experimental design to find the optimized conditions. After liquid-liquid extraction, the extracted samples were loaded by hydrodynamic injection (10 psi, 90s). The separation was performed at -20 kV and detected at 214 nm using phosphate buffer (50 mM, pH 3) containing 30% methanol and 80 mM sodium dodecyl sulfate. During method validation, calibration curves were linear (r≧0.990) over a range of 5-100 ug/mL for BP and IBP, 2.5-250 ug/mL for PP, 0.05-10 ug/mL for EP, 0.2-50 ug/mL for DHA, 0.5-70?nug/mL for MP, 5-350 ug/mL for SO, 0.05-10 ug/mL for SA and BA, 0.02-450 ug/mL for PHBA. For the evaluation of precision and accuracy, the relative standard deviations and relative errors were all less than 7.8% in intra-batch and inter-batch analysis. The analytes could be simultaneously analyzed and have detection limits down to 0.005-2 ug/mL. This method was successfully used in detection of preservatives in commercial cosmetic products