高效能液相層析法配合二極體列陣分光光度計偵測器檢測八種使用於防曬劑紫外線阻隔成份之分析研究

本研究為開發快速簡易安全的分析方法，可分離含PABA（Para-aminobenzoic Acid）、B-3 (Benzo-phenone-3)、BM-DBM (Butyl methoxydibenzoylmethane)、OMC (Octyl methoxycinnamate)、EHS (Ethylhexyl Salicylate) 、DMABA (4-Dimethylaminobenzoic acid) 、MBBT (Methylene bis-benzotriazolyl tetramethylbutylphenol)、BEMT (Bis-ethylhexyloxyphenol methoxylphenyl triazine) 、八種混合之防曬劑成分。以HPLC搭配二極體列陣分光光度計偵測器進行分析，並以LC-MS鑑定五種成分之母峰及主要分子碎片。於建立分析方法中，探討移動相有機溶媒的比例、並找出最適化的分離條件。以Supelco discovery® C18 (150 mm × 4.6 mm, 5 μm)為固定相，移動相為H2O/THF以梯度流析方式進行，流速為1ml/min，樣品注射量10 μl，檢測波長為325 nm，分析時間共20分鐘。於此條件可成功地分離PABA、B-3、BM-DBM、EHS、DMABA、OMC、MBBT、BEMT等八種混合之防曬劑成分。本分析方法之精密度於同日間(intra-day)重複性面積CV%為0.02-0.74%，異日間(inter-day)再現性面積CV%為0.04-1.52%，線性迴歸係數為R2=0.9998~0.9999。目前市售防曬劑，正發展趨向使用MBBT、BEMT這類新型大分子結構的防曬劑成分。本研究開發的分析方法，可大幅縮短對這類新型大分子防曬劑之分析時間。故本分析方法可提供相關檢測單位及添加防曬劑化妝品的製造廠商，對其相關產品的品質管制，可參考的分析方法。

關鍵字

高效能液相層析儀；防曬劑

並列摘要

The purpose of this study is to develop a quick, easy, and safe method to analyze a sunscreen mixture with eight active ingredients: PABA（Para-aminobenzoic Acid）、B-3 (Benzo-phenone-3)、BM-DBM (Butyl methoxydibenzoylmethane)、OMC (Octyl methoxycinnamate)、EHS (Ethylhexyl Salicylate) 、DMABA (4-Dimethylaminobenzoic acid) 、MBBT (Methylene bis-benzotriazolyl tetramethylbutylphenol)、BEMT (Bis-ethylhexyloxyphenol methoxylphenyl triazine) 、. HPLC with diode array spectrophotometer detector was used for separation and detection. LC-MS was used to identify the main peaks of these five components as well as their major molecular fragments. In order to find out the optimum condition, some critical parameters such as the ratio of organic solvents in mobile phase and the pH of buffer solution, which have impacts to the separation, were studied during the development of this method. In this method, Supelco discovery® C18 (150 mm × 4.6 mm, 5 μm) was used as stationary phase, whereas H2O/THF with gradient elution was used as mobile phase. The other conditions are: flow rate 1 mL/min; injection volume 10 μL; detection wavelength 325 nm; analysis run time 20 minutes. The above five sunscreen ingredients PABA，B-3，BM-DBM，EHS，DMABA，OMC，MBBT, and BEMT were successfully separated by this method. The precision of this method was CV% =0.02%-0.74% for intra-day and CV % = 0.04%-1.52% for inter-day by reproducibility area tests. The linear regression coefficient for above tests were R2 = 0.9998 - 0.9999. Currently, the trend of sunscreens in the market is to use new macro-molecular, such as MBBT, BEMT, as the ingredients. The analytical method developed in this study can substantially reduce the analytical time of the new sunscreen macro-molecular. Therefore, this method can be a reference tool of testing or quality control for relevant analysis institutes or sunscreen manufacturers. IV

並列關鍵字

HPLC ； screen

參考文獻

1. T. John, B. Robert, C. Pete, D. Guido, F. Eberhard, F. Eberhard, G. Julian, H. Dominic, M. Paul, S. Colin, Scientific Committee on Antarctic Research, (2009). Version 1.1 25 November 2009 ISBN 978-0-948277-22-1.