利用高效液相層析儀分析化粧品中12種防腐劑之方法開發與應用

The Analytical Method Development and Application of Twelve Preservatives in Cosmetics with High-Performance Liquid Chromatography

防腐劑已廣泛運用於食品、藥品及化粧品等產品中，其可經由抑制微生物生長以延長產品保存期限，然過量的防腐劑可能導致皮膚不適或過敏等現象。本研究針對臺灣衛生福利部食品藥物管理署（Taiwan Food and Drug Administration, TFDA）化粧品中防腐劑之建議檢驗方法所提及的2種防腐劑（苯甲酸、水楊酸、對羥苯甲酸、己二烯酸、去水醋酸、對羥苯甲酸甲酯、對羥苯甲酸乙酯、對羥苯甲酸丙酯、對羥苯甲酸異丙酯、對羥苯甲酸丁酯、對羥苯甲酸異丁酯及對羥苯甲酸第二丁酯）以高效液相層析儀搭配光二極體陣列檢測器（high-performance liquid chromatography with photodiode array, HPLC-PDA）進行分析方法開發及確效，並針對32種市售產品進行背景值調查。結果顯示，使用含0. %三氟醋酸的水及乙腈溶液作為移動相搭配Kinetex C 8管柱可於44.2分鐘內將2種防腐劑完全分離，定量極限為0.25~μg/mL，於酸類防腐劑~20μg/mL及酯類防腐劑0.25~5μg/mL之線性範圍內，線性回歸係數皆大於0.99，且於3種常見化粧品的基質（水類、凝膠類及乳液類）添加回收率（酸類防腐劑83.9~ 5. %、酯類防腐劑86.4~ 0.9%）及重複性（酸類防腐劑0.2~8.7%、酯類防腐劑0.4~ 3.8%）皆符合化學檢驗方法之確效規範。針對32件市售產品進行調查，其中30件樣品皆符合法規，其餘2件樣品未符合法規規範。

Preservatives are widely added to products such as foods, medicine, and cosmetics to extend the shelf life of products by inhibiting the growth of microorganisms, but excessive preservatives may cause skin allergies or discomfort. Twelve preservatives (benzoic acid, salicylic acid, 4-hydroxybenzoic acid, sorbic acid, dehydroacetic acid, methylparaben, ethylparaben, propylparaben, isopropylparaben, butylparaben, isobutylparaben and sec-butylparaben) mentioned in the recommended test methods for preservatives in cosmetic products of Taiwan Food and Drug Administration (TFDA), the Ministry of Health and Welfare of Taiwan, were analyzed by high-performance liquid chromatography with photodiode array (HPLC-PDA) and the investigation was carried out for 32 commercially available products. The results showed that using water containing 0.1% trifluoroacetic acid and acetonitrile solution as mobile phase, and Kinetex C18 column could completely separate 12 preservatives in 44.2 minutes. The quantitative limit is 0.25~1μg/mL, and the linear regression coefficient is greater than 0.99 in the linear range of acid preservative (1~20μg/mL) and ester preservative (0.25~5μg/mL). The accuracy of acid preservatives and ester preservatives was 83.9~115.1% and 86.4~110.9%, respectively. The precision of acid preservatives and ester preservatives was 0.2~8.7% and 0.4~13.8%, respectively. All results met the validation criteria of TFDA chemical testing methods. Thirty-two commercially available products were investigated, of which 30 samples were comply with regulatory requirements and the remaining 2 samples were not.