化粧品中禁用染髮劑成分檢驗方法之建立   全文下載

Establishment of an Analytical Method for Prohibited Hair Dye Ingredients in Cosmetics

衛生福利部分別於110及111年公告修正「化粧品禁止使用成分表」，增列多項不得使用於染髮用途之化粧品成分，為保障消費者產品使用安全及完備化粧品檢驗方法，本研究以液相層析串聯質譜法（Liquid Chromatography/Tandem Mass Spectrometry, LC-MS/MS）建立化粧品中5項禁用染髮劑成分之檢驗方法，利用電灑游離法（Electrospray Ionization, ESI）搭配多重反應偵測模式（Multiple Reaction Monitoring, MRM），並以ACQUITY UPLC HSS T3（1.8μm, 2.1×100 mm）作為分析管柱，檢測化粧品中Sulfanilic acid、Disperse brown 1、Disperse orange 3、Disperse red 11及Disperse blue 7等5項成分。檢體經甲醇萃取，以10 mM甲酸銨水溶液（pH 8）及甲醇：乙腈（1：1, v/v）溶液作為移動相，進行梯度沖提，並以LC-MS/MS分析，整體分析時間為15分鐘，即可獲得良好分析結果。另分別以粉、液及膏劑等3種劑型之染髮產品進行基質標準品添加試驗，以評估方法偵測極限及專一性，結果顯示不同劑型之基質添加標準品均無干擾，各分析物層析峰滯留時間、定性離子之相對離子強度及訊躁比（S/N≥3）具良好的鑑別及重複性。在偵測極限部分，Disperse brown 1、Disperse orange 3及Disperse blue 7均為2μg/g，Disperse red 11為0.1μg/g，而Sulfanilic acid則為200μg/g。未來將公開本研究之檢驗方法，供各界參考使用。

The Ministry of Health and Welfare in Taiwan announced amendments to the“List of Ingredients Prohibited in Cosmetic Products”in 2021 and 2022, adding several ingredients prohibited for hair dyeing purposes. In order to ensure user safety, and the completeness of analytical methods of cosmetics, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of five banned hair dye ingredients in cosmetics. Employing electrospray ionization (ESI) coupled with multiple reaction monitoring (MRM) mode, and utilizing ACQUITY UPLC HSS T3 (1.8μm, 2.1×100 mm) as the analytical column, the method was used to detect the presence of sulfanilic acid, disperse brown 1, disperse orange 3, disperse red 11, and disperse blue 7 in hair dye cosmetic products. Methanol was used as the extraction solvent, along with a gradient elution composed of a 10 mM ammonium formate aqueous solution (pH 8) and a solution of methanol: acetonitrile (1:1, v/v) as the mobile phase with a total analysis time of 15 minutes to achieve optimal analytical results. Furthermore, matrix spiking tests were conducted to evaluate the detection limits and specificity of the method on three types of hair dye products with the formulation forms of powder, liquid, and cream. The results showed that there was no interference from different types of matrix, and the method exhibited good discrimination and repeatability for each analyte in terms of retention time, relative ion intensity and signal-to-noise ratio (S/N≥3). The detection limits of disperse brown 1, disperse orange 3, and disperse blue 7 were 2μg/g, and those of disperse red 11 and sulfanilic acid were 0.1μg/g and 200μg/g, respectively. The established testing method will be published for public use.