化粧品中色素檢驗方法之建立   全文下載

Establishment of Analytical Method for Colorants in Cosmetics

本研究係利用液相層析串聯質譜儀（Liquid Chromatograph/tandem Mass Spectrometer, LC-MS/MS）建立一簡單、快速的方法，可同時分析化粧品中Acid blue 62等13項色素。檢體以含0.1%氨水之二氯甲烷：甲醇（2: 8, v/v）溶液萃取，經超音波振盪30分鐘後定容，經濾膜過濾後，以LC-MS/MS進行分析。使用ACQUITY BEHShield RP 18層析管柱，並採用10 mM甲酸銨溶液及甲醇：乙腈（1: 1, v/v）溶液作為移動相進行梯度沖提；利用電灑游離法（Electrospray Ionization, ESI），搭配多重反應偵測模式（Multiple Reaction Monitoring, MRM），可於15分鐘完成分析。於空白唇膏基質中添加標準品溶液（依各成分之分析範圍添加濃度介於0.2-50μg/g），進行連續3日5重複之回收率試驗，其平均回收率為87.7-113.2%，變異係數均小於9.4%，基質之離子增強或抑制效應皆小於19.54%。本檢驗方法可應用於上市後產品之監測，以確保消費者之健康安全。

A simple and fast method was developed for simultaneous determination of Acid blue 62 and other 12 colorants in cosmetics by liquid chromatography/tandem mass spectrometry (LC-MS/MS). The sample was uniformly dispersed with a solution of methanol: dichloromethane (8: 2, v/v) containing 0.1% ammonia water and then extracted by ultrasonication for 30 mins. After centrifugation and filtration, the filtrate was separated by a ACQUITY BEH Shield RP 18 column using gradient elution with 10 mM ammonium formate and methanol: acetonitrile (1: 1, v/v) solutions. The analysis could be accomplished within 15 mins by employing electrospray ionization (ESI) with the multiple reaction monitoring (MRM) mode for detection. The average recoveries of 13 compounds ranged from 87.7-113.2%, and the coefficients of variation were all less than 9.4%, by spiking multiple concentrations levels of standards ranging from 0.2-50μg/g in lipstick samples. The matrix effects for ion enhancement or inhibition were less than 19.54%. This method can be employed to monitor the post-marketing products and further safeguard the health and safety of consumers.