化粧品中禁用染髮劑成分分析方法之建立   全文下載

Establishment of Analytical Method for Banned Hair Dyes 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、快速的方法能同時分析染髮產品中1-naphthylamine等22種禁用染髮成分。檢體以甲醇溶解，經超音波振盪萃取並定容，經濾膜過濾後，以LC-MS/MS進行分析。層析管柱使用ACQUITY BEH Shield RP 18，以移動相10 mM甲酸銨與乙腈進行梯度沖提；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。採用市售染髮劑為空白檢體，添加適量標準品溶液，使最終濃度為0.02-50ppm，進行連續3天、5重複之添加回收試驗，其平均回收率為88.5-110.8%，變異係數均小於10.6%。基質之離子增強或抑制效應皆小於9.1%。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 22 banned hair dyes in cosmetics by liquid chromatography/tandem mass spectrometry (LC-MS/MS). The sample was dissolved by methanol and then extracted by ultrasonication for 30 min. After centrifugation and filtration, the filtrate was separated by the ACQUITY BEH Shield RP 18 column at gradient elution of 10 mM ammonium formate and acetonitrile. The analysis could be accomplished within 15 min by employing electrospray ionization (ESI) with the multiple reaction monitoring (MRM) mode for detection. By using commercially available hair dyes as blank sample, and adding appropriate amount of standard solution to get the final concentration between 0.2-50 ppm. After performing 5 repetitions for 3 consecutive days, the average recovery rate was between 88.5% and 110.8%. The coefficients of variation (CV, %) were all less than 10.6%. The ion enhancement or inhibition of the matrix effects were less than 9.1%. This method can be applied to the monitoring of post-marketing products to protect the health and safety of consumers.