染髮劑中芳胺成分檢驗方法建立   全文下載

Establishment of an Analytical Method for Aromatic Amines in Hair Dyes

本研究係利用液相層析串聯質譜法（liquid chromatography/tandem mass spectrometry, LC-MS/MS）建立一簡單、快速的方法能分析染髮劑中29項芳胺成分。檢體以含0.1%氨水之甲醇溶液萃取，經超音波振盪30分鐘後定容，經濾膜過濾後進行定性及定量分析。分析條件採用ZORBAX Eclipse XDB-C18（3.5μm，2.1 mm x 50 mm）層析管柱，移動相為含0.05%甲酸之5 mM醋酸銨溶液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分鐘內完成分析。於市售染髮劑空白基質中添加標準溶液（依各成分之分析範圍添加濃度介於0.02-400μg/g），進行連續3日5重複之回收試驗，其平均回收率為88.4-116.3%，變異係數均小於9.7%，基質之離子增強或抑制效應皆小於9.49%。本檢驗方法可應用於上市後染髮劑產品之監測，以確保消費者之健康安全。

A simple and rapid method was developed for simultaneous determination of 29 aromatic amines in hair dyes by liquid chromatography/tandem mass spectrometry (LC-MS/MS). The sample was uniformly dispersed with methanol containing 0.1% ammonia water and then extracted by ultrsonication for 30 min. After centrifugation and filtration, the filtrate was separated on a ZORBAX Eclipse XDB-C18 (3.5 μm, 2.1 mm x 50 mm) column by gradient elution of 5 mM ammonium acetate containing 0.05% formic acid and acetonitrile. The analysis can be accomplished within 15 min. by employing electrospray ionization (ESI) with multiple reaction monitoring (MRM) mode for detection. The average recoveries of 29 compounds ranged from 88.4-116.3%, and the coefficients of variation were all lower than 9.7%, when spiking multiple concentration levels of standards ranged from 0.02-400 μg/g in hair dye samples. The matrix effects for ion enhancement or inhibition were lower than 9.49%. This method can be applied to the monitoring of post-marketing products and safeguard the health and safety of the consumers.