利用液相層析串聯質譜法分析化粧品中染髮劑成分

Determination of Oxidative Hair Dyes in Cosmetic by Liquid Chromatography-Tandem Mass Spectrometry

本研究係利用高效液相串聯質譜儀（LC/MS/MS）建立一簡單、快速的方法能同時分析等24種限用及1種禁用染髮劑成分。檢體以50%甲醇溶液溶解定容後，以0.22 μm濾膜過濾，經Waters AQUITY UPLC HSS T3層析管柱（2.1 × 100 mm, 1.8 μm）；採用10mM甲酸銨水溶液（以氨水調整pH值至9）及甲醇/乙腈（1:1, v/v）為移動相作梯度沖提；流速為0.3 mL/min；利用正負離子電灑游離法（ESI），搭配多重反應監測模式（MultipleReaction Monitoring, MRM）偵測。25種成分之標準曲線線性範圍為0.05 - 25 μg/mL，迴歸係數R^2皆為0.997以上，同日內及異日間之相對標準偏差均小於10.44%，添加回收試驗結果，回收率介於81.2 - 120.3%，相對標準偏差均小於6.9%。本方法將提供各界檢驗之參考。

A rapid and specific method for the determination and quantification of 25 hair dyes in cosmetics by liquid chromatography-tanden mass spectrometry (LC/MS/MS) was established. 24 kinds banned and 1 restricted dyestuffs in hair dyes was established. The samples were dissolved in 50% methanol for analysis liquid chromatography was performed using an Acquity UPLC HSS T3 (2.1 × 100 mm, 1.8 μm) column with 10 mM ammonium formate (adjusted topH 9 with ammonia) and methanol/acetonitrile (1:1, v/v) solution as eluent under gradient program at flow rate of 0.3 mL/min. Electrospray ionization (ESI) tandem mass spectrometry with multiple reaction monitoring (MRM) mode was use for detection. The concentration range of the standards was 0.05 - 25 μg/mL, with excellent linearity at R^2＞0.997 and intraday and inter-day relative standard deviations of less than 10.44%. The average of recoveries of spiked samples were 81.2 - 120.3%, with relative standard deviations of less than 6.9%.