化粧品中aminoether型之antihistamine成分以LC/MS/MS分析之檢驗方法建立

Determination of Antihistamines in Cosmetics by Liquid Chromatography - Tandem Mass Spectrometry

許闊顯(Kuo-Hsien Hsu)；黃守潔(Shou-Chieh Haung)；陳玉盆(Yu-Pen Chen)；周秀冠(Hsiu-Kuan Chou)；陳惠芳(Hwei-Fang Cheng)

化粧品 ； 抗組織胺 ； 超高效液相層析串聯質譜儀 ； cosmetics ； antihistamine ； UPLC/MS/MS

食品藥物研究年報

6期（2015 / 12 / 01）

281 - 287

繁體中文

本研究利用超高效液相層析串聯式質譜儀(UPLC/MS/MS)，建立一簡便快速的分析方法，可同步分析化粧品中bromodiphenhydramine、carbinoxamine、clemastine、diphenhydramine、diphenylpyraline、doxylamine等6種常見Aminoether型antihistamine成分。檢體以甲醇溶解後，經ACQUITY UPLC HSS T3層析管柱(2.1×100 mm, 1.8μm)，採用0.1%甲酸溶液及甲醇/乙腈(75：25，v/v)溶液為移動相作梯度沖提，並以多重反應監測模式(MRM)偵測，6種成分之標準曲線線性範圍為0.25-10 ng/mL，線性回歸係數r2皆為0.995以上。同日內及異日間之相對標準偏差均小於11.8%，添加回收試驗之回收率介於90.9-113.9%，相對標準偏差皆小於13.1%，定量極限皆可達0.5 mg/g。應用本研究所建立之方法檢測市售頭部用化粧品共25件，結果均符合相關規定。

In this study, a simple and rapid UPLC/MS/MS method was set up for the quantification of 6 antihistamines, namely bromodiphenhydramine, carbinoxamine, clemastine, diphenhydramine, diphenylpyraline and doxylamine, in cosmetics. The samples were dissolved in methanol and analyzed using an Acquity UPLC HSS T3 (I.D. 2.1 mm x 10 cm, 1.8 mm) column with 0.1% formic acid and methanol/acetonitrile (75: 25, v/v) solution as eluents under a gradient program. The linear concentrations of 6 standard solutions were in the range of 0.25-10 ng/mL with r2 values greater than 0.995. The average recoveries of 6 compounds spiked into the samples were 90.9-113.8% and the relative standard deviations of average recoveries were less than 13.1%. The limits of quantification were 0.5 mg/g for bromodiphenhydramine, clemastine, diphenhydramine and diphenpyraline and 1 mg/g for carbinoxamine and doxylamine. The test results showed that all of the 25 commercial cosmetics products were compliant with the regulations.