Determination of Coumarin Allergen and Its Derivatives in Cosmetics by HPLC and Their Verification by HPLC-MS/MS
  
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KeyWord:coumarin and its derivatives  allergen  high performance liquid chromatography(HPLC)  high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  cosmetics
  
AuthorInstitution
MENG Xian-shuang,MA Qiang*,YUAN Han-cheng,BAI Hua,ZHANG Qing,GUO Xiang-yu 1.中国检验检疫科学研究院;2.沃特世科技上海有限公司
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Abstract:
      A high performance liquid chromatographic(HPLC) method was developed for the determination of coumarin allergen and its seven derivatives,including dihydrocoumarin,7 methoxycoumarin,7 methylcoumarin,7 ethoxy 4 methylcoumarin,cyclocoumarol,dicoumarol and acenocoumarol in cosmetics.Cosmetic samples were ultrasonically extracted with 0.1 mol/L aqueous sodium hydroxide-acetonitrile(1∶9).The extract was centrifuged,and filtered by microporous membrane.The chromatographic separation for the analytes was achieved on a ZORBAX SB-C18(250 mm×4.6 mm,5 μm) column.Gradient elution was performed using 0.05 mol/L aqueous ammonium acetate solution(containing 0.25% acetic acid) and acetonitrile.The quantification was carried out by the external standard method,and the suspected samples were further verified by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The experimental results indicated that good linearities were observed over a certain concentration range with correlation coefficients better than 0.999 6,and the limits of quantitation(LOQs) were between 8 and 20 mg/kg.The average recoveries for the analytes at three spiked levels ranged from 84.6% to 100.7% with relative standard deviations(RSDs) of 0.8%-9.7%.The proposed method is accurate,robust and specific,and could provide scientific basis and a technical support for the inspection and quality control of cosmetics.
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