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| Determination of Hexamidine,Chlorhexidine and Their Salts in Cosmetics by Ultra Performance Liquid Chromatography and Their Verification by High Performance Liquid Chromatography Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:hexamidine chlorhexidine solid phase extraction(SPE) ultra performance liquid chromatography(UPLC) mass spectrometric verification cosmetics |
| Author | Institution |
| MENG Xian-shuang,MA Qiang,BAI Hua,ZHANG Qing,GUO Xiang-yu,L? Qing |
中国检验检疫科学研究院 |
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| Abstract: |
| Analytical methods were developed for the determination of hexamidine,chlorhexidine and their salts in cosmetics by ultra performance liquid chromatography(UPLC) and verification by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Cosmetic samples of toning lotion,shampoo,powder and cream were firstly demulsificated with saturated sodium chloride solution,and wax type samples(e.g.lipstick) were dispersed with tetrahydrofuran.Water and methanol were then added successively,followed by thorough vortex oscillation.The extraction and clean up procedures were performed using ultrasound assisted extraction and solid phase extraction separately.Afterwards,chromatographic separation was conducted on an ACQUITY UPLC BEH C18 column(2.1 mm × 50 mm,1.7 μm) by a gradient elution of 0.1% aqueous trifluoroacetic acid solution and acetonitrile containing 0.1% trifluoroacetic acid.The detection was completed using a diode array detector(DAD).The external standard method was used for quantitation.Under the optimum conditions,good linearity(r2>0.999 6) was observed over a certain range of concentration.The limits of detection(LODs) and the limits of quantitation(LOQs) were 10 mg/kg and 20 mg/kg,respectively.The mean recoveries at three spiked levels ranged from 81.9% to 97.6%,with relative standard deviations(RSDs) of 0.9%-7.8%.This method was proved to be rapid,accurate,sensitive and high specified,and could be used in the practical determination of commercial cosmetics. |
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