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《Chinese Journal of Chromatography》 2007-02
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Simultaneous Determination of Phthalates and Parabens in Cosmetic Products by Gas Chromatography/Mass Spec-trometry Coupled with Solid Phase Extraction

SHEN Haoyu,YING Liyan,CAO Yunfeng,PAN Gang,ZHOU Lu(Analysis and Testing Center,Ningbo Institute of Technology,Zhejiang University,Ningbo 315100,China)  
Studies have been carried out on the simultaneous determination of 8 phthalates, i.e.di-ethyl phthalate(DEP),di-propyl phthalate(DPP),di-isobutyl phthalate(DIBP),di-butyl phthalate(DBP),benzyl butyl phthalate(BBP),di-cyclohexyl phthalate(DCHP),di-(2-ethylhexyl) phthalate(DEHP),di-octyl phthalate(DOP) and 4 parabens,i.e.methylparaben(MPB),ethylparaben(EPB),propyl paraben(PPB),and butyl paraben(BPB) by gas chromatography in combination with mass spectrometry(GC/MS) in electron ionisation mode(EI) with selected-ion monitoring(SIM) acquisition method.The phthalates and parabens in 15 cosmetic products,including hair sprays,perfumes,deodorants,cream,lotion,etc.were determined.The determination of the samples were performed after sonicationassisted extraction with methanol,cleaned up with an LC-C18 column(3 mL) and analyzed by GC/MS method.The base peak(m/z 149) of the phthalates and the base peak(m/z 121) of the parabens were selected for the screening studies.The characteristic ions,m/z 121,149,177,222 for DEP;m/z 149,191,209 for DPP;m/z 57,149,223 for DIBP;m/z 104,149 for DBP;m/z 91,132,149,206 for BBP;m/z 55,149,167 for DCHP;m/z 113,149,167,279 for DEHP;m/z 149,279 for DOP;m/z 65,93,121,152 for MPB;m/z 93,121,138,166 for EPB;m/z 93,121,138,180 for PPB;and m/z 93,121,138,194 for BPB were chosen for quantitative studies.These techniques are capable to detect phthalates and parabens at the level of 0.1-5.0 μg/kg.Overall recoveries were 80%-100% with relative standard deviations(RSDs) less than 10%.Only one of the 15 examined samples was free from phthalates and parabens.The rest 14 samples were found to contain at least 3 or more of these phthalates and/or parabens.The predominant phthalates detected in the studied samples were MPB,PPB,DPP,DCHP and DEHP.The residue levels were at 1.42-4 278 mg/kg.
【Fund】: 宁波市科技攻关资助项目(2004C10065);; 浙江大学宁波理工学院创新基金资助项目
【CateGory Index】: TQ658;O657.63
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