[Simultaneous determination of phthalates and parabens in cosmetic products by gas chromatography/mass spectrometry coupled with solid phase extraction]. 2007

Haoyu Shen, and Liyan Ying, and Yunfeng Cao, and Gang Pan, and Lu Zhou
Analysis and Testing Center, Ningbo Institute of Technology, Zhejiang University, Ningbo 315100, China. haoyushen2000@yahoo.com

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) , dibutyl 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 sonication-assisted 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 microg/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.

UI MeSH Term Description Entries
D008401 Gas Chromatography-Mass Spectrometry A microanalytical technique combining mass spectrometry and gas chromatography for the qualitative as well as quantitative determinations of compounds. Chromatography, Gas-Liquid-Mass Spectrometry,Chromatography, Gas-Mass Spectrometry,GCMS,Spectrometry, Mass-Gas Chromatography,Spectrum Analysis, Mass-Gas Chromatography,Gas-Liquid Chromatography-Mass Spectrometry,Mass Spectrometry-Gas Chromatography,Chromatography, Gas Liquid Mass Spectrometry,Chromatography, Gas Mass Spectrometry,Chromatography, Mass Spectrometry-Gas,Chromatography-Mass Spectrometry, Gas,Chromatography-Mass Spectrometry, Gas-Liquid,Gas Chromatography Mass Spectrometry,Gas Liquid Chromatography Mass Spectrometry,Mass Spectrometry Gas Chromatography,Spectrometries, Mass-Gas Chromatography,Spectrometry, Gas Chromatography-Mass,Spectrometry, Gas-Liquid Chromatography-Mass,Spectrometry, Mass Gas Chromatography,Spectrometry-Gas Chromatography, Mass,Spectrum Analysis, Mass Gas Chromatography
D010226 Parabens Methyl, propyl, butyl, and ethyl esters of p-hydroxybenzoic acid. They have been approved by the FDA as antimicrobial agents for foods and pharmaceuticals. (From Hawley's Condensed Chemical Dictionary, 11th ed, p872) 4-Hydroxybenzoic Acids,Paraben,para-Hydroxybenzoic Acids,4 Hydroxybenzoic Acids,para Hydroxybenzoic Acids
D010795 Phthalic Acids A group of compounds that has the general structure of a dicarboxylic acid-substituted benzene ring. The ortho-isomer is used in dye manufacture. (Dorland, 28th ed) Acids, Phthalic
D003358 Cosmetics Substances intended to be applied to the human body for cleansing, beautifying, promoting attractiveness, or altering the appearance without affecting the body's structure or functions. Included in this definition are skin creams, lotions, perfumes, lipsticks, fingernail polishes, eye and facial makeup preparations, permanent waves, hair colors, toothpastes, and deodorants, as well as any material intended for use as a component of a cosmetic product. (U.S. Food & Drug Administration Center for Food Safety & Applied Nutrition Office of Cosmetics Fact Sheet (web page) Feb 1995) Personal Care Products,Care Product, Personal,Care Products, Personal,Personal Care Product,Product, Personal Care,Products, Personal Care
D015203 Reproducibility of Results The statistical reproducibility of measurements (often in a clinical context), including the testing of instrumentation or techniques to obtain reproducible results. The concept includes reproducibility of physiological measurements, which may be used to develop rules to assess probability or prognosis, or response to a stimulus; reproducibility of occurrence of a condition; and reproducibility of experimental results. Reliability and Validity,Reliability of Result,Reproducibility Of Result,Reproducibility of Finding,Validity of Result,Validity of Results,Face Validity,Reliability (Epidemiology),Reliability of Results,Reproducibility of Findings,Test-Retest Reliability,Validity (Epidemiology),Finding Reproducibilities,Finding Reproducibility,Of Result, Reproducibility,Of Results, Reproducibility,Reliabilities, Test-Retest,Reliability, Test-Retest,Result Reliabilities,Result Reliability,Result Validities,Result Validity,Result, Reproducibility Of,Results, Reproducibility Of,Test Retest Reliability,Validity and Reliability,Validity, Face
D052616 Solid Phase Extraction An extraction method that separates analytes using a solid phase and a liquid phase. It is used for preparative sample cleanup before analysis by CHROMATOGRAPHY and other analytical methods. Extraction, Solid Phase,Extractions, Solid Phase,Solid Phase Extractions

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