• Title/Summary/Keyword: gas chromatography with mass spectrometric detector

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Accurate Analysis of Trace Phthalates and Method Validation in Cosmetics using Gas Chromatography with Mass Spectrometric Detection (화장품에 함유된 미량의 프탈레이트 함량을 정확히 분석하기 위한 가스크로마토그래피-질량분석 시험법 및 그 시험법의 유효성)

  • Kim, Min-Kee;Jeong, Hye-Jin;Cho, Jun-Cheol
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.38 no.1
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    • pp.33-41
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    • 2012
  • An effective, environmentally friendly analytic methods using gas chromatography with mass spectrometric detector (GC-MSD) have been developed for the quantitative analysis of trace phthalate levels in cosmetics such as nail lacquer and hair spray. Since such cosmetics are largely comprised of organic solvents, conventional clean-up methods that have been widely used for phthalate analyses are in adequate. In addition, analysis of trace phthalate levels is notorious for its sensitivity to contamination, which causes high analytical values. A direct sample dilution method using an organic solvent was adopted to the sample preparation process to determine the exact amounts of phthalates and simultaneously avoid the high risk of secondary contamination. The method has many advantages including high accuracy, sensitivity, and simplicity in sample preparation. Dibutyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) were selected for analysis because they have been frequently detected in cosmetics and consistently reported as endocrine disruptors in humans and animals. Internal standard method using two deuterium substitutes (DBP-$d_4$, DEHP-$d_4$) as the internal standard was also used. The results of 'Method validation' showed the capabilities of this method for the routine analysis of phthalates at the ppm level. The recovery ranges were between 95 % and 106.1 %, and relative standards deviations (RSD) were less than 3.9 % in fortified nail lacquer and hair spray samples at the concentration of $25{\mu}g/g$.

Simple Method in Trace Analysis of Phthalates in Cosmetics : Analytical Conditions and Skills for Better Results (화장품에서 프탈레이트 미량분석을 위한 간편한 분석법 : 향상된 결과를 위한 분석조건과 기술)

  • Kim, Min-Kee;Jung, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.34 no.1
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    • pp.51-55
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    • 2008
  • Although phthalates aren't used as an cosmetic ingredient, some cosmetics especially nail lacquer, hair spray, and perfume still have phthalates. This is mainly caused by contamination and carryover during manufacturing process, so analysis of phthalates in those cosmetics has became a very important thing for quality-assurance(Q.A). The main phthalates under debate are diethyl phthalate(DEP), dibutyl phthalate(DBP), and bis(2-ethylhexyl) phthalate (DEHP) in domestic market. Gas chromatography-mass spectrometry(GC-MS) coupled with solvent extraction and concentration has been used for ppm level and sub ppm level analysis of phthalates. It requires much time and cost to use mass spectrometric detector and to prepare the test solution. Moreover analysis of phthalates at low concentrations is difficult because of contamination which results in wrong analytical results. In the present study, we showed a simple method using gas chromatography-flame ionization detector(GC-FID) which has fast analysis time, minimum use of solvent, reduced sample preparation steps for minimizing contamination and quantitative range of $2{\sim}50{\mu}g/g(ppm)$ in products. Consequently, this method will be proper for Q.A analysis in related companies.

A Proposal of Standard Method for the Analysis of Total Petroleum Hydrocarbons (TPHs) in Marine Sediments and Biota (해양환경시료(해저퇴적물과 해양생물)에 축적된 석유계총탄화수소(TPHs) 분석에 대한 공정시험기준 제안)

  • Kim, Chang-Joon;Hong, Gi-Hoon;Jeon, Ji-Yeun;Kim, Suk-Hyun
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.13 no.4
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    • pp.249-262
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    • 2010
  • Regulatory test method for Total Petroleum Hydrocarbons (TPHs) in the marine sediment and biota has not still been established even though TPHs are one of the major pollutants in marine environment. Based on the Korean Soil Standard Method (SSM) for TPHs, we considered a new treatment method for determining TPHs in marine environmental samples by using a Gas chromatography coupled with Mass spectrometric detector. We suggested an improved recovery test for quality control procedures and introduced analytical procedures of removing sulfur, polar organic materials, water and saponification for removing neutral lipids in marine bottom sediments and biota.