• 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 $25{\mu}g/g$.

• Journal of Environmental Health Sciences
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• v.34 no.4
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• pp.271-278
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• 2008

Dialkylated phthalates have been commonly used as plasticizers and a variety of applications. Phthalate diesters have been shown to be developmental and reproductive toxicants. It is very difficult to exactly estimate the dose of dialkylated phthalates taken up by the general population because of environmental contamination. Urinary metabolites of phthalates enabled to estimate internal exposure. The objective of this study was quantitative determination of phthalate metabolites by LC/MS/MS with on-line cleanup method to analyze phthalate metabolites in Korean children's urine. We employed LC/MS/MS with on-line enrichment and column-switching techniques for this biological monitoring. Metabolites determined were 4 primary metabolites; MEHP, MnBP, MiBP, MEP and 2 secondary metabolites of DEHP; 5-OH-MEHP), 5-oxo-MEHP. We analyzed children's urine from 30 boys and 30 girls. The method detection limit of phthalate metabolites were 0.03 ng/mL for MEP, 1.05 ng/mL for MBP, 0.22 ng/mL for MEHP, 0.15 ng/mL for 5-OHMEHP and 0.16 ng/mL for 5-oxo-MEHP, respectively. Switching Column LC/MS/MS was proven to be a useful tool to determine metabolites of phthalate diesters in human urine. The correlation among phthalate metabolites was very high and statistically significant, except MEP. The children's age (months) was negatively correlated to the concentration of phthalate metabolites. The geometric mean concentration of phthalate metabolites (mg/g creatinine) in children's urine were 25.5 for MEP, 130.3 for MnBP, 56.8 for MiBP, 19.5 for MEHP, 85.6 for 5-OH-MEHP and 83.1 for 5-oxo-MEHP, respectively. Levels of estimated daily intake of parent phthalate compounds (${\mu}g$/kg bw/day) were 0.8 for DEP, 5.0 for DnBP, 1.9 for DiBP and $8.9{\sim}14.2$ for DEHP, respectively. Estimated daily intake for DEP and DiBP were lower than those of other studies but the value for DEHP was higher than that of other study.

• Journal of Environmental Health Sciences
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• v.49 no.6
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• pp.324-333
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• 2023

Background: Human exposure to phthalates in indoor environments occurs via dermal absorption, oral ingestion of indoor dust, and inhalation of indoor air. However, systematic studies to investigate the exposure rate to phthalates among the three exposure routes in indoor environments are currently limited. Objectives: A theoretical exposure ratio between inhalation and oral exposure was calculated based on the total amount of di(2-ethyl-hexyl) phthalate (DEHP) emitted into indoor air and deposited into floor dust in a test house. Methods: Flooring and wallpaper containing DEHP were installed in a test house and the concentration of DEHP in both indoor air and floor dust were monitored for five months. Based on the measured DEHP concentrations, the theoretical total amount ratio of DEHP that could be exposed through inhalation and oral ingestion was calculated. Results: Considering the period of operation in the test house, the theoretical total amount of DEHP through inhalation and oral ingestion exposures in the entire test house space was calculated to be 0.014 mg and 5.5 mg, respectively. The exposure ratio of the two routes between inhalation and oral exposure corresponding to the total DEHP amount in flooring and wallpaper was 6.0×10^-7% and 2.3×10^-4%, indicating that theoretical oral exposure to DEHP is approximately 380 times higher than inhalation. Conclusions: Monitoring results from a test house has shown that oral exposure is the main exposure route for DEHP in indoor environments. The experimental design employed in this study and theoretical exposure ratio obtained can be applied to investigate actual exposure to DEHP and to determine the exposure characteristics of various types of semi-volatile organic compounds.

• Bulletin of the Korean Chemical Society
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• v.26 no.5
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• pp.815-818
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• 2005

• Proceedings of the Korean Environmental Sciences Society Conference
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• 2004.05a
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• pp.274-275
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• 2004

본 연구결과로 부터, Phenols, Alihatic compounds, Aromatic compounds, Phthalates, Pesticides와 같은 유기오염물질로 인한 영산강 유역 방류수의 오염을 알 수 있었고, 하수 성상별, 계절별로 검출된 물질을 보면 농공 폐수가 생활하수보다 다종의 유기오염물질들을 포함하고 있음을 알 수 있었다. 특히 여름철에 다량의 농약 사용으로 인해 Pesticides가 다종 고농도로 검출되었으며, Phenols, Phthalates는 주변공장의 제조과정에서 발생된 유기물질들에 의한 오염으로 추측된다. 또한, 검출 화학물질 중에서 dieldrin, edosulfan, diethyl phthalates와 같은 환경호르몬성 물질이 포함되었다.

• Proceedings of the PSK Conference
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• 2000.10a
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• pp.169.1-169.1
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• 2000

• Journal of Korean Society for Atmospheric Environment
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• v.25 no.5
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• pp.382-391
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• 2009

The aim of the study was to assess the levels in typical central borough of phthalate exposure by monitoring children's facilities (19 kindergartens and 21 elementary schools) and households (17 old apartments and 22 new apartments) via sampling indoor floor dust. A vacuum cleaner specifically prepared for sampling dust was attached to a filter of a vacuum cleaner dust collecting container. During the sample preparation process, containers made of glass were used and analysis was performed using GC-MSD. The mean concentration of DEHP was $412{\mu}g/g$, DnBP was $24{\mu}g/g$, and BBzP was $10{\mu}g/g$ dust. The indoor characteristics including floor, wall materials, years after construction, water leakage history for the past three years, and ventilation were also examined to categorize phthalate esters from the dust samples. From the flooring and wallpaper materials of kindergartens and elementary schools, DEHP in the dust sample appeared at a statistically significant level (p<0.05) when PVC materials were present. DEHP in the indoor dust also increased significantly (p<0.01) during the construction period. The daily intake of DEHP measured from indoor dust was 0.08~$19.7{\mu}g/kg/day$ for children and 0.02~$1.1{\mu}g/kg/day$ for adults (women). The results clearly revealed that phthalate exposure is greater in children than in adults (women) due to the indoor dust.

• Journal of Environmental Health Sciences
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• v.36 no.6
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• pp.510-517
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• 2010

Phthalates, such as di (2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP) have been proved to be teratogenics and endocrine disruptors, metabolized rapidly and excreted in the urine. In this study, a simultaneous analytical method for 10 phthalate metabolites, MnBP, MiBP, MBzP, MCHP, MEHP, MEHHP, MEOHP, MnOP, MiNP and MiDP, in human urines, based on switching system with on-line pretreatment column using HPLC-MS/MS has been developed. This method was validated according to the guideline of bioanalytical method validation of National Institute of Toxicological Research. Limits of detection range between 0.2 and 0.9 ng/ml for 10 phthalate metabolites. The calibration curves showed linearity in the range 0.997~0.999, and the results of the intra- and inter-day validations were in the range from 0.4 to 14.7% RSD and from 0.3 to 9.4% RSD, respectively. Recoveries of phthalate metabolites varied from 87.0 to 116.1%. This analytical method showed high accuracy and stable precision for all metabolites, and seems to be suitable for biomonitoring of phthalates in human urine.

• Environmental Mutagens and Carcinogens
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• v.22 no.4
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• pp.259-265
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• 2002

Phthalate analogues are a plasticizer and solvent used in industry. Phthalates were reported to be a potential carcinogen classified in the category of suspected endocrine disruptors. Most common human exposure to these compounds may occur with contaminated food. They may migrate into food from plastic wrap or may enter food from general environmental contamination. Since these substances are not limited to the original products, and enter the environment, they have become widespread environmental pollutants, thus leading to a variety of phthalates that possibly threaten the public health. Concern about their use has been mounting. To screen and elucidate the endocrine disrupting activity and their mechanism of phthalate analogues, first of all, E-screen assay was performed in MCF7 human breast cancer cells with seven phthalate analogues. In this cell proliferation assay, only dibutyl phthalate (DBP) showed weak estrogenic activity. Also the yeast-based transcription assay to assess the interactions of DBP with the estrogen, androgen, and progesterone receptors was conducted. DBP in the concentration ranges from 10$^{-16}$ to 10$^{-11}$ M was active in the estrogen transcriptional assay, but it did not show the effect on $\beta$-galactosidase activity in the progesterone and androgen transcriptional assays. These data indicate that DBP shows estrogenic potential and can be classified as weak and/or suspected endocrine disrupting chemicals.

• Journal of Korean Society of Environmental Engineers
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• v.32 no.5
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• pp.455-460
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• 2010

This study was carried out to find out any inherent problems occurring in the sampling and analytical procedures, and to suggest the relevant solutions to the problems. In addition, an optimal condition of clean-up process was developed, which was based on a method using silica glass column. As a result of experiments to test any artificial contamination of blank samples such as glassware and collection media, artifacts of DBP and DEHP appeared to be detected in various kinds of laboratory tools and apparatuses used in the sampling and analytical works. Therefore, it is necessary to investigate a degree of contamination before laboratory works by conducting a prior check any possible contaminations in all experimental tools and apparatus. It is also necessary to devise a method to avoid a tool, if possible, or to use a substitute of phthalate free. If the use of any plastic tool to cause contamination is inevitable, it should be properly corrected with a blank level, as is equally treated as the sample. The clean-up process demonstrated in this study can give us a significant benefit in terms of the quantity and quality of a target compound by GC/MS analysis.