• Journal of Environmental Health Sciences
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• v.38 no.6
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• pp.561-567
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• 2012

Objectives: Parabens are widely used as antimicrobial agents in pharmaceuticals and cosmetics as well as by the food industry. Parabens have been reported to show weak estrogenic activity and be related to health effects such as allergic reactions and skin and breast cancer. We evaluated an online solid phase extraction (SPE) method coupled with LC-MS/MS technique using free and conjugated parent parabens in human urine for assessing human exposure to parabens. Methods: We employed LC/MS/MS through online solid phase extraction and column-switching techniques and analyzed free and conjugated parabens as biomarkers of human exposure. Four major parabens, methyl-paraben (MP), ethyl-paraben (EP), propyl-paraben (PP) and butyl-paraben (BP), were analyzed. Method validation was performed by sensitivity, accuracy, precision and comparison of the results of online SPE with offline SPE. Results: The limits of detection (LOD) were in the range of 0.2-2 ng/mL, and actual limits of quantification (LOQ) were in the range of 0.7-6 ng/mL urine, depending upon the compound. Accuracy was in the range of 98.3-106.4%, and precision was in the range of 1.3-8.7% (CV) depending upon the compound. We found a good correlation between the results of analysis by online SPE method and that by off-line SPE method. Conclusions: The online SPE method showed proper LOD and validated accuracy, precision and good correlation with the offline method for analyzing parabens in urine.

• YAKHAK HOEJI
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• v.46 no.4
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• pp.231-236
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• 2002

A high-performance liquid chromatographic method for the simultaneous quantitative analysis of methylparaben (MP), ethylparaben (EP), propylparaben (PP), butylparaben (BP) and imidazolidinyl urea(IU) or diazolidinyl urea(DU) in cosmetics was studied by using a cyano-propyl column and 0.05M hexanesulfonic acid at 228 nm. Calibration curves were found to be linear in the 60-1000 $\mu\textrm{g}$/mL range (parabens), 100-1,250 $\mu\textrm{g}$/mL range (IU) and the 120-2000 $\mu\textrm{g}$/mL range (DU). Linear regression analysis of the data demonstrates the efficacy of the method in terms of precision and accuracy. An extraction method is developed and validated in order to apply this chromatographic method to a commercial cosmetic cream. The precision of this method, calculated as the relative standard deviation (RSD) of the recoveries (0.46-2.71％) was excellent for all compounds.

• Bulletin of the Korean Chemical Society
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• v.34 no.4
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• pp.1131-1136
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• 2013

Parabens, the esters of p-hydroxybenzoic acid, have been widely used as antimicrobial preservatives in cosmetic products, drugs, and processed foods and beverages. However, some parabens have been shown to have weak estrogenic effects through in vivo and in vitro studies. Because such widespread use has raised concerns about the potential human health risks associated with exposure to parabens, we developed a simultaneous analytical method to quantify 4 parabens (methyl, ethyl, propyl, and butyl) in human urine, by using solid-phase extraction and high-performance liquid chromatography coupled with triple quadrupole mass spectrometry. This method showed good specificity, linearity ($R^2$ > 0.999), accuracy (92.2-112.4%), precision (0.9-9.6%, CV), and recovery (95.7-102.0%). The LOQs for the 4 parabens were 1.0, 0.5, 0.2, and 0.5 ng/mL, respectively. This method could be used for quick and accurate analysis of a large number of human samples in epidemiological studies to assess the prevalence of human exposure to parabens.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.32 no.1 s.55
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• pp.65-68
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• 2006

Sensory irritation is one of the important side effects of cosmetics and it is required to develop new products that are more tolerable to the consumers. There are lots of cosmetic ingredients known to induce sensory irritation such as lactic acid, glycolic acid, ethanol, preservatives, fragrances and menthol etc. It is also known that sensory irritation increases by change of pH as well as additional occlusive conditions. The aim of this study is to know various factors affecting sensory irritation due to preservatives (methylparaben, propylparaben, phenoxyethanol and chlorophenecin). We also wanted to investigate the effect of preservatives to sensory irritation according to change of formulations. Our results showed that sensory irritation increased with the conditions of increasing absorption such as packs. We have also found that sensory irritation increased synergistically when to apply two different preservatives together. For example, phenoxyethanol and chlorphenesin themselves have weak sensory irritation potentials, but we observed phenoxyethanol combined with chlorpenesin synergistically increase of sensory irritation potentials. In conclusion, formulation and combination of different preservatives should be considered to reduce the unwanted sensory irritation of preservatives.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.43 no.4
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• pp.381-390
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• 2017

This study was conducted to determine 16 preservatives and 18 UV filter ingredients levels in 100 sunblock products. The order of detection rates of preservatives was phenoxyethanol (n=61), benzoic acid (n=19), methyl paraben (n=11), benzyl alcohol (n=8), propyl paraben (n=7). Also the order of detection rates of UV filter ingredients was titanium dioxide (n=81), ethylhexyl methoxycinnamate (n=69), zinc oxide (n=48), ethylhexyl salicylate (n=48), bis-ethylhexyloxyphenol methoxyphenyltriazine (n=44). The content of the detected preservatives and UV filter ingredients was within maximum allowed amount established by KFDA. In addition, preservatives and UV filter ingredients, which were not labeled in the products, were detected in 31 and 2 products respectively.

• Journal of Food Hygiene and Safety
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• v.21 no.4
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• pp.197-203
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• 2006

Parabens are most wildly used in food, cosmetics and pharmaceutic products as preservatives caused of safety and cheap. we had examined that paraben had estrogenic activity through the in vivo and in vitro experiments in last year. We demonstrated that most of parabens(ethyl, butyl, propyl, isobutyl, isopropyl) increased significantly uterus weight as well as induced proliferation of MCF-7 cell and binding of estrogen receptor as endocrine disrupter compounds. In this study, we evaluated that whether parabens have effect on male reproductive system or not. the male rats were administrated parabens by oral injection then examined separation of preputial day for $PND23\simPND52$. As the results, most parabens delayed pubertal development compare to control group. The separation of preputial day of Butyl and Propyl parabens at high concentration were PND 44 days and PND 45days compared to control group as PND 40 days. Even though, parabens as endocrine disrupter wildly spread in food, cosmetics and pharmaceutic products, we didn't have the safe guideline. In abroad, they are re-evaluating safety assessment for parabens. In conclusion, parabens delayed pubertal development in juvenile parabens are consider as endocrine disrupter chemicals.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.22 no.2
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• pp.201-210
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• 1996

Predictive tests for the identification of contact sensitizing chemicals have been developed. We measured the sensitization potential with three predictive tests, the in vitro and the in vivo Local Lymph Node Assay(LLNA), ELISA to detect interferon-gamma(IFN-${\gamma}$) from supernatant and flow cytometry to detect change of cell surface proteins, using draining lymph nodes of mice. BALB/c mice were exposed to various chemicals or vehicles on the ears daily for 3 consecutive days in all experiments. With some exceptions of propyl paraben, neomycin sulfate, the in vivo LLNA was able to detect the sensitizing capacity of test chemicals and was more sensitive than the in vitro LLNA for chemicals used in the present study. In another experiment, contact sensitivity was assessed by the ELISA to detect IFN-Υ from the supernatants of the cultured LNCs after sensitization with chemicals. There was a good correlation between the LLNA and the IFN-Υ production for test chemicals. We also examined the change of cell surface proteins on LNCs after sensitization by flow cytometry for some cell adhesion molecules(ICAM-1, E-cadherine, B7 molecule), T cell markers(CD3, CD4, CD8, T$\alpha$$\beta$,T${\gamma}$$\delta$) and B cell markers(LR1, CD45R, I-Ad). The number of ICAM-1 positive cells and B cells in LNCs were increased after sensitization with DNCB, TNCB, isoeugenol and 25%, 50% cinnamic aldehyde compared with that of vehicle as a control. In conclusion, the in vivo LLNA could provide more sensitive screening test for moderate to strong sensitizers and some weak sensitizers including cosmetic raw materials than the in vitro LLNA. The production of IFN-Υ by allergen-activated LNCs might be a values indicators without radioisotopes for the identification of contact allergens. Detection of allergens by testing the increase of ICAM-1 positive cells and B cells in LNCs by flow cytometry might be used as a test method to detect allergens.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.45 no.4
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• pp.399-408
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• 2019

Arbutin, which is used as a whitening ingredient, can produce hydroquinone, known as causing skin disease and carcinogen. Preservatives are essential to prevent microbial contamination during long-term storage and use of cosmetics, but safety issues such as toxicity and skin irritation are being raised. This study was conducted to determine hydroquinone and 21 preservatives levels in 40 arbutin-containing whitening functional cosmetics sold on-line and off-line. Result showed that 9 products contained hydroquinone. The concentrations in 7 products were ranged from 0.3 to 0.9 ppm, which were within the maximum allowed amount established by the Ministry of Food and Drug Safety. However, 2 products were 8.4 and 50.5 ppm and exceeded the allowed amount. Preservatives were detected 20 products. Detected items and ranges were phenoxy ethanol 0.1 ~ 0.7% (N = 15), Methyl paraben 0.19 ~ 0.21% (N = 2), Chlorphenesin 0.13% (N = 1), chlorhexidine 0.006% (N = 1), Propyl paraben 0.06% (N = 1), which were within maximum allowed amount established by the Ministry of Food and Drug Safety. Also, in cases of functional cosmetics the phrase "functional cosmetics" should be expressed on the primary or secondary package of cosmetics by cosmetics act. However, 1 product did not state the phrase as functional cosmetics. This study suggest that preservatives were safely managed. However, hydroquinone in hydroquinone-detected products could be produced by the decomposition of arbutin. Thus, further studies on the decomposition of arbutin are required to improve the quality control of the cosmetics.

• Korean Journal of Veterinary Service
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• v.38 no.2
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• pp.127-136
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• 2015

A simultaneous determination method was developed for nine preservatives (benzoic acid, sorbic acid, dehydroacetic acid, methyl-, ethyl-, isopropyl-, propyl-, isobutyl- and butyl-parabens) in sausage by liquid chromatography with electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Each parameter was established by multiple reaction monitoring in negative mode. Separation was achieved on a phenyl-hexyl ($2.5{\mu}m$, $2.1{\times}150mm$, Waters) with A-20 mM ammonium acetate containing 0.1% acetic acid in water, B-Acetonitrile as mobile phase with gradient mode at a flow rate of 0.3 mL/min. The developed method was validated for specificity, linearity, accuracy and precision in sausages samples. Linearity was over 0.998 with calibration curve of the mixed standards. The mean recoveries from sausages fortified at the level of 2.0~10.0 mg/L were in range of 98.60~109.16% with RSDs lower than 8.93%. The limits of detection (LOD) and the limits of quantification (LOQ) were in the range between 0.0003~0.085 mg/L and 0.01~0.257 mg/L, respectively. Intra-day precision and inter-day precision were 0.45~6.16% and 2.81~13.33%, respectively. Using presently developed determination method, 33 field sausage samples from Gwangju city in Korea were screened over nine preservatives. As a result, no preservatives were detected in all samples.