• Title/Summary/Keyword: Extraction Esterification

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Pretreatment method of urinary thiodiglycolic acid as metabolite of vinyl chloride (염화비닐의 요중 대사물질인 thiodiglycolic acid의 분석을 위한 전처리 조건)

  • Hong, Joo Youn;Kim, Chi Nyon;Jung, Jae Hoon;Chang, Jung Hwan;Roh, Jaehoon
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.9 no.1
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    • pp.23-40
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    • 1999
  • The analysis of thiodiglycolic acid in urine has been used as an index of biological exposure to vinyl chloride. Unfortunately thiodiglycolic acid has a strong hydrophilic character, because it has two carboxylic groups, so that it can only be extracted with organic solvent with a great difficulty. Underivatized thiodiglycolic acid tends to tail because of non-specific interaction with the inert support. Therefore, esterification is the obvious first choice for derivatization of thiodiglycolic acid, particularly for gas chromatography. In this study, the focus of interest is to compare two method of esterifications (methylation and silylation). Methylation is to make the methyl ester of thiodiglycolic acid by reaction with diazomethane. Silylation is to make the trimethylsilyl ester of thiodiglycolic acid by reaction with N-trimethylsily-ldiethylamine. The results and conclusions are as the following: 1. The detection limit (sensitivity) of methylated thiodiglycolic acid was $5.00{\mu}g/m{\ell}$ and silylated thiodiglycolic acid was $3.07{\mu}g/m{\ell}$ by gas chromatography with flame ionization detector. 2. The optimal liquid-liquid extraction of thiodiglycolic acid was as following: To each of the tubes, $15m{\ell}$ of urine, concentrated sulfuric acid (pH 1 - 2) and 5 gsodium sulfate were added. The samples was extracted three times with $5m{\ell}$ ethylacetate each time. 3. The methylated thiodiglycolic acid was more stable than silylated thiodiglycolic acid in extractional solvent which contained humidity. 4. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.07324 in methylated thiodiglycolic acid with external standard calibration, and 0.07033 in methylated thiodiglycolic acid with internal standard calibration. 5. The precision (pooled coefficient of variation for 4 days) of the analysis was 0.10914 in silylated thiodiglycolic acid with external standard calibration, and 0.13602 in silylated thiodiglycolic acid with internal standard calibration. From the above results, the analysis of methylated thiodiglycolic acid was more sensitive (limit of detection) than silylated thiodiglycolic acid by gas chromatography. However, the methylated thiodiglycolic acid was stable in the humidity and was separated sharply on chromatogram. Also, analysis of methylated thiodiglycolic acid was more precise (pooled coefficient of variation for 4 days) than silylated thiodiglycolic acid. In conclusion, it is established that the analysis of methylated thiodiglycolic acid is appropriate for biological monitoring of exposure to vinyl chloride.

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Physicochemical Properties and Glucose Transport Retarding Effect of Pectin from Flesh of Asian Pear at Different Growth Stages (생장단계별 배 과육에서 추출된 펙틴의 이화학 특성 및 포도당 흡수 저해 효과)

  • Zhang, Xian;Lee, Fan Zhu;Eun, Jong-Bang
    • Korean Journal of Food Science and Technology
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    • v.40 no.5
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    • pp.491-496
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    • 2008
  • Properties of pectin extracted from flesh of Asian pear in 3 cultivars were investigated at different growth stages. The extraction yields of pectin by the acidic treatment decreased during the growth. The $L^*$ value of young fruit was lower than unripe and ripe fruit, and $a^*$ and $b^*$ value were higher in the same cultivars. The degree of esterification (DE) and intrinsic viscosity of pectin were 21.1-41.3% and 1.90-3.81 dL/g, respectively. The pectin extracted from flesh of pear showed about 30% glucose retarding effect. The DE value had a high correlation with retarding effect on glucose transport and intrinsic viscosity (p<0.01 and p<0.05). The intrinsic viscosity of the pectin seems to affect the retardation of glucose transport in blood. Pectin extracted from flesh of Asian pear by acidic treatment could be a good source to develop low calorie and functional food.

Synthesis and Plasticity of Cyclic Ester Compounds Using Fatty Acids (지방산을 이용한 고리형 에스터 화합물의 합성 및 그의 가소 특성 연구)

  • Han-Na Lee;Hye-Jin Jang;Je-Wan Woo
    • Applied Chemistry for Engineering
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    • v.34 no.3
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    • pp.252-257
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    • 2023
  • In this study, to replace phthalate-based plasticizers known as endocrine disruptors, compounds as plasticizer candidates were synthesized by using alcohols containing rings and fatty acids extracted from animal and vegetable oils, and their properties as plasticizers, including their plasticization efficiency, were evaluated. Nine compounds synthesized by esterification of fatty acids (caprylic acid, capric acid, lauric acid) and alcohols (solketal, benzyl alcohol, cyclohexanol) were identified by 1H-NMR. The nine synthetic compounds were evaluated for their plasticity by adding them to PVC resin, and compared with the commercial plasticizers DEHP, DINCH, and ESO. According to the results, plasticization efficiency was 0.96 to 1.02 times higher than DEHP, 0.94 to 0.98 times higher than ESO, and 1.05 to 1.10 times higher than DINCH. Thermal stability was somewhat lower than that of DEHP and DINCH, but showed better results than ESO. The results of the solvent extraction test showed that both aqueous and oily solvents showed higher values than DEHP and DINCH but showed similar or superior properties to ESO.