• 한국산업보건학회지
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• 제9권1호
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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.

• Bulletin of the Korean Chemical Society
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• 제33권12호
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• pp.3943-3949
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• 2012

A series of aromatic hydrazides 3a-j were prepared by refluxing esters 2a-j with hydrazine hydrate in methanol, which were prepared by the esterification of 1a-j. Acetohydrazides 3a-j upon treatment with carbon disulfide and methanolic potassium hydroxide yielded potassium dithiocarbazate salts 4a-j, which on refluxing with hydrazine hydrate yielded substituted 4-amino-5-aryl-3H-1,2,4-triazole-3-thiones 5a-j. The target compounds 6a-j were synthesized by condensing furan-3-carboxylic acid in the presence of polyphosphoric acid under reflux. The structures of newly synthesized compounds were characterized by IR, $^1H$ NMR, $^{13}C$ NMR, elemental analysis and mass spectrometric studies. All the synthesized compounds were screened for their urease, acetylcholine esterase inhibition, antioxidant and alkaline phosphatase inhibition activity. Almost all of the compounds 6a-j showed good to excellent activities against urease and acetylcholine esterase more than the reference drugs. Compounds 6f and 6g were more potent scavenger of free radicals than the reference n-propyl gallate. Compound 6b and 6h showed excellent activities of alkaline phosphatase as compare to the reference $KH_2PO_4$.

• 공업화학
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• 제24권5호
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• pp.530-536
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• 2013

경유의 윤활성향상제로 사용하기 위하여 식물유 기반 다이머산 유도체를 합성하여 윤활성능을 평가하였다. 다이머산 유도체의 합성은 2단계의 반응을 거쳐 합성하였는데, 1단계 반응으로 폐식물유(다크오일)를 가수분해반응을 통하여 합성한 지방산을 사용하여 고온에서 디엘스-알더 반응을 행하여 다이머산을 합성하였다. 2단계 반응으로 합성한 다이머산을 사용하여 메탄올과 에스테르화 반응을 행하여 다이머산 유도체를 합성하였다. 합성한 다이머산 유도체는 1 wt% 범위 내에서 초저유황 경유에 잘 용해되었으며 일정량(120 ppm)을 초저유황 경유에 첨가하여 HFRR 시험법으로 마모흔을 측정하여 윤활성능을 평가하였다. 그 결과, 첨가 전 초저유황 경유의 마모흔의 직경이 $552{\mu}m$에서 첨가 후 $300{\sim}05{\mu}m$으로 현저히 작아져 초저유황 경유의 윤활성능을 향상하는 것으로 확인되었다. 한편, 식물유의 종류에 따른 마모흔의 차이는 크지 않아 다이머산 유도체의 알킬기의 구조에 따른 윤활성능의 차이는 크게 나타나지 않았으나, 카르복실산 그룹을 함유하는 다이머산 유도체가 함유하지 않은 유도체보다 윤활성능이 우수하였다.

• 대한핵의학회지
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• 제28권2호
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• pp.167-171
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• 1994

Ethylcystein dimer (ECD) was synthesized by dimerizatlon of L-thiazolidine-4-carboxylic acid in liquid ammania with sodium metal and successive esterification in ethanolic solution of hydrogen chlorde. The purified product was labeled with $^{99m}Tc$ in the presence of sodium glucarate(pH= 5.6) and stannous chloride. Best result was obtained from the preparation con sisting of 0.1mg ECD, $40{\mu}l$ of 0.4M sodium glucarate (pH=5.6), and $20{\mu}g$ of stannous chloride. The labeling efficiency was 90% with previous condition. The labeled $^{99m}Tc$-ECD was stable at least for 3 hours in PBS(pH=7.4) at room temperature. About 10mCi of $^{99m}Tc$-ECD was injected to normal volunteer, and SPECT image of brain was obtained by triple head camera 10 minutes after inection. The image showed similar distribution of radioactivity in brain with that of HMPAO image.

• Korean Chemical Engineering Research
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• 제54권4호
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• pp.510-518
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• 2016

본 연구에서는 폴리에틸렌글리콜-카르복실산과 에틸셀룰로스 사이의 에스테르화 반응을 통해 에틸셀룰로스-폴리에틸렌글리콜 가지형 고분자를 합성하고 이를 정삼투 수처리 공정을 위한 복합막의 지지체 소재로 사용하고자 하였다. 합성한 에틸셀룰로스-폴리에틸렌글리콜은 핵자기공명 분광법 및 푸리에 변환 적외선 분광법을 통해 그 구조를 확인하였다. 비용매 유도 상분리법을 통해 에틸셀룰로스-폴리에틸렌글리콜 소재를 이용한 지지체를 형성하여 이를 에티셀룰로스 지지체와 비교해 보았을 때, 폴리에틸렌글리콜 작용기의 도입으로 인하여 친수성이 증가한 것을 확인하였다. 지지체 위에 계면중합을 통해 폴리아미드 활성층이 추가된 복합막을 형성하였고, 염화나트륨 용액을 유도 용액으로 사용하여 cross-flow 방식의 정삼투 수처리 장치에서의 성능을 비교하였다. 2M 농도의 염화나트륨 수용액을 유도 용액으로 사용하였을 때, 6.6 LMH의 수투과도를 보이는 에틸셀룰로스 지지체를 사용한 복합막에 비해, 에틸셀룰로스-폴리에틸렌글리콜 지지체를 사용한 복합막은 15.7 LMH의 증가된 수투과도를 보여주었으며, 이는 지지체의 증가된 친수성에서 기인한 것이다. 이러한 결과는 에틸셀룰로스-폴리에틸렌글리콜 지지체를 이용한 복합막의 막구조 파라미터가 감소한 것에서도 설명할 수 있으며, 지지체 소재의 친수성 증가가 정삼투 공정에 최적화된 복합막 지지체 구조를 형성할 수 있음을 시사한다.