• Title/Summary/Keyword: solvent-free

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Three Component Solvent-free Synthesis of Chroman-2,4-dione-based Heterocyclic Ketene Aminal (HKA) Derivatives by "GAP" Chemistry

  • Yu, Fu-Chao;Hao, Xiao-Pan;Jiang, Xiu-Yang;Yan, Sheng-Jiao;Lin, Jun
    • Bulletin of the Korean Chemical Society
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    • v.35 no.6
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    • pp.1625-1632
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    • 2014
  • A concise and efficient one-pot synthesis of chroman-2,4-dione-based HKA derivatives by three component reaction of HKAs, triethoxymethane and 4-hydroxycoumarin derivatives under solvent-free and catalyst-free conditions is described. This protocol has many advantages, in that the GAP (Group-Assistant-Purification) chemistry process is involved in this method. As a result, the experimenter can avoid cumbersome process steps such as traditional chromatography and recrystallization purifications. The desired products can be easily obtained by washing the crude products with 95% EtOH.

A Study on the Synthesis of Acrylic Phenol Resins and Their Properties as a Paint (아크릴계 페놀수지 합성과 이를 이용한 도료의 물성연구)

  • Hwang, Sue In;Kim, Young Jin;Kim, Dong Kwon
    • Applied Chemistry for Engineering
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    • v.24 no.2
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    • pp.171-176
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    • 2013
  • The need of volatile organic compound (VOC) free coating material has been increased to solve environmental problems such as the global warming. Nowadays, about 70~80% of coating materials used in the worldwide are a liquid type. Therefore, the development of non-solvent coating material that can minimize VOCs emissions is necessary to solve the global warming problem. In this study, acrylic monomers were added to develop non-solvent paints in order to improve disadvantages of the poor adhesion of a conventional phenolic resin caused by acidification. As a result, the blend resins of 2.818 Mpa phenol- formaldehyde resin/poly methyl methacrylate (PE/PMMA) has the best properties and performances for the adhesives.

Quality Characteristics of Centella asiatica Species and Antioxidant Activities of Solvent Extracts (병풀 품종별 품질 특성 및 추출 용매별 항산화 활성)

  • Lee, Kyung-Haeng;Yu, Kwang-Won;Bae, Yun-Jung;Kim, Chae-Young;Joo, Ga-Young;Yun, Ji-Hye
    • The Korean Journal of Food And Nutrition
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    • v.34 no.3
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    • pp.255-262
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    • 2021
  • Centella asiatica (CA) is a vegetable that has been used for medicinal purposes for a long time, but it is not well known in Korea. In this study, the approximate analysis, physicochemical properties, free sugars, free amino acids and minerals of native and improved CA cultivated in Chungju area were measured. And the antioxidant contents and activities of CA solvent extracts were measured. There was no significant difference between native and improved species. As for the characteristics of CA, it was confirmed that the improved species had a large weight, size and a tough texture. Glucose was detected in native CA, fructose, glucose and sucrose were detected in improved species. A total of 15 free amino acids were detected and the content was slightly higher in improved species than in native species. The mineral content in CA was slightly higher in the improved species, and the detected minerals were Na, P, Ca, K, Mg and Fe. Polyphenols, ascorbic acid and flavonoids in each extraction solvent (water, 70% and 100% ethanol) were all higher in the improved species than in native species. And it was found that the antioxidant activities of ethanol extracts were higher than that of water.

The Analysis of Volatile Components of Fresh Ginseng, Red Ginseng and White Ginseng by Solvent Free Solid Injector (SFSI) Techniques (Solvent Free Solid Injector (SFSI)를 이용한 수삼, 홍삼, 백삼의 향기성분 분석방법)

  • Kim, Mi-Ra;Kim, In-Hae;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.24 no.2
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    • pp.164-168
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    • 2005
  • An experimental design has been used to optimize the analysis of volatile component from fresh ginseng using solvent free solid injector (SFSI). The analysis were performed at three different sample preparing methods (fresh, oven drying and freezed drying), different injector port temperatures (100, 150, 200, 250 and $300^{\circ}C$) and different preheating time (3, 5, 7, 10 and 15 min) according to the above experimental design. The optimum conditions from analytical results were fresh sample (sample preparing methods), $250^{\circ}C$ (injector temperature) and 10 min (preheating time). Ginsengs grown for six years at Gumsan were prepared for fresh, white and red ginsengs. These fresh, white and red singsengs were analyzed for their volatile components by GC/MS equipped with SFSI according to the above the optimum conditions. A total of thirty-three volatile components were identified in fresh ginseng by SFSI, thirty-six in white ginseng and thirty-eight in red ginseng. These results suggested that the SFSI method could be used for isolating volatile component in ginsengs.

Development of the analytical method for pesticide residues in crops by using gas chromatograph / solvent free solid injector (GC / SFSI) (무용매 고체 시료 주입기(SFSI)를 이용한 작물 중 잔류농약의 기체크로마토그래피 분석법 개발)

  • Kim, M.R.;Lee, Y.;Park, B.J.;Choi, J.H.;Kim, I.S.;Shim, J.H.
    • The Korean Journal of Pesticide Science
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    • v.9 no.3
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    • pp.237-242
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    • 2005
  • This experiment was carried out to develop the fast and simple method for pesticide residue analysis by using solvent free solid injector (SFSI) and to validate the efficiency of the method developed for the residue analysis of the endocrine disruptor-like pesticides such as endosulfan, metribuzin, trifluralin and vinclozolin. The samples after freeze drying were sealed in glass capillary tubes and then introduced into the heated injector of gas chromatogaphy. The required pre-heating times were 1 min for endosulfan and trifluralin, 5 min for vinclozolin, and 10 min for metribuzin. The detection limits of endosulfan in chinese cabbages, metribuzin in lettuces, trifluralin in spinachs and vinclozolin in hot peppers were 0.05, 0.1, 0.05 and 0.05 ng, respectively and their recoveries were ranged from 74%, $98{\sim}107%$, $86{\sim}95%$ and $94{\sim}95%$, respectively. The detected level of metribuzine residue in field lettuce samples by using the SFSI was 0.6 ng/mg.

fabrication of Ceramic Tape By Ultrasonic Spray (초음파 분무를 이용한 세라믹 테이프의 성형)

  • 윤정한;박양수;심수만;이해원
    • Journal of the Korean Ceramic Society
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    • v.36 no.6
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    • pp.625-631
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    • 1999
  • Ceramic tapes were fabricated by ultrasonically spraying slurries of monodispersed spherical and alumina powders. Effects of slurry compositions on tape forming were investigated. A relatively fast rate of solvent evaporation caused pores and cracks to be formed. A good chemical affinity between solvent and binder gave rise to binder separation resulting in inhomogeneous distribution of binder. Defect-free silica tapes with uniform distribution of particle packing and the binder were obtained from the solvent having a low chemical affinity and a slow evaporation rate and containing appropriate amounts of the binder and the plasticizer. Tape thickness could be controlled by adjusting solids loadings and slurry feed rates. It was possible to fabricate a tape in 15 $\mu\textrm{m}$ thickness from 7 vol% alumina slurry.

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Norfloxacin Release from Surfactant-Free Nanoparticles of Poly(DL-lactide-co-glycolide) and Biodegradation (계면활성제를 사용하지 않는 Poly(DL-lactide-co-glycolide) 나노입자로부터의 Norfloxacin 방출과 생분해 특성)

  • 권중근;정영일;장미경;이창형;나재운
    • Polymer(Korea)
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    • v.26 no.4
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    • pp.535-542
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    • 2002
  • We have prepared the surfactant-free nanoparticles of poly(DL-lactide-co-glycolide) (PLGA) by dialysis method and their physicochemical properties such as particle size and drug contents were investigated against various solvent. The size of PLGA nanoparticles prepared by using dimethylacetamide (DMAc), dimethylformamide (DMF), and dimethylsulfoxide (DMSO) was smaller than that from acetone. Also, the order of drug contents was DMAc>DMF>DMSO=acetone. These phenomena could be expected from the fact that solvent affects the size of nanoparticles and drug contents. The PLGA nanoparticles have a good spherical shapes as observed from scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Also, surfactant-free nanoparticles entrapping norfloxacin (NFx) have a good drug loading capacity without free-drug on the surface of nanoparticles confirmed by the analysis of X-ray powder diffraction. Release kinetics of NFx used as a model drug was governed not only by drug contents but also by particle size. Also, the biodegradation rate of PLGA nanoparticles prepared from DMF was faster than that prepared from acetone, indicating that the biodegradation of PLGA nanoparticles is size-dependent.

Comparison of Free Amino Acids in Soybean Paste (Doenjang) by Different Extraction Solvents and Analytical Methods (추출 용매와 분석 기법에 따른 된장의 유리아미노산 비교)

  • Kang, Ok-Ju
    • Korean journal of food and cookery science
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    • v.23 no.1 s.97
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    • pp.150-155
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    • 2007
  • This work was conducted to obtain a rapid, accurate, and precise procedure for free amino acids analysis in Doenjang with HPLC-OPA (high performance liquid chromatography using-phthalaldehyde) and AAA (automatic amino acid analyzer) methods. Different sample extraction procedures among water, 0.1 M perchloric acid, and 0.1% meta-phosphoric acid were also compared. The optimal extraction solvent was 0.1% meta-phosphoric acid for both the HPLC-OPA and AAA methods. Good recoveries for glycine and methionine were observed using the 0.1% meta-phosphoric acid extraction with HPLC-OPA method. Method precisions (% relative standard deviation) for the free amino acids ranged for 1.62% to 8.27%, in which the HPLC-OPA method with water extraction showed the lowest value at 1.62%. Inhibition rates of the free amino acids in Doenjang were greatest with an addition of NaCI at a 1% concentration.

Effect of Template Removal on Synthesis of Organic-Inorganic Hybrid Mesoporous MCM-48

  • Zhao, Ya Nan;Li, San Xi;Han, Chong-Soo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3196-3202
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    • 2012
  • Post-synthesis is used to synthesize organic hybrid inorganic mesoporous sieves. In this method, the activity and structure of the base sieve are crucial to obtain the definable hybrid materials. The chemical and physical properties of the base can be largely changed either by the final step of its synthesizing processes, by template removal which is accomplished with the oxidative thermal decomposition (burning) method or by solvent extraction method. In this paper we compared two methods for the post-synthesis of organic hybrid MCM-48. When the template was extracted with HCl/alcohol mixture, the final product showed larger pore size, larger pore volume and better crystallinity compared to the case of the thermal decomposition. The reactivity of the surface silanol group of template free MCM-48 was also checked with an alkylsilylation reagent $CH_2=CHSi(OC_2H_5)_3$. Raman and $^{29}Si$ NMR spectra of MCM-48 in the test reaction indicated that more of the organic group was grafted to the surface of the sample after the template was removed with the solvent extraction method. Direct synthesis of vinyl-MCM-48 was also investigated and its characteristics were compared with the case of post-synthesis. From the results, it was suggested that the structure and chemical reactivity can be maintained in the solvent extraction method and that organic grafting after the solvent extraction can be a good candidate to synthesize a definable hybrid porous material.

Anti-Inflammatory Activity of the Solvent-Partitioned Fractions from Spergularia marina in LPS-Stimulated RAW 264.7 Cells

  • Kong, Chang-Suk
    • Preventive Nutrition and Food Science
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    • v.19 no.4
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    • pp.261-267
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    • 2014
  • As a part of ongoing research to elucidate and characterize antioxidant and anti-inflammatory nutraceuticals, solvent-partitioned fractions from Spergularia marina were tested for their ability to scavenge radicals and suppress inflammation. The results of the 2',7'-dichlorofluorescein diacetate assay indicate that solvent-partitioned fractions from S. marina scavenged intracellular radicals in $H_2O_2$-stimulated mouse macrophages. The tested fractions decreased the generation of nitric oxide (NO) and the expression of inflammation mediators, namely, inducible nitric oxide synthase (iNOS) and interleukin (IL)-6, by lipopolysaccharide (LPS)-induced mouse macrophages, indicating that S. marina decreases inflammation. Among all tested fractions [i.e., $H_2O$, n-buthanol (n-BuOH), 85% aqueous methanol (aq. MeOH), and n-hexane], the 85% aq. MeOH fraction showed the strongest antioxidant and anti-inflammatory response. The 85% aq. MeOH fraction scavenged 80% of the free radicals produced by $H_2O_2$-induced control cells. In addition, NO production was 98% lower in 85% aq. MeOH fraction-treated cells compared to LPS-induced control cells. The mRNA expression of iNOS and IL-6 was also suppressed in 85% aq. MeOH fraction-treated cells. The results of the current study suggest that the phenolic compound components of S. marina are responsible for its antioxidant and anti-inflammatory effects.