• Title/Summary/Keyword: good solvent condition

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Development of Ruthenium/TEMPO/Nitrate Catalyst System for Efficient Oxidation of Isosorbide (아이소소바이드의 효과적 산화반응을 위한 루테늄/템포/나이트레이트 촉매 시스템 개발)

  • Irshad, Mobina;Yu, Jung-Ah;Oh, Youngtak;Kim, Jung Won
    • Applied Chemistry for Engineering
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    • v.33 no.1
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    • pp.103-108
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    • 2022
  • This research work reports the development of a Ruthenium/2,2,6,6-tetramethylpiperidine-N-oxyl (TEMPO)/nitrate catalyst system for the highly selective transformation of isosorbide (1,4:3,6-dianhydro-D-glucitol) to isosorbide-diketone (2,6-dioxabicyclo (3,3,0)octan-4,8-one). Isosorbide is a critical platform molecule for future manufacturing processes. TEMPO has been utilized to convert alcohols to carbonyl compounds for a long time. The optimal chemical reaction condition was found to be when using isosorbide (0.5 mmol) with supported Ru (10 mol%), TEMPO (5 mol%), and sodium nitrate (0.03 mmol) in the presence of acetic acid (3 ml) as a solvent at 50 ℃ and 1 atm oxygen pressure. This catalyst system demonstrated good selectivity (> 97%) and yield (87%) with respect to the desired product, in addition to a putative catalytic double oxidation mechanism.

Comparative analysis of glycerin in cosmetics by LC/MS and 1H NMR (LC/MS와 1H NMR을 이용한 화장품속의 글리세린 비교분석)

  • Park, Gyo-Beom;Park, Chan Jo;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.400-405
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    • 2007
  • The comparative analysis of glycerin in cosmetic samples was carried out by LC/MS and $^1H$ NMR spectrometry. For the LC/MS analysis, aqueous solution was controlled in strong basic condition with sodium hydroxide, and benzoyl chloride was added to the solution for the derivatization of glycerin. The derivative was extracted using pentane and analyzed by the LC/MS. For the $^1H$ NMR analysis, sample was directly dissolved in $D_2O$ solvent without pretreatment. The quantitative analysis of glycerin was done by $^1H$ NMR ERETIC method. The analysis results of LC/MS and $^1H$ NMR showed that the calibration curves were a good linearity with $r^2=0.9991$ in the range of 0.1 to $10{\mu}g/mL$ and $r^2=1$ in the range of 25 to $500{\mu}g/mL$, respectively.

STUDIES ON THE UTILIZATION OF ANTARCTIC KRILL 2. Processing of Paste Food, Protein Concentrate, Seasoned Dried Product, Powdered Seasoning, Meat Ball, and Snack (남대양산 크릴의 이용에 관한 연구)

  • PARK Yeung-Ho;LEE Eung-Ho;LEE Kang-Ho;PYEUN Jae-Hyeung;KIM Se-Kweun;KIM Dong-Soo
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.13 no.2
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    • pp.65-80
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    • 1980
  • Processing conditions of the krill products such as paste food, krill protein concentrate, seasoned dried krill, powdered seasoning, meat ball, and snack have been examined and the quality was evaluated chemically and organoleptically. In the processing of paste food, krill juice was yielded $71\%$ and krill scrap $29\%$. The yields of paste and broth from the krill juice showed $53\%$ and $43\%$, respectively. In amino acid composition of the krill paste, proline, glutamic acid, aspartic acid, lysine, and leucine were abundant, while histidine, methionine, tyrosine, serine and threonine were poor. The optimum condition for solvent extraction in the processing of krill protein concentrate was the 5 times repetitive extraction using isopropyl alcohol at $80^{\circ}C$ for 5 mins. The yield of krill protein concentrate when used fresh frozen materials was $10.2\%$ in isopropyl alcohol solvent and $8.8\% in ethyl alcohol, and when used preboiled frozen materials, the yield was $13.0\%$ in isopropyl alcohol and $11.8\%$ in ethyl alcohol. Amino acid composition of krill protein concentrate showed a resemblance to that of fresh frozen krill meat. In quality comparison of the seasoned dried krill, hot air dried krill was excellent as raw materials and sun dried krill was slightly inferior to hot air dried krill, but preboiled frozen krill showed the poorest quality. The result of quality evaluation for seasoning made by combination of dried powdered krill, parched powdered sesame, salt, powdered beef extract, monosodium glutamate, powdered red pepper and ground pepper showed that the hot air dried krill was good in color and sundried krill was favorable in flavor. When krill meat ball was prepared using wheat flour, monosodium glutamate and salt as side materials, the quality of the products added up to $52\%$ of krill meat was good and the difference in quality upon the results of the organoleptic test for raw materials was not recognizable between fresh frozen and preboiled frozen krill. In the experiment for determining the proper amount of materials such as dried Powdered krill, $\alpha-starch$, sweet potato starch, sugar, salt, monosodium glutamate, glycine, potassium tartarate, ammonium bicarbonate, and sodium bicarbonate in processing krill snack, sample B(containing $7.7\%$ of dried powdered krill) and sampleC (containing $10.8\%$ of dried powdered krill) showed the most palatable taste from the view point of organoleptic test. Sweet potato starch in testing side materials was good in the comparison of suitability for processing krill snack. Corn starch and kudzu starch were slightly inferior to sweet potato starch, while wheat flour was not proper for processing the snack. In the experiment on frying method, oil frying showed better effect than salt frying and the suitable range of frying temperature was $210-215^{\circ}C$.

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Growth Characteristic, Mono-strain Mass Culture and Antioxidant Effects of Two Benthic Diatoms Amphora coffeaeformis and Achnanthes longipes from Korea

  • Abu Affan, Md.;Karawita, Rohan;Jeon, You-Jin;Lee, Joon-Baek;Kang, Do-Hyung;Park, Heung-Sik
    • Journal of Marine Bioscience and Biotechnology
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    • v.2 no.3
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    • pp.174-186
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    • 2007
  • Amphora coffeaeformis and Achnanthes longipes are commonly found as dominant benthic microalgae in Jeju coastal water throughout the year. In order to investigate pharmaceutical uses of these diatoms, each single species was isolated with micropipette under phase contrast microscope and subcultured with synthetic seawater media which was enriched with F/2 media, trace metal solution and $Na_2SiO_3$). Growth characteristics of these species were also determined with different combination of salinity, nutrients concentration and temperature. Thereafter, mass culture of each species was done based on the maximum growth condition. Biomass was collected after two weeks of mass culture and freeze dried for antioxidant study. The antioxidant properties of different fractions (n-hexane, chloroform and ethylacetate) obtained by solvent fractionation of 80% methanolic extract of two microalgae were investigated for free radical, reactive oxygen species scavenging (Super oxide, Hydrogen peroxide, Hydroxyl radical and Nitric oxide), metal chelating and lipid peroxidation inhibition activities. All fractions of A. longipes showed higher $DPPH^{\cdot}$ (free radical) scavenging activities (n-hexane: 89.0%, Chloroform: 76.0%, Ethylacetate: 66.0%, Methanol: 90.6% and aqueous residue: 63.0%). N-hexane fraction of A. longipes showed significantly higher activity (49.0%) on nitric-oxide. Ethylacetate fraction of A. longipes and aqueous residue of A. coffeaeformis exhibited 64.0% and 75.6% metal chelating activity which was higher than commercial antioxidants (${\alpha}$-tocopherol: 18.0% and BHT: 16.0%). The n-hexane fraction of A. coffeaeformis had 67.5% activity on $DPPH^{\cdot}$. Chloroform and n-hexane fractions of A. coffeaeformis exhibited 46.2% and 47.6% $H_2O_2$ scavenging effects which were closely similar to commercial antioxidants (${\alpha}$-tocopherol: 49.2% and BHT: 58.6%). Chloroform and ethylacetate fractions of A. longipes and fraction of n-hexane and chloroform of A. coffeaeformis showed better lipid peroxidation activities than ${\alpha}$-tocopherol. These data suggest that both organic and aqueous fractions have good antioxidative compounds with different antioxidant properties.

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Characteristics of Degradation and Improvement of Properties with Conducting Polypyrrole (전도성 Polypyrrole의 분해 특성과 물성 개선)

  • Lee, Hong-Ki;Eom, Jung-Ho;Park, Soo-Gil;Shim, Mi-Ja;Kim, Sang-Wook;Lee, Ju-Seong
    • Applied Chemistry for Engineering
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    • v.5 no.5
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    • pp.764-771
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    • 1994
  • Electrochemical synthesis of conductive polypyrrole films was carried out in nucleophilic solvent containing p-toluenesulfonic acid or bezensulfonic acid as supporting electrolyte and dopant. Also characteristics of degradation and improvement of mechanical properties were studied. The conductivity, tensile strength and elongation of the films obtained in dimethyformamide/p-toluenesulfonic acid had the highest value of 10-40S/cm, $25N/mm^2$ and 10%, respectively. The optimum condition of electrochemical synthesis was $2mA/cm^2$ for constant current method and 0.9V for constant potential method containing 0.5M pyrrole and 0.5M p-TSA. The obtained films showed good stability in air and electrode characteristics of secondary battery by reversibility in doping and undoping. The degradation process was 1st order reaction at various temeprature. The activation energy and rate constant of degradation reaction were $1.01JK^{-1}mol^{-1}$ and $3.1{\times}10^{-7}min^{-1}$ respectively at $25^{\circ}C$. For the improvement of mechanical properties, composition of polypyrrole films with various host polymer were investigated and increase of tensile strength and elongation was confirmed.

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Analysis of volatile aroma compounds from vanilla perfume using headspace disk type monolithic material sorptive extraction (시료상층부 원판 형태 단일 다공성 물질을 이용한 바닐라 향수의 휘발성 아로마 성분 추출 분석)

  • Son, Hyun-Hwa;Lee, Dong-Sun
    • Analytical Science and Technology
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    • v.24 no.6
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    • pp.421-428
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    • 2011
  • In this study, headspace disk type monolithic material sorptive extraction (HS-MMSE) was developed, validated and applied to the analysis of volatile aroma compounds from vanilla perfume by gas chromatography -mass spectrometry (GC/MS). HS-MMSE uses monolithic material (MonoTrap) based on silica bonded with octadecyl silane (ODS) and activated carbon as a sorbent. Aroma compounds was adsorbed onto the MonoTrap in headspace and extracted by only 100 ${\mu}L$ of solvent. Total 12 volatile compounds from vanilla perfume were successfully analyzed using HS-MMSE. The influence of extractive parameters was investigated and optimized, using benzyl acetate, linalyl acetate, vanillin, ethyl vanillin as target compounds. Under the optimum condition, the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) of proposed method for the target compounds were obtained within the range of 8.35~13.76 ng and 27.82~45.88 ng, respectively. The method showed good linearity with correlation coefficient more than 0.9888, satisfactory recovery and reproducibility. These results showed that HS-MMSE using disk type MonoTrap is a new promising technique for the analysis of volatile aroma compounds from vanilla perfume.

Optimization for Electron Donating Ability and Organoleptic Properties of Ethanol Extracts from Chrysanthemum Petals (전자공여작용과 관능적 특성을 고려한 산국(山菊) 에탄올 추출물의 제조조건 최적화)

  • Park, Nan-Young;Lee, Gee-Dong;Jeong, Yong-Jin;Kim, Hyun-Ku;Kwon, Joong-Ho
    • Korean Journal of Food Science and Technology
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    • v.30 no.3
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    • pp.523-528
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    • 1998
  • Response surface methodology (RSM) was used to monitor extraction characteristics of electron donating ability and organoleptic properties for ethanol extracts from Chrysanthemum petals, thereby determining optimum extraction conditions. A central composite design was applied to investigate effects of solvent per sample $(X_1)$, ethanol concentration $(X_2)$ and extraction time $(X_3)\;at\;60^{\circ}C$ on dependent variables such as electron donating ability $(Y_1)$, organoleptic color $(Y_2)$ and organoleptic aroma $(Y_3)$ of the extracts. Second-order models were employed to generate 4-dimensional response surfaces for qualitative and quantitative aspects of ethanol extracts. Coefficients of determination $(R_2)$ of the models for dependent variables were ranged from 0.8180 to 0.9696. Optimum extraction conditions for each variable were 50 mL/g, 61% and 16 hrs in electron donating ability, 88 mL/g, 21% and 16 hrs in organoleptic color, 55 mL/g, 73% and 19 hrs in organoleptic aroma, respectively. The optimum condition ranges for maximized characteristics of ethanol extracts were $65{\sim}78\;mL/g,\;90{\sim}100%\;and\;15{\sim}25\;hrs$. Predicted values at the optimum conditions were in good agreement with experimental values.

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Synthesis of 1,2-Dodecylaminopropanediol and Its Mixing Effect with 1,2-Alkanediols as Preservatives (보존제로서 1,2-도데실아미노프로판디올의 합성 및 1,2-알칸디올 화합물의 혼합 효과)

  • Cha, Kyung-On;Kwak, Sang-Woon;Jeong, Kook-In;Kim, Young-Ho
    • Applied Chemistry for Engineering
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    • v.33 no.2
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    • pp.179-187
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    • 2022
  • In this study, the synthesis of 1,2-dodecylaminopropanediol (1,2-DDAP) having a 12 carbon chain length and an amine group was designed to improve the preservation and hydrophilicity of 1,2-alkanediol-based compounds. 1,2-DDAP was prepared by reacting dodecylamine (DDA) with 3-monochloro-1,2-propanediol (3-MCPD) in an ethanol solvent at 40 ℃, and its yield and purity were about 56% and 98%, respectively, under a reaction condition of 2 h and a DDA:3-MCPD molar ratio of 1:0.8. The antimicrobial effect of 1,2-DDAP showed the values of the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) against microorganisms at concentrations of 10 to 100 times lower than those of 1,2-octanediol(1,2-ODIOL) or 1,2-decanediol (1,2-DDIOL). Based on the hydrophilic properties of 1,2-DDAP, mixed preservatives were prepared by adding small amounts of 1,2-ODIOL or 1,2-DDIOL, which are poorly soluble in water, with 1,2-DDAP. Mixed preservatives exhibited an effect of inhibiting microorganisms equal to or greater than that of 1,2-DDAP alone in antimicrobial activity tests. As a result of confirming the preservation effect in lotion (cosmetic formulation) for application, 1,2-DDAP showed similar antimicrobial activity at concentrations of 0.3 to 0.6 times lower than that of 1,2-ODIOL or 1,2-DDIOL. Therefore, it is considered that the use of 1,2-DDAP alone and the mixed use with small amounts of 1,2-ODIOL or 1,2-DDIOL can be a good alternative to preservatives in the product.