• Journal of the Korean Society of Tobacco Science
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• v.32 no.2
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• pp.88-94
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• 2010

The ether extract(EE) of leaf tobacco contains diverse compounds such as lipid, resinoid, paraffin hydrocarbons and pigments. Although the correlation of EE concentertion with leaf tobacco has not been established clearly, it is known that in some concentration range, EE concentration of leaf tobacco exerts good influence on the quality of tobacco. Recently, The American Oil Chemist's Society introduced new method(Am 5-04; AOCS, 2009) to determine EE concentration by AT15 extractor. This method is based on extraction with organic solvent at relatively high temperature and pressure, which significantly reduces the extraction time and ensures safety. The aim of this study is to optimize analytical condition of AOCS method for analyzing EE concentration of leaf tobacco. When sample pre-drying time and extraction time of XT15 were set to 3 hour and 30 minute and 30 minute respectively, EE concentration obtained from AOAC method. Statistical analysis(T-test) showed that there is no difference(P>0.05) between EE concentrations from two methods.

• Food Science and Preservation
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• v.12 no.6
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• pp.591-599
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• 2005

This study was conducted to optimize the extraction conditions from cabbage by a response surface methodology. In extraction conditions based on the central composite design with variations, the ratio of solvent to sample ($10\~30$mL/g), ethanol concentration ($0\~100\%$) and extraction temperature ($35\~95^{circ}C$) coefficients of determinations ($R^2$) were 0.8162(p<0.1), 0.8173(p<0.1), 0.9374(p<0.01) and 0.9116(p<0.05) in extraction yield, electron donating ability, tyrosinase inhibition and SOD-like ability, respectively. Estimated extraction conditions for the maximizing yield, electron donating ability and SOD-like ability were $15\~30$ mL/g in ratio of solvent to sample, $40\~80\%$; ethanol concentration, and $50\~90^{\circ}C$ ; extraction temperature. Predicted values at the optimum condition (25 mL/g solvent to sample, $50\%$ ethanol concentration and $70^{\circ}C$ in extraction temperature) were in good agreement with observed values.

• Journal of the Korean Chemical Society
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• v.33 no.3
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• pp.287-294
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• 1989

The optimum condition for the separation of priority pollutant phenols using isocratic elution has been determined. The elution behavior of eleven phenols has been also studied to interpret the retention. The reversed phase liquid chromatographic methods were performed on a ${\mu}$-Bondapak $C_{18}$ column with methanol-water, acetonitrile-water, and THF water mixtures as mobile phases. The COF method, where Snyder's solvent triangle concept was combined with a mixture-design statistical technique, was used to optimize the strength and selectivity of solvents for the separation of phenols. The optimum solvent composition, which gives a complete separation of eleven phenols, was found to be $MeOH:ACN:H_2O$ = 7:40:53. The plots of ln k' vs. -${\Delta}H^{\circ}$ and ${\Sigma}{\pi}$ of phenols showed relatively good linearities. Effect of van der Waals volume, pi-energy and hydrogen bonding on the retention of phenols were investigated. The following equation with the correlation coefficient of 0.9927 for ACN-water solvent system was obtained; $log^{k'}=2.515{\times}10^{-2}VWV-1.301{\times}10^{-1}E-3.674{\times}10^{-1}$

• Journal of the Society of Cosmetic Scientists of Korea
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• v.30 no.2
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• pp.189-195
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• 2004

Carbon black have not been used as pigment material in cosmetic because of very low density and dispersity, but carbon black have applicable character as black pigment because of non-toxic, stable physico-chemical property, and black colority. In this study, mesoporous silica samples were synthesized by sol-gel reaction using surfactants-template method; TEOS (tetraethoxysilane) - a) PEO/lecithin, b) PEO/polyethylene glycol, c) lecithin/polyethylene glycol in ethanol/water solution. Synthesized organic-inorganic hybrid - silica were heat-treated in N2 condition at 500$^{\circ}C$. Mesoporous silica with black carbon in pore have the effective density and show the good dispersity in both hydrophilic and hydrophobic solvent. Properties of the samples were measured; specific surface area (750㎡/g) and pore size (4-6nm) using BET, pore structure (cylindrical type) using XRD, morphology (spherical powder with 0.1-0.5$\mu\textrm{m}$ partical size) of the samples using SEM. Carbon-silica black color applied to mascara, it shows a dark black colority and good dispersity as compared with the general black color titania pigment. Moreover, it is possible to control the density of black color pigment because it is possible to control pore volume and particle size of mesoporous silica properly. It show the good volume effects in mascara. That is why possible to apply all kinds of cosmetic products.

• Journal of the Korean Chemical Society
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• v.48 no.1
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• pp.28-32
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• 2004

The condensation reaction of (benzylene)triphenylphosphoranes with carbonyl compounds in supercritical carbon dioxide was examined. Reactions of (benzylene)phosphoranes (ca. 1 mmol) with several benzaldehydes in a supercritical carbon dioxide (80 $^{\circ}C$, 2,000 psi) containing THF entrainer (5%) in a 24 mL reactor proceed smoothly to yield olefination products in fairly good to excellant yields but slower, compared to reactions in a conventional THF solvent. Generally, phosphoranes that are not substituted with a nitro group show more (Z)-selective reactions with aromatic aldehydes under $scCO_2$ condition than in THF. The reaction of (benzylene)triphenylphosphoranes with 4-t-butylcyclohexanone gave the corresponding olefin compounds with a low conversion under both the supercritical carbon dioxide and the organic THF solvent. Our preliminary study showed the Wittig reaction carries out smoothly in supercritical carbon dioxide medium and also a possibile tunability of this reaction pathway by adding a entrainer. The results would be useful for devising a novel process for the environmentally friendly Wittig reaction.

• Applied Chemistry for Engineering
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• v.7 no.4
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• pp.743-749
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• 1996

A new static contractor using capillary phenomena induced by a highly packed fiber bundle was developed for the solvent extraction. When two immiscible phases being cocurrently and forcedly fed into the packed fiber bundle, the contactor brings about a very large liquid-liquid contact area for mass transfer within a small definite space without any turbulence and drop phenomena. In order to test the characteristics and stability of the static contractor system, continuous extraction experiments of TBP-uranyl ion-nitric acid system were done and compared with the batch extraction experiment of the same chemical system. The performance of the static contractor were the same as that of the ideal batch extractor with the same extraction condition. For the increase of the extraction yield by the contactor, the increase of organic flow rate was required at a fixed aqueous flow rate, and a certain residence time of the aqueous phase flow within the contactor system had to be maintained to meet the performance of the batch system of the same phase ratio. The residence time in the case of TBP-uranyl ion-nitric acid system was about 1.9 minutes. This system was confirmed to be effective and stable enough for purposes of the kinetic study of solvent extraction as well as the mutual separation and purification of ordinary materials because of good reproducibility and the stable and large static liquid-liquid contact area.

• Korean Journal of Pharmacognosy
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• v.40 no.4
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• pp.309-314
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• 2009

Licorice(Glycyrrhizae Radix et Rhizoma) is recorded as the root of Glycyrrhiza uralensis Fischer or Glycyrrhiza glabra Linne or Glycyrrhiza inflata Bat.(Leguminosae) in Korean Pharmacopoeia $9^{th}$ edition (KP9) and Chinese Pharmacopoeia 2005(CP2005), Glycyrrhiza uralensis Fischer or Glycyrrhiza glabra Linne in Japanese Pharmacopoeia 2005(JP2005). It is established the content standard of Glycyrrhizin 2.5 % and liquiritin 1% in KP9 and CP2005. But, according to the reports, all Licorice species were not sufficient for content standard of liquiritin 1.0% for licorice in KP9 and CP2005. It shows different content of liquiritin among G. uralensis, G. glabra and G. inflata. Also, it was reported liquiritin, liquiritin apioside are transformed into liquiritigenin by human internal flora. Therefore, we have studied for the pre-treatment condition and analytical method of liquiritigenin; It was good efficinet in 2M HCl reflux(1 hr) for hydrolysis and in methylene chloride for solvent fractionation. And 1% acetic acid in DW(A) and acetonitrile(B) with gradient condition as a mobile phase was most effective in HPLC analytical condition. According to these experimental methods, we have anlayzed content of liquiritigenin about 77 Licorice sample. In this research, it was also examined the content of liquiritin and liquiritigenin for Glycyrrhizae Radix related growing area. According to the results, we suggested the content standard of glycyrrhizin more than 2.5%, liquiritigenin more than 0.7%(after hydrolysis) of licorice.

• Korean Journal of Medicinal Crop Science
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• v.16 no.6
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• pp.446-454
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• 2008

An advanced extraction method by ultrasonic extraction with applied solid phase extraction (SPE) has been developed for the determination of simultaneous eight major ginsenosides, namely ginsenosides Rg1, Re, Rf, Rb1, Rg2, Rc, Rb2, and Rd in the root of Panax ginseng. Four extraction methods including n-BuOH reflux extraction (Method A), 70% EtOH reflux extraction (Method B), 50% MeOH reflux extraction with SPE (Method C), and 50% MeOH ultrasonication with SPE clean-up process (Method D) were investigated for the determination of eight major ginsenosides. Total contents of ginsenosides were highest by extraction of Method C as $2.408{\pm}0.011%$. However, Method D was evaluated as relatively simpler and more efficient method due to short extraction time, small solvent consumption and less expensive, compared to conservative reflux method. Ginsenosides were also satisfactorily separated with good resolution and the accuracy range was between 1.05 and 4.06% as relative standard deviation (RSD) by Method D. SPE condition and HPLC condition were further optimized for determination of eight major ginsenosides by the ultrasonic extraction method. Conclusively, ultrasonic extraction of 2 g sample of ginseng using ultrasonic bath and 1 loading for SPE was evaluated as proper condition for extraction of ginseng.

• Journal of the Korean Chemical Society
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• v.43 no.4
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• pp.438-446
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• 1999

The optimum analytical method of aldehydes, ozone by-products, was established by reverse phase liquid chromatography. Six aldehydes including formaldehyde, acetaldehyde, acrolein, propionaldehyde, butylaldehyde and benzaldehyde, and one ketone including acetone were selected as aldehyde test samples through preliminary experiments. Such analytical conditions as the pH of citrate buffer solution, reaction temperature, reaction time, and concentration of DNPH, the component and composition of desorption solvent were optimized. As the result, pH 3.0 of citrate buffer solution, 40$^{\circ}C$ of reaction temperature, 15 minutes of reaction time, and 0.012% of DNPH concentration were chosen as optimum conditions. Aldehydes-DNPH derivatives in water were concentrated on $C_18$ Sep-Pak cartridge and followed by elution of their derivatives fraction with THF/ACN(70/30) mixture, and showed recoveries of the range from 87 to 107%. Separation condition on Nova-Pak $C_18$ column with low pressure gradient elution from ACN/MeOH/water(30/10/60) of an initial condition to 80% ACN of a final condition was found to give a good resolution within 20 minutes of run time. 86% to 103% of recovery for aldehydes using this method was similar to that for aldehyde using EPA Method 554 which is ranged from 84% to 103%.

• Journal of the Korean Chemical Society
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• v.33 no.5
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• pp.522-529
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• 1989

Symmetrical divinyl ketones and divinyl ${\alpha}$-diketones were synthesized in moderately good yields through palladium catalyzed carbonylative homocoupling reaction of vinylic halides. Divinyl ${\alpha}$-diketones were obtained in the highest yield in the presence of 10 atm of carbon monoxide, using 2 mol% ligand added to palladium(II) acetate as catalyst and three equivalents of tributylamine as base in polar solvent at $100^{\circ}C$. Divinyl ketones were synthesized mainly under atmospheric pressure of carbon monoxide. The reaction was also proceeded to several other vinylic halides under the above reaction condition. Thus, divinyl ketones and divinyl ${\alpha}$-diketones were synthesized selectively as expected.