• 분석과학
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• 제34권4호
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• pp.153-159
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• 2021

In this study, we describe the development of a new high-performance liquid chromatography (HPLC) method for the simultaneous analysis of six bioactive compounds (including gallic acid, epicatechin 3-gallate, quercitrin, afzelin, quercetin, and kaempferol) from Orostachys japonicus. The extraction method was investigated and optimization of the extraction time (min), solvent composition (%), and solvent to material ratio were conducted. As a result, 30 min extraction with 50% methanol and 40:1 mL/g of solvent: material ratio achieved the highest extraction efficiency with a yield of 3.32 mg/g. Furthermore, the developed HPLC method was validated and the correlation coefficient (R) values were within the satisfactory range of 0.9995-0.9999 over the linearity range of 1.53-417 ㎍/mL. The limit of detection and limit of quantification for the six active components were between 0.03-0.08 ㎍/mL and 0.08-0.26 ㎍/mL, respectively. With these newly optimized and developed methods, four batches of O. japonicus were analyzed to confirm the high extraction efficiency of the method and the feasibility of an application.

• Bulletin of the Korean Chemical Society
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• 제33권10호
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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.

• Bulletin of the Korean Chemical Society
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• 제29권1호
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• pp.99-103
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• 2008

Solvent extraction using salphen as a ligand has been investigated for the selective separation and determination of trace Fe(II) and Fe(III). A salphen ligand was synthesized, and solvent extraction variables, such as solution pH, the concentration of salphen, the type of organic solvent, auxiliary agents, oxidants and the effect of interference were optimized. Salphen is stable at pH 3-4, and Fe(III)-salphen complexes can be selectively extracted into an MIBK(4-methyl-2-pentanone) phase from an aqueous solution within this pH range. For the determination of the total amount of iron in 100 mL of aqueous solution, Fe(II) ions were completely oxidized using 0.05 mL of 3.5% H2O2 without side reactions. To evaluate its applicability, the proposed method was applied to determine trace Fe(II) and Fe(III) in several kinds of water samples. Reproducible results were obtained with RSD of less than 3.0%, and the recoveries for this reliability were obtained with 91-112%.

• KSBB Journal
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• 제23권4호
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• pp.281-284
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• 2008

본 연구에서는 식물세포배양액에서 회수한 식물세포인 biomass로부터 항암제 paclitaxel을 효율적으로 회수하기 위해, microwave를 이용한 추출 (MAE) 방법을 도입하여 기존의 유기용매 추출 (CSE) 방법과 추출효율을 비교하였다. CSE 방법에서 추출온도 25, $30^{\circ}C$에서는 추출시간 (3, 6, 10 min)에 대해 추출효율이 온도에 영향을 받지 않은 반면, 40, $50^{\circ}C$에서는 추출시간 10 min에서 paclitaxel 수율이 감소하는 경향을 보여 온도에 영향을 받음을 알 수 있었다. CSE 방법의 경우 총 4회의 추출로 식물세포 내 대부분의 paclitaxel을 회수 (>99%) 가능한 반면 MAE 방법의 경우 1회의 추출로 식물세포 내 대부분의 paclitaxel을 회수 (>99%) 가능하였다. MAE 방법이 CSE 방법보다 paclitaxel를 회수하는데 있어서 높은 추출효율, 공정시간 단축, 에너지 절감 효과가 있음을 알 수 있었다. 또한 MAE 공정에서 최적의 biomass/methanol의 비율은 1/1 (w/v)임을 알 수 있었다.

• 한국물환경학회지
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• 제22권1호
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• pp.122-127
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• 2006

Fundamental studies were carried out for an effective removal and recovery of silver from waste photo-developing solution by solvent extraction. The organic solvents examined for silver-extraction were ALIQUAT 336, D2EHPA, KELEX 100, and TBP. ALIQUAT 336, which is an anionic exchanger, was found to be efficient for the extraction of silver and the reason for this was considered to be due to the chloride ion contained in its structure. The extent of silver extraction was examined to increase with the concentration of ALIQUAT 336 until it reached 0.6 M and no more extraction was observed above this concentration. The extraction of silver by ALIQUAT 336 was found to reach its pseudo-equilibrium within a few minutes after the reaction started and additional slight increase in silver extraction was observed until 30 minutes of reaction time. The observed differences in silver extraction for artificial and actual waste solutions were considered to be based upon the different ionic form of silver-containing species in these solutions.

• 한국식품저장유통학회지
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• 제8권4호
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• pp.456-461
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• 2001

감 과피로부터 천연식용색소를 개발하고자 7가지 (acetone, ethanol, ether, ethyl acetate, ethylene chloride, hexan, methanol)의 유기용매로 carotenids를 추출하고 추출수율을 비교하였다. 이들 용매중 아세톤의 추출수율이 가장 크게 나타나 아세톤을 이용한 추출조건의 최적화를 위하여 중심합성계획에 의한 반응표면분석을 행하였다. 시료에 대한 추출온도(X$_1$), 추출시간(X$_2$), 용매비(X$_3$)를 요인변수로 하고 caroteniods 함량(Y)을 종속변수로 하여 5가지 수준으로 추출을 실시하였다. 반응표면분석으로 수립된 회귀식에 대하여 적합결여분석을 행한 결과 유의성이 없어 회귀식이 적절함을 알 수 있었으며 추출온도가 가장 큰 영향을 미치는 변수로 나타났다. carotenoids함량은 추출온도 $25^{\circ}C$부근까지 증가하다. 가 감소하는 것으로 나타났는데 이는 열에 의해 carotenoids의 산화가 촉진된 것으로 생각된다. 또한 carotenoids 함량은 추출시간과 용매비의 증가에 따라 carotenoids함량이 높게 나타났다. 기울기로 보아 추출온도가 추출시간보다 더 큰 영향을 주는 것을 알 수 있었다. 요인 변수 중 추출량에 가장 영향이 적은 용매비를 중심점의 조건으로 고정하고 추출온도와 추출시간만을 변수로 하였을 경우 carotenoids 함량을 최대로 하는 영역의 추출온도와 추출시간을 각각 29$^{\circ}C$, 93min으로 결정할 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제27권4호
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• pp.563-567
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• 2006

The application of a synergistic solvent extraction by the formation of ternary complex with pyrocatechol violet (PV) and benzalkonium chloride (BC) was studied for determination of trace Zn(II) in water samples. The pH of sample solution and the amount of PV and BC added were optimized for the formation of the stable complex, a proper solvent was selected for the effective extraction, and the concentration of nitric acid was fixed for the back extraction of the complex from the solvent. After the ionic strength of 100 mL sample solution was adjusted to 0.1 M by adding NaCl and the pH was fixed at 9 with a carbonate buffer, 1.0 mL of 2% PV solution was added to form Zn(II)-PV complex then the Zn(II)-PV/BC ternary complex was made by adding 1.0 mL of 10% BC solution. The ternary complex was extracted into 10 mL of MIBK. And the ternary complex was back-extracted with 10 mL of 1.0 mol/L nitric acid to determine Zn(II) by a flame atomic absorption spectrophotometer (flame-AAS). The interference of concomitant ions on the extraction of Zn(II) was investigated. This procedure was applied to the analysis of three real samples such as Dalbang-dam water, laboratory tap water and Jungnajin seawater. The recoveries of Zn(II) in spiked samples were 86.58-104.1%.

• 한국환경보건학회지
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• 제19권2호
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• pp.40-45
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• 1993

A solvent extraction system of copper-thiocyanate complex into various types of alkylamines such as secondary, tertiary and quaternary ammonium salt for the determination of trace copper by atomic absorption spectrometry is presented. The maximum extraction of copper shows at 0.1 M-thiocyanate and single extraction with 10 ml of 1% amine-MIBK from 50 ml of aqueous solution is enough to be quantitative for micro amounts of copper. The effect of amine diluents and of diverse ions are also examined.

• Biotechnology and Bioprocess Engineering:BBE
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• 제9권3호
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• pp.207-211
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• 2004

Predispersed solvent extraction (PDSE) of succinic acid with Tri-n-octylamine (TOA) dissolved in 1-octanol from aqueous solutions of 50 g/L succinic acid was examined. It was found that the equilibrium data in PDSE was equal to that in conventional solvent extraction in spite of the lack of mechanical mixing in PDSE. The influence of salts on succinic acid extraction and the stability of colloidal liquid aphrons (CLAs) were also investigated. Results indicated that in the presence of sodium chloride, less succinic acid was extracted by CLAs and the stability of CLAs decreased. However, the stability of CLAs was sufficient to make PDSE practically applicable to real fermentation broth, considering the concentration range of salts in the fermentation process for succinic acid.

• 한국환경보건학회지
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• 제25권3호
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• pp.103-107
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• 1999

Even if odorous compounds remain very low concentration in water, it cause strong odor. Because Geosmin and most of odorous compound had very low vaporization, those were difficult to analyze with GC/MSD and Purge & Trap. So, we needed pre-treatment method for decreasing amounts of extracting solvents, improving recovery efficiencies and increasing analytical efficiencies. This study developed efficient technology for analyzing odorous compounds, using various adsorbents and extracting solvents. The optimum adsorbent was XAD resins. Especially, XAD-2, XAD-7 and XAD-2010 were superior, but XAD-2 of these and the optimum extraction solvent is MTBE. Other extraction solvents' efficiency is in order of MTBE>Dichloromethane>n-Hexane>Diethylether. The optimum NaCl dosage for increasing efficiency is 5 g in liquid-liquid extraction method. The shaking time(0~24hr) has no concern with adsorption efficiency. The optimum adsorbent is XAD-2 resin and extraction solvent is MTBE. Dosing NaCl, adsorption efficiency is increased in liquid-liquid extraction method, but NaCl has no effect on liquid-solid extraction method. In this experimental results, this algae toxins(Mycrocystin, Anatoxin etc.).