• Title/Summary/Keyword: solvent recovery

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Separation Behavior of Paclitaxel and Its Semi-synthetic Precursor 10-Deacetylpaclitaxel from Plant Cell Cultures (식물세포배양으로부터 파클리탁셀 및 이의 반합성 전구체 10-디아세틸파클리탁셀의 분리 양상)

  • Lee, Chung-Gi;Kim, Jin-Hyun
    • Korean Chemical Engineering Research
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    • v.54 no.1
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    • pp.89-93
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    • 2016
  • In this study, we investigated the separation behavior of the anticancer agent paclitaxel and its semi-synthetic precursor 10-deacetylpaclitaxel (10-DAP) from plant cell cultures. As a result of sequential separation/purification performed by biomass extraction with solvent, liquid-liquid extraction, adsorbent treatment, hexane precipitation, and fractional precipitation, the adsorbent treatment was found to be the most effective in separating and recovering 10-DAP from paclitaxel. The optimal adsorbent type, crude extract/adsorbent ratio, and adsorbent treatment temperature were sylopute, 1:1.5 (w/w), and $20^{\circ}C$, respectively. The separation/recovery of 10-DAP from paclitaxel was 74.1% in adsorbent treatment process under optimal conditions.

Development of a Novel Process to produce Biodiesel and its use as fuel in CI Engine performance study

  • Mishra, Prasheet;Lakshmi, D.V.N.;Sahu, D.K.;Das, Ratnakar
    • International journal of advanced smart convergence
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    • v.4 no.1
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    • pp.154-161
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    • 2015
  • A novel process has successfully been developed by overcoming major difficulties through the elimination of number of process steps involved in the Classical Transesterification reaction during the preparation of Fatty Acid Methyl/Ethyl Ester (FAME.FAEE) called biodiesel. The Classical process with cost intensive process steps such as the utilization of excess alcohol, needing downstream distillation for the recovery and reutilization of excess alcohol/cosolvent, unrecoverable homogenous catalyst which consumes vast quantity of fresh distilled water during the purification of the product and downstream waste water treatment before its safe disposal to the surface water body. The Novel Process FAME/FAEE is produced from any vegetable oil irrespective of edible or inedible variety using sonication energy. The novelty of the finding is the use of only theoretical quantity of alcohol along with a co-solvent and reduced quantity of homogeneous catalyst. Under this condition neither the homogeneous catalyst goes to the FAME layer nor is the distillation needed. The same ester also has been prepared in high pressure high temperature reactor without using catalyst at sub critical temperature. The quality of prepared biodiesel without involving any purification step meets the ASTM standards. Blended Biodiesel with Common Diesel Fuel (CDF) and FAME is prepared, characterized and used as fuel in the Kirloskar make CI Engines. The evaluation of the engine performance result of pure CDF, B05 biodiesel, B10 biodiesel of all types of biodiesel prepared by using the feedstock of Soybean (Glycine max) and Karanja (Pongamia pinnate) oil along with their mixed oil provides useful information such as brake power, brake thermal efficiency, brake specific fuel consumption, etc, and established it as ideal fuel for unmodified CI engine.

Determination of Thiamine in Pharmaceutical Preparations by Reverse Phase Liquid Chromatography Without Use of Organic Solvent

  • Suh, Joon Hyuk;Kim, Junghyun;Jung, Juhee;Kim, Kyunghyun;Lee, Seul Gi;Cho, Hyun-Deok;Jung, Yura;Han, Sang Beom
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1745-1750
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    • 2013
  • A novel green aqueous mobile phase modified with room temperature ionic liquids (RTILs) was employed in the absence of volatile organic solvents or ion-pairing reagents to analyze thiamine, a very polar compound, by reverse phase high performance liquid chromatography (RP-HPLC). Due to its strongly hydrophilic nature, thiamine was eluted near the column dead time ($t_0$) using a mobile phase without adding RTILs or ion-pairing reagents, even if a 100% aqueous mobile phase, which has weak elution power under reverse phase conditions, was used. Thus, 1-ethyl-3-methyl-imidazolium hexafluorophosphate ([EMIM][$PF_6$]), which has the strongest chaotropic effect, was selected as a mobile phase additive to improve retention and avoid baseline disturbances at $t_0$. Various mobile phase parameters such as cation moiety, chaotropic anion moiety, pH and concentration of RTILs were optimized to determine thiamine at the proper retention time. Method validation was performed to assess linearity, intra- and inter-day accuracy and precision, recovery and repeatability; all results were found to be satisfactory. The developed method was also compared to the current official United States Pharmacopoeia (USP) and Korean Pharmacopoeia (KP) methods using an organic mobile phase containing an ionpairing reagent by means of evaluating various chromatographic parameters such as the capacity factor, theoretical plate number, peak asymmetry and tailing factor. The results indicated that the proposed method exhibited better efficiency of thiamine analysis than the official methods, and it was successfully applied to quantify thiamine in pharmaceutical preparations.

Economic Analysis of Upgrading Low Rank Coal Process (저등급석탄 고품위화 공정의 경제성 분석)

  • Chun, Dong-Hyuk;Kim, Sang-Do;Rhim, Young Joon;Lee, Si Hyun
    • Korean Chemical Engineering Research
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    • v.49 no.5
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    • pp.639-643
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    • 2011
  • Fry-drying of coal slurry is one of the upgrading low rank coal processes. It consists of slurry mixing, slurry dewatering, solvent recovery and briquetting. Cost estimation and economic feasibility are examined for the upgrading low rank coal process based on capacity of 1 million ton/yr. In case that investment costs are $100,000,000, discount rate is 12%, and service life is 20 years, the results of economic analysis are enough to satisfy the evaluation criteria of investment such as IRR, B/C ratio, NPV and discounted payback period. According to sensitivity analysis, investment value are very sensitive to raw material cost and product price. Since the bituminous coal price is currently soaring, it is expected that the investment value will increase more and more.

Simultaneous Determinaton of Octylphenol, Nonylphenol, Bis(2-ethylhexyl) phthalate in Biological Samples (생체시료 중 Octylphenol, Nonylphenol, Bis(2-ethylhexyl) phthalate의 동시정량)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.95-102
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    • 2001
  • A comprehensive analytical method of endocrine disruptors[i.e., nonylphenol(NP), octylphenol(OP), bis(2-ethylhexyl) phthalate(BEHP)] in meat or pork samples was developed. The method employed closed culture tube extraction with dichloromethane and solvent exchange to iso-hexane and SPE(2g) aminopropyl column, followed by determination on gas chromatography linked to mass spectrometry(GC/MS) operated in the single ion monitering(SIM) mode. For the multipoint recovery of nonylphenol, octylphenol and bis(2-ethlhexyl) phthalate OP, NP were showen good recoveries in $0.125-1.25{\mu}g/g$ range of concentration, and BEHP more good recoveries in $0.0125-12.5{\mu}g/g$ wide range of concentration. The present method was applied to beef or pork samples of mart and butcher in Cheonju city and near Cheonju. The range of concentrations was respectively, $0.06-0.24{\mu}g/g$ in nonylphenol(NP) and $0.36-2.35{\mu}g/g$ in bis(2-ethylhexyl) phthalate(BEHP), but octylphenol(OP) was not dected in any samples. This method provides a powerful analytical tool to investigate a wide range of endocrine disruptors in biological samples of limited quantity.

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A Study on Analysis of Residual Antibiotics and Prop Acid in Honey (벌꿀중의 잔유항생물질 및 Propionic Acid 분석011 관한 조사연구)

  • 전상수
    • Journal of environmental and Sanitary engineering
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    • v.5 no.2
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    • pp.63-80
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    • 1990
  • A sensitive and simple analytical system for the simultaneous determination of residual oxytetracycline, tetracycline, and doxycycline in honey was described, and that the analytical method for determination of residual propionic acid in honey was established. Experimental subjects were purchased four kinds of honey, native kind honey, acaccia honey, mixed floral honey, chestnut honey in Kyung Sang Nam Do. Several microbiological methods are available to determine tetracycline antibiotecs(TCs) in foods but their precision apears to be variable and the specificity is questionable. These methods are considered to be not suitable for analysis of tetracycline antibiotics in honey because honey itself has bacteriostatic action. For determination of tetracycline antibiotics in honey, therefore the High Performance Liquid Chromatography(HPLC) method was applied, and the propionic acid were determined by Gas Chromatography(5.C). Ethylacetate, as an extract solvent, was found to be suitable for seperation of TCs in honey, but methanol and acetone were not. The recoverly rate of Oxytetracycline(OTC), Tetracycline(TC), Doxycycline(DC) from honey spiked at a level of 10 $\mu $g/g were 97%, 89%, and 91%, respectively. The cailbration curve in TCs was linear expression from 2$\mu $g/ml to 10$\mu $g/ml. As the results of analysis, the residual tetracycline antibiotics were not detected in the 100 samples of honey. The recovery rate of propionic acid from honey spiked at level of 10$\mu $g/g was 98.3% , and the calibra lion curves were linear expression from 21$\mu $g/ml to 101$\mu $g/ml. As the results of analysis, the residual propionic acid was not detected in the 100 samples of honey. Retention time(min) of OTC, DC, and TC were 3.35, 4.61, and 5.30 minutes at the conditions of table 2, respectively, and retention time(min) of propionic acid was 3.50 minutes at the conditions of table 3. The residual TCs and propionic acid were not detected in the 100 samples of honey, but there is a possibility that antibiotics or propionic acid will be to remain in honey if they are used during product period in order to prevent putrefaction of honey-bee.

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A Study on Sample Preparation for the Analysis of Trace Elements in Foods of Animal Origin by Ultra High Pressure Microwave Digestion (초고압초음파분해법을 이용한 축산물내 미량금속 잔류분석을 위한 시료전처리 방법)

  • Lee, Myoung-heon;Lee, Hee-su;Son, Seong-wan;Jung, Gab-soo;Park, Jong-myung;Kim, Sang-keun
    • Korean Journal of Veterinary Research
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    • v.43 no.3
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    • pp.393-398
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    • 2003
  • Simple and rapid sample preparation method for trace elements in foods of animal origin using ultra high pressure microwave digestion system (UHP/MDS) and inductively coupled plasma atomic emission spectrometer (ICP/AES) were developed. 1. For the digestion of sample using UHP-MDS, 20% nitric acid (v/v) was the most suitable solvent for the determination of trace elements in foods of animal origin. 2. The optimal digestion conditions for UHP-MDS were as follows: final temperature $180^{\circ}C$, final pressure 400 PSI, and magnetic power 900 W in the solid sample. For the liquid sample final temperature $170^{\circ}C$, final pressure 300 PSI and magnetic power 700 W were optimal conditions. 3. As result of interlaboratory test, the average recovery rate of the for solid sample were 88.3~99.1% for As, 82.4~93.3% for Cd, 89.2~101.2% for Hg and 86.5~93.8% for Pb, respectively. In liquid sample, it were 87.0~96.8% for As, 80.9~96.6% for Cd, 87.5~91.2% for Hg and 91.4~95.5% for Pb, respectively. 4. The average coefficient variation rate were 3.3~15.9% for solid sample and 2.9~10.8% for liquid sample.

Establishment of Analytical Method of Prochloraz in Cabbage, Apple, Mandarin, Pepper and Hulled rice with GC-ECD (GC-ECD를 이용한 배추, 사과, 감귤, 고추, 현미 중 살균제 Prochloraz의 분석법 확립)

  • Lee, Eun-Mi;Lee, Hye-Ri;Riu, Myoung-Joo;Park, Hee-Won;Na, Ye-Rim;Song, Hyuk-Hwan;Keum, Young-Soo;Zhu, Youngzhe;Kim, Jeong-Han
    • Korean Journal of Environmental Agriculture
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    • v.28 no.4
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    • pp.427-434
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    • 2009
  • Analytical method for prochloraz in cabbage, apple, pepper, mandarin, and hulled rice was established by conversion it to 2,4,6-trichlorophenol (TCP). Crop samples were extracted with acetonitrile, and partitioned with dichloromethane. The sample extracts were hydrolyzed with pyridine hydrochloride in a vial by heating for 1 hour, and analyzed with GC-ECD after partitioning with dichloromethane. Method quantification limit (MQL) of prochloraz was 0.01 mg/kg. Recoveries at 0.1 mg/kg level was 105-113% while at 0.5 mg/kg level was 82-87%. In both of the cases CV was less than 10%. Through this procedure soxhlet extraction and refluxing apparatus of conventional method were discarded and simple solvent extraction and small vial were successfully employed, resulting in simple, rapid, economic and more precise method.

Leaching Kinetics of Yttrium Extraction from Coal Fly Ash using Sulfuric Acid

  • Kim, Jae-kwan;Park, Seok-un;Hong, Jun-seok;Shin, Dong-ik;Jeong, Jae-hyeok
    • KEPCO Journal on Electric Power and Energy
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    • v.3 no.1
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    • pp.29-34
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    • 2017
  • Leaching kinetics for extracting yttrium from the coal fly ash was investigated in the presence of sulfuric acid during extraction. The leaching kinetics of yttrium were conducted at reactant densities of 5~1,000 g coal fly ash per L of $1.0{\sim}10.0N\;H_2SO_4$, agitation speed of 250 rpm and temperature ranging from 30 to $90^{\circ}C$. As a result, the leaching kinetic model was determined in a two-step model based on the shrinking core model with spherical particles. The first step was proceeded by chemical reaction at ash surface, and the second step was proceeded by ash layer diffusion because the leaching conversion of yttrium by the first chemical reaction increases with increased the time irrelevant to the temperature whereas it increases with increased the leaching temperature. The activation energy of the first chemical leaching step was determined to be $1.163kJmol^{-1}$. After the first chemical reaction, the activation energy of ash layer diffusion leaching was derived to be $41.540kJmol^{-1}$. The optimum conditions for leaching the yttrium metal of 60 % were found to be the slurry density of 250 g fly ash per L of $H_2SO_4$, solvent concentration of $2.0N\;H_2SO_4$, second step leaching of temperatures of $30^{\circ}C$ for 3 hours and then $90^{\circ}C$ for 3 hours at agitation rate of 250 rpm.

Rapid Isolation of Cyanidin 3-Glucoside and Peonidin 3-Glucoside from Black Rice (Oryza sativa) Using High-Performance Countercurrent Chromatography and Reversed-Phase Column Chromatography

  • Jeon, Heejin;Choi, Janggyoo;Choi, Soo-Jung;Lee, Chang Uk;Yoon, Shin Hee;Kim, Jinwoong;Yoon, Kee Dong
    • Natural Product Sciences
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    • v.21 no.1
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    • pp.30-33
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    • 2015
  • Anthocyanins are water soluble plant pigments which are responsible for the blue, red, pink, violet colors in several plant organs such as flowers, fruits, leaves and roots. In recent years, anthocyanin-rich foods have been favored as dietary supplements and health care products due to diverse biological activities of anthocyanins including antioxidant, anti-allergic, anti-diabetic, anti-microbial, anti-cancer and preventing cardiovascular disease. High-performance countercurrent chromatography (HPCCC) coupled with reversed-phase medium pressure liquid chromatography (RP MPLC) method was applied for the rapid and efficient isolation of cyanidin 3-glucoside (C3G) and peonidin 3-glucoside (P3G) from black rice (Oryza sativa L., Poaceae). The crude black rice extract (500 mg) was subjected to HPCCC using two-phase solvent system composed of tert-butyl methyl ether/n-butanol/ acetonitrile/0.01% trifluoroacetic acid (TBME/B/A/0.01% TFA, 1 : 3 : 1 : 5, v/v, flow rate - 4.5 mL/min, reversed phase mode) to give enriched anthocyanin extract (37.4 mg), and enriched anthocyanin extract was sequentially chromatographed on RP-MPLC to yield C3G (16.5 mg) and P3G (8.7 mg). The recovery rate and purity of isolated C3G were 76.0% and 98.2%, respectively, and those of P3G were 58.3% and 96.3%, respectively. The present study indicates that HPCCC coupled with RP-MPLC method is more rapid and efficient than multi-step conventional column chromatography for the separation of anthocyanins.