• Title/Summary/Keyword: Liquid Liquid Extraction

Search Result 1,075, Processing Time 0.032 seconds

Separation of Co(II), Ni(II), and Cu(II) from Sulfuric Acid Solution by Solvent Extraction (황산용액에서 용매추출에 의한 코발트(II), 니켈(II) 및 구리(II) 분리)

  • Moon, Hyun Seung;Song, Si Jeong;Tran, Thanh Tuan;Lee, Man Seung
    • Resources Recycling
    • /
    • v.31 no.1
    • /
    • pp.21-28
    • /
    • 2022
  • The smelting reduction of spent lithium-ion batteries results in metallic alloys of cobalt, nickel, and copper. To develop a process to separate the metallic alloys, leaching of the metallic mixtures of these three metals with H2SO4 solution containing 3% H2O2 dissolved all the cobalt and nickel, together with 9.6% of the copper. Cyanex 301 selectively extracted Cu(II) from the leaching solution, and copper ions were completely stripped with 30% aqua regia. Selective extraction of Co(II) from a Cu(II)-free raffinate was possible using the ionic liquid ALi-SCN. Three-stage cross-current stripping of the loaded ALi-SCN by a 15% NH3 solution resulted in the complete stripping of Co(II). A process was proposed to separate the three metal ions from the sulfuric acid leaching solutions of metallic mixtures by employing solvent extraction.

Liquid Chromatography-Tandem Mass Spectrometric Determination of Geniposide in Rat Plasma and its Pharmacokinetic Application

  • Jin, Ming Ji;Kim, In Sook;Kim, Dong-Hyun;Yoo, Hye Hyun
    • Bulletin of the Korean Chemical Society
    • /
    • v.34 no.9
    • /
    • pp.2760-2764
    • /
    • 2013
  • Geniposide is a biologically active ingredient of gardenia fruit. A liquid chromatography-tandem mass spectrometric method was developed and validated for the determination of geniposide in rat plasma. The plasma samples were pretreated by solid-phase extraction and introduced into a BDS Hypersil $C_{18}$ column ($50{\times}2.1mm$, $5{\mu}m$) for chromatographic separation. The mobile phase consisted of 0.1% formic acid and 0.1% formic acid in acetonitrile, and gradient elution was performed at a flow rate of 0.25 mL/min. For mass spectrometric detection, multiple reaction monitoring was performed via an electrospray ionization source in positive mode. The calibration curve for geniposide was linear ($r^2=0.997$) in the concentration range of $0.005-1{\mu}g/mL$. The intra- and inter-day accuracies and precisions fulfilled the required criteria (${\pm}15%$). The developed method was subsequently used for pharmacokinetic analysis of geniposide after oral administration to rats at a dose of 50 mg/kg. The mean maximum plasma concentration of geniposide was $0.68{\pm}0.29{\mu}g/mL$ at $0.44{\pm}0.13h$, and the mean area under the plasma concentration versus time curve was $1.46{\mu}g{\cdot}h/mL$.

Aroma Characteristics of Acai Berry (아사이베리의 향기성분 특성 연구)

  • Lim, Seung-Hee;Nam, Heesop;Baek, Hyung-Hee
    • Korean Journal of Food Science and Technology
    • /
    • v.48 no.2
    • /
    • pp.122-127
    • /
    • 2016
  • The objective of this study was to identify the volatile compounds and aroma-active compounds from acai berry (Euterpe oleracea). Volatiles were isolated by high vacuum distillation using solvent-assisted flavor evaporation (SAFE) and liquid-liquid continuous extraction (LLCE). To identify the characteristic aroma-active compounds of acai berry, gas chromatography-mass spectrometry-olfactometry was used. Aroma-active compounds were evaluated by aroma extract dilution analysis (AEDA). A total of 51 and 54 volatile compounds from acai berry were identified from SAFE and LLCE extracts, respectively. Alcohols were confirmed to be important volatile compounds in acai berry, as the major volatile compounds were 2-phenylethanol, (Z)-3-hexenol, and benzyl alcohol. ${\beta}-Damascenone$ (berry, rose), trans-linalool oxide (woody), (Z)-3-hexenol (grass), and 2-phenylethanol (rose, honey) were considered the aroma-active compounds in acai berry. The most intense aroma-active compound of acai berry was ${\beta}-damascenone$.

Determination of Oxycarboxin Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 농산물 중 Oxycarboxin의 분석)

  • Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
    • /
    • v.37 no.2
    • /
    • pp.117-124
    • /
    • 2018
  • BACKGROUND: Oxycarboxin(5,6-dihydro-2-methyl-N-phenyl-1,4-oxathiin-3-carboxamide-4,4-dioxide) as oxanthiin is a systemic fungicide commonly used for control of various pathogens in agronomic and horticultural crops. In an effort to develop an analytical method to trace the fungicide, a method using HPLC equipped with UVD/MS was studied. METHODS AND RESULTS: Oxycarboxin was extracted with acetone from hulled rice, soybean, Kimchi cabbage, green pepper, and apple samples. The extract was diluted with saline water, followed by liquid-liquid extraction with methylene chloride. Florisil column chromatography was employed for the purification of the extracts. Oxycarboxin was determined on a Zorbax SB-AQ $C_{18}$ column by HPLC with UVD. Accuracy of the proposed method was validated by the recovery tests from crop samples fortified with oxycarboxin at 3 levels per crop. CONCLUSION: Mean recoveries ranged from 78.3% to 96.1% in five representative agricultural commodities. The coefficients of variation were less than 10%, and limit of quantitation of oxycarboxin was 0.04 mg/kg. A confirmatory technique using LC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. The method was reproducible and sensitive to determine the residue of oxycarboxin in agricultural commodities.

Purification and Characterization of Lysyl Oxidase from Fetal Bovine Aorta in the presence of protease inhibitors -Evidence against polymorphism- (소(牛) 태아(胎兒) 대동맥(大動脈)으로부터 단백 분해효소 억제제 존제 하에 Lysyl Oxidase의 순수분리(純棒分離) -다양성(多形性)에 대(對)한 반론(反論)-)

  • Han, Song
    • Journal of Oral Medicine and Pain
    • /
    • v.25 no.1
    • /
    • pp.29-39
    • /
    • 2000
  • Lysyl Oxidase from fetal bovine aorta was purified to homogenity using extraction, Sephacryl S200HR chromatography, Hydropore AX ion-exchange high performance liquid column chromatography, Cibacron blue affinity chromatography, and Sephacryl S-300 HR chromatography in the presence of protease inhibitor. The purified enzyme was active toward lathyritic collagen as well as elastin and was sensitive to aminonitriles such as BAPN. Upon Sephacryl S-300 HR chromatography, the enzyme was eluted as a peak with a $K_{av}$ value of 0.45 (65% of $V_t$ ) and it eluted from high performance liquid ion-exchange column (Hydropore |AX) at single position (ionic strength, I = 0.1~0.15). Once purified, it showed one band upon SDS-PAGE. It migrated to a band the mobility of which corresponded to a Mr of 33,500 upon reduction while it migrated to a 24,500 Mr position under the non-reducing condition. In constrast to other reports, it is concluded that fetal bovine aorta contains only one type of lysy oxidase.

  • PDF

Bioequivalence Study of Hydrocortisone Tablets while Secretion of Endogenous Cortisol Suppressed

  • Ok, Tae-Suk;Lee, Kyoung-Jin;Shin, Young-Hee
    • Biomolecules & Therapeutics
    • /
    • v.16 no.3
    • /
    • pp.255-260
    • /
    • 2008
  • The purpose of this study was to evaluate the bioequivalence of the test (Daewoo Hydrocortisone 10 mg, Daewoo Pharm. Co., Busan, Korea) and reference (Jenapharm Hydrocortisone 10 mg, JayTech Biogen, Seoul, Korea) hydrocortisone tablets. Twenty-four healthy male Korean volunteers were divided into two groups with a randomized $2{\times}2$ cross-over design. In order to suppress the endogenous cortisol secretion, a single oral dose of Dexamethasone (4 mg) was administered 10 hr prior to hydrocortisone administration. Blood samples were withdrawn for 10 hr at the predetermined intervals after a single oral dose of hydrocortisone (20 mg). The serum concentration of hydrocortisone was analyzed by HPLC/UV using a column switching method after liquid-liquid extraction process. The pharmacokinetic parameters ($AUC_{0{\sim}10hr}$, $C_{max}$, and $T_{max}$) of the test and reference hydrocortisone tablets were determined while the secretion of endogenous cortisol was being suppressed. The pharmacokinetic parameters of the test tablet were not statistically different from those of the reference tablet at ex value was 0.05. The 90% confidence intervals for the average ratio (test/reference) of $AUC_{0{\sim}10hr}$ and $C_{max}$ were within the Korea Food and Drug Administration acceptance range of 0.80-1.25 ($0.89{\sim}0.99$ and $0.86{\sim}0.99$ for $AUC_{0{\sim}10hr}$ and $C_{max}$, respectively). Therefore it was concluded that the test tablet, Daewoo Hydrocortisone tablet was bioequivalent to the reference tablet, Jenapharm Hydrocortisone tablet.

Study on Subcritical Water Degradation of RDX Contaminated Soil in Batch and Dynamic Mode (배치형과 연속흐름형에 의한 토양 중 RDX의 아임계 분해특성 비교연구)

  • Choi, Jae-Heon;Lee, Hwan;Lee, Cheol-Hyo;Kim, Ju-Yup;Park, Jeong-Hun;Jo, Young-Tae
    • Journal of Soil and Groundwater Environment
    • /
    • v.20 no.6
    • /
    • pp.95-102
    • /
    • 2015
  • The purpose of this study is to compare the degradation characteristics by subcritical water of RDX contaminated soil using batch mode and dynamic mode devices. First, upon application of RDX contaminated soil, RDX treatment efficiency was increased with increasing the temperature in both modes. At 150℃, the treatment efficiency was 99.9%. RDX degradation efficiency got higher with lower ratio of solid to liquid. However, the treatment efficiency in the dynamic mode tended to be decreased at a certain ratio of solid to liquid or lower. The treatment efficiency was increased when it took longer time for the reactions in both modes. As the results of analysis on concentration of treated water after subcritical water degradation, the RDX recovery rate of dynamic and batch modes at 150℃ was 10.5% and 1.5%, respectively. However, both modes showed very similar recovery rates at 175℃ or higher. RDX degradation products were analyzed in treated water after it was treated with subcritical water. According to the results, RDX degradation mechanism was mostly oxidation reaction and reduction reaction was partially involved. Therefore, it suggested that most of RDX in soil was degraded by oxidation of subcritical water upon extraction. According to this result, it was found that both batch and dynamic modes were very effectively applied in the treatment of explosive contaminated soil.

Simplified HPLC Method for the Determination of Pseudoephedrine Hydrochloride from Allegra D Tablet

  • Park, Moon-Hee;Shin, In-Chul
    • Biomolecules & Therapeutics
    • /
    • v.15 no.2
    • /
    • pp.123-126
    • /
    • 2007
  • A sensitive, simple and highly selective liquid chromatography method of determination for extraction of pseudoephedrine hydrochloride from Allegra D tablet was developed. The chief benefit of the present method is the minimal sample preparation, as the procedure is only filtering through pore syringe filter. Two drugs (pseudoephedrine hydrochloride, fexofenadine) were separated on a C$_{18}$ column and analyzed by high performance liquid chromatography (HPLC). The method had a chromatographic run time of 8.0 min. 1 ml of pseudoephedrine hydrochloride solution (1 mg/ml) was filtered through 0.22 um pore syringe filter. 50 ul of filtering solution was injected to HPLC pump and we knew the retention time (1.85 min) of separating of pseudoephedrine hydrochloride using UV detector at 280 nm. We used C$_{18}$ column (4.6 mm${\times}$250 mm), mobile phase solution (<0.05 mol/L NaH$_2$PO$_4$, 2 ml/L H$_3$PO$_4$>/CH$_3$CN / sodium dodesyl sulfate = 60 ml / 40 ml / 1 g). We separated psedoephedrine hydrochloride at run time of 1.85 min from Allegra D tablet solution (1 mg/ml) filtered through 0.22 um pore syringe filter using UV detector at 280 nm. Flow rate was set at 1.0 ml/min and the column temperature was set at 40$^{\circ}C$. Psedoephedrine hydrochloride solution (1 mg/ml) separated from Allegra D tablet was filtered through 0.22 um pore syringe filter and injected 50 ul. We confirmed the peak of psedoephedrine hydrochloride at same retention time and the separating solution was freeze-dried. In conclusion, A simple isocratic reverse-phase HPLC method has been developed that provides excellent separation of pseudoephedrine from Allegra D tablet.

Distribution of Seven N-Nitrosamines in Food

  • Park, Jong-eun;Seo, Jung-eun;Lee, Jee-yeon;Kwon, Hoonjeong
    • Toxicological Research
    • /
    • v.31 no.3
    • /
    • pp.279-288
    • /
    • 2015
  • N-nitrosamines, which are classified as carcinogens by IARC and US EPA, can be easily found in various foods. They are reaction products between nitrogen oxide and secondary amines, but can also be generated during fermentation. Ever since the 1960s, when nitrite, used as a preservative in processed meats, was suspected to generate N-nitrosamines, the usage of the food additive has been debated. However, the benefit of nitrite in food supply could not be ignored and the risk-benefit analysis has become a key issue in the use of the additive. For a risk analysis, an accurate estimation of the hazardous material is necessary; therefore, analytical methods for nitrosamines have continuously evolved from the 1950s. Solid supported liquid-liquid extraction and solid phase extractions have replaced the distillation for the clean-up steps, and tandem mass spectrometry is employed for higher selectivity and sensitivity. In the present study, for a better estimation of N-nitrosamine intake, the total diet study samples were prepared for the N-nitrosamines analysis. In order to obtain the most sensitive results, a partial preparation procedure was developed and modified for different food matrices. Among seven N-nitrosamines (N-nitrosodimethylamine, N-nitrosomethylethylamine, N-nitrosodiethylamine, N-nitrosodibutylamine, N-nitrosopiperidine, N-nitrosopyrrolidine, and N-nitrosomorpholine) analyzed in the present study, N-nitrosodiethylamine has shown the highest detection rate in agricultural foods, while N-nitrosodimethylamine has appeared most frequently in livestock and fishery food products. The concentration of N-nitrosodimethylamine was the highest in seasoning.

Isolation and Identification of Major Component from Roots of Potentilla chinensis (딱지꽃(Potentilla chinensis) 뿌리 추출물의 주요성분 분리동정)

  • Jung, Hae Soo;Kim, Hyoung Shik;Lee, Jeong Hun;Moh, Seo Jin;Yeo, Jin Hui;Park, Gi won;Moh, Sang Hyun
    • Journal of Applied Biological Chemistry
    • /
    • v.59 no.1
    • /
    • pp.5-7
    • /
    • 2016
  • One of oriental medicinal plants, Potentilla chinensis, has been used for anti-inflammation, hemostatic, decryption, and antipyretic. Especially, a root of Potentilla chinensis was used as important material for oriental medication. Although several kinds of bioactive component of Potentilla chinensis extract from stems and leaves were identified, the major component of Potentilla chinensis from roots is not well established. In this study, the root of Potentilla chinensis was extracted in different solvent system and analyzed by high performance liquid chromatography (HPLC). According to HPLC analysis, a major component was isolated and its physicochemical properties were evaluated by mass spectrometry and nuclear magnetic resonance. Based on these results, isolated compound was identified as 2,3,8-Tri-O-methylellagic acid. And quantification of 2,3,8-Tri-O-methylellagic acid with different extraction solvent system was performed for industrial application.