• Title/Summary/Keyword: Liquid Liquid Extraction

Search Result 1,075, Processing Time 0.03 seconds

Validated HPLC Method for the Pharmacokinetic Study of Atenolol and Chlorthalidone Combination Therapy in Korean Subjects

  • Kang, Hyun-Ah;Kim, Hwan-Ho;Kim, Se-Mi;Yoon, Hwa;Cho, Hea-Young;Oh, Seaung-Youl;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
    • /
    • v.36 no.5
    • /
    • pp.331-338
    • /
    • 2006
  • A rapid, selective and sensitive reverse-phase HPLC methods for the determination of atenolol and chlorthalidone in human serum and whole blood were validated, and applied to the pharmacokinetic study of atenolol and chlorthalidone combination therapy. Atenolol and an internal standard, pindolol, were extracted from human serum by liquid-liquid extraction, and analyzed on a $\mu$-Bondapak C18 $10-{\mu}$ column in a mobile phase of methanol-0.01 M potassium dihydrogenphosphate(30:70, v/v, adjusted to pH 3.5) and fluorescence detection(emission: 300 nm, excitation: 224 nm). Chlorthalidone and an internal standard, probenecid, were extracted form human whole blood by liquid-liquid extraction, and analyzed on a Luna C18 $5-{\mu}$ column in a mobile phase of acetonitrile containing 77% 0.01 M sodium acetate and UV detection at 214 nm. These analysis were performed at three different laboratories using the same quality control(QC) samples. The chromatograms showed good resolution, sensitivity, and no interference by human serum and whole blood, respectively. The methods showed linear responses over a concentration range of 10-1,000 ng/mL for atenolol and 0.05-20 ${\mu}g/mL$ for chlorthalidone, with correlation coefficients of greater than 0.999 at all the three laboratories. Intra- and inter-day assay precision and accuracy fulfilled international requirements. Stability studies(freeze-thaw, short-, long-term, extracted sample and stock solution) showed that atenolol and chlorthalidone were stable. The lower limit of quantitation of atenolol and chlorthalidone were 10 ng/mL and 0.05 ${\mu}g/mL$, respectively, which was sensitive enough for pharmacokinetic studies. These methods were applied to the pharmacokinetic study of atenolol and chlorthalidone in human volunteers following a single oral administration of Hyundai $Tenoretic^{\circledR}$ tablet(atenolol 50 mg and chlorthalidone 12.5 mg) at three different laboratories.

A Study on the Elution Behavior of Pd-Isonitroso ethylacetoacetate imine Chelates by Reversed-phase High Performance Liquid Chromatography (역상 고성능 액체 크로마토 그래피에 의한 Pd(II) - isonitrosoethylacetoacetate imine 유도체 킬레이트의 용리거동에 관한 연구)

  • Kim, Hyun
    • Journal of the Society of Cosmetic Scientists of Korea
    • /
    • v.19 no.1
    • /
    • pp.20-30
    • /
    • 1993
  • Liquid Chromatographic behavior of Pd(II) in Isonitosoethylacetoacetate imine IEAA-NR: R=H, CH3, C2H5, n-C3H7, n-C4H9, C6H5-CH2) Chelates were investigated by reversed phase high performance 1iquid chromatography on Micropak MCH-5 Column using Methanol /water as mobile phase. The optimum condition for the separation of Pd-Isonitrosoethylacetoacetate imine chelates were examined with respect to the flow rate, mobile phase strength. It was found that Pd(IEAA-NR)2 chelates were eluted in an acceptable range of the capacity factor value (0 $\leq$ log k' $\leq$ 1), The dependence of the logarithm of capacity factor(k') on the volume fraction of water in mixture with in the binary mobile phase was examined. Also, the dependence of k'on the liquid-liquid extraction distribution constant in methanol-water / n-alkane extraction system was on system was invert tigated for Pd(IEAA-NR)2. Both kinds of dependence are linear, which suggests that the retention of the electroneutral metal chelates be largely due to the solvophobic effect.

  • PDF

Studies on the Simultaneous Analysis of Organochlorine Pesticide Residues by Gas-Liquid Chromatography (I). Solvent Extraction and Cleanup of Pesticides (기체-액체 크로마토그래피에 의한 잔류 유기염소제 농약들의 동시 분석에 관한 연구 (제1보). 농약의 용매추출 및 불순물 제거)

  • Taek-Jae Kim;Song-Ja Park;Young-Sang Kim
    • Journal of the Korean Chemical Society
    • /
    • v.29 no.5
    • /
    • pp.496-502
    • /
    • 1985
  • The solvent extraction and cleanup processes for the simultaneous gas-liquid cliromatographic determination of 16 kinds of organochlorine pesticide residues were investigated. The pesticides were extracted out from-various crops with the aqueous acetone solution acidified (pH < 1.5) by adding conc. $H_3PO_4$. Most of the pesticides were partitioned from the solution with petroleum ether. Evaporated the extracting solvent, the residues were dissolved in ethylether-petroleum ether (6 : 94) eluent and eluted through the Florisil column activated at 650$^{\circ}$C for 2.5hrs. The extraction efficiency was over 94% and impurities were effectively removed by the column chromatography.

  • PDF

A study on Calcination Characteristics of Powdered Oyster Shell (굴패각 재활용 방안에 관한 기초연구 -굴패각 소성가공특성-)

  • Kim, Jong-Oh;Lee, Sang Eun;Lee, Chang-Ho
    • Journal of the Korea Organic Resources Recycling Association
    • /
    • v.15 no.1
    • /
    • pp.143-148
    • /
    • 2007
  • The objective of this study was to investigate the proper conditions of calcination and calcium extraction from powdered oyster shell. The physical characteristics such as particle size distribution, surface morphology, and thermal gravity were examined. The following result were obtained. As the powdered oyster shell was ignited in high temperature of $650^{\circ}C$ to $950^{\circ}C$, the calcination reactions was effectively progressed. The amount of weight loss during calcination would be matched with the generation of carbon dioxide gas. In the calcination of powdered oyster shell, the amount of weight loss increased according to the increased of calcination temperature and the decrease of mean particle size. It was founded that the proper temperature and retention time of calcination was $850^{\circ}C$ and 40 minute. In the extraction of calcium into liquid form using acid addition, the calcination oyster shell was more effective than the non-calcinated shell. The liquid calcium extraction technique using the calcinated oyster shell needed more researches considering cost evaluation.

  • PDF

Evaluation of Grinding Effects on the Extraction of Photosynthetic Pigments for HPLC Analysis (광합성 색소의 HPLC 분석을 위한 여과지 분쇄 효과 평가)

  • Jang, Su Jin;Park, Mi Ok
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
    • /
    • v.20 no.2
    • /
    • pp.71-77
    • /
    • 2015
  • High-Performance Liquid Chromatography (HPLC) is a widely used method for measuring the concentration of chlorophyll a as an indicator for estimating phytoplankton biomass and primary production and also for identifying carotenoids to determine phytoplankton composition. However, tissue grinding procedure requires a lot of time and experience in the analysis of multiple sample. Accordingly, we measured the concentrations of photosynthetic pigments before and after the grinding, in order to understand the grinding effects on the quantitative analysis of chlorophylls and carotenoids using samples from southwestern East Sea. When tissue grinding procedure was omitted, we found that Chl a concentrations were underestimated up to 45% in average. Also, concentrations of Zeaxanthin, 19'-butanoyloxyfucoxanthin, 19'-hexanoyloxyfucoxanthin, biomarkers of pico and nano-size phytoplankton, were underestimated up to maximum 77~85% without grinding. We found that the smaller the phytoplankton, the bigger underestimation of their biomarker pigments concentration is likely to happen due to the incomplete extraction. Thus, tissue grinding procedure should be included for HPLC analysis in all cases, to prevent the underestimation of not only Chl a but also carotenoids pigments.

Competitive Extraction and Trace Analysis of BTEX and MTBE by Solid-Phase Microextraction (SPME) (고체상미량추출법을 이용한 BTEX와 MTBE의 경쟁적 추출효과 및 미량분석에 관한 연구)

  • An, Sang-Woo;Chun, Suk-Young;Lee, Si-Jin;Park, Jae-Woo;Chang, Soon-Woong
    • Journal of Korean Society on Water Environment
    • /
    • v.26 no.4
    • /
    • pp.622-628
    • /
    • 2010
  • In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of BTEX and MTBE. Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50 mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of BTEX and MTBE. The general affinity of analytes to CAR/PDMS fiber was high in the order p-Xylene>Toluene>Ethylbenzene>MTBE>Benzene. The linearity of $R^2$ for BTEX and MTBE was from 0.970 to 0.999 when analyte concentration ranges from $30{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.5% to 3.2% for concentration of $100{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for BTEX and MTBE were from $7.5{\mu}g/L$ to $15{\mu}g/L$, respectively.

Study on the Development of Practical Application of Indigo Dyes (실용화를 위한 쪽 염료의 관한 연구)

  • Lee, Sang-Phil;Kim, Soon-Hee
    • The Research Journal of the Costume Culture
    • /
    • v.19 no.3
    • /
    • pp.612-621
    • /
    • 2011
  • The process of making or cultivating indigo dyes is very cumbersome and complex. The dye extraction and dyeing methods using general plant dye, moth repellent dye, fast acting natural dye, and other dyes are very different. This research investigates the extraction of indigo dye and liquid dye extraction of polygonum(indigo) plants using calcium oxide water. While extracting indigo dye the concentration of purified indigo dye may be controlled by adjusting the pH level. Due to the various uses of dyes the adjustment of surface color must be considered. In regard to the change according to different concentrations of reducing agents, it was found that cotton fabrics and ramie fabrics show the highest color difference at 0.4% and 0.3% respectively. As the reduction temperature increases, the color difference increases as well. The maximum color difference was found to appear at $90^{\circ}C$. Cotton fabrics and ramie fabrics showed 70.55 and 67.01 respectively. The color difference increases as the concentration of dyes increases, but at a concentration of 300%, cotton fabrics was found to show 6.22PB in H value using the Munsell color system, containing purple and blue color. The pH of the polygonum dyes extracted through this experiment were adjusted by adding calcium oxide to the experimental water, without directly adding calcium oxide to the liquid polygonum extract. In a refine state, it was mixed with polygonum extract to extract a more refine and highly concentrated indigo dye. When lye and reducing agents are added to extracted indigo dye and sealed for long-term storage, it can be effective and easily used for dyeing.

Solvent Selection for the Detection of Siloxanes in Landfill gas (매립가스내 규소화합물류 검출을 위한 용매선택에 관한 연구)

  • Kim, Nack-Joo;Choi, Ju-Mi;Ji, Eun-Jung
    • Journal of Korean Society of Environmental Engineers
    • /
    • v.29 no.8
    • /
    • pp.915-921
    • /
    • 2007
  • As a preliminary measurement of siloxanes in landfill gas(LFG), this study was conducted to determine the best suitable solvent applicable to the extraction of siloxanes in the domestic landfill using liquid-absorption method. Three solvents of n-hexane, acetone, and methanol were tested and the results obtained from GC analysis for each solvent were compared to their properties. Results showed that the resolution in the GC spectrum was the best from methanol due to the lack of overlapping of the peaks between silane and solvent. The detected siloxanes concentration were varied at maximum 2.6 times depending on the types of solvent as well as extraction velocity and impinger steps. In total, the highest concentration of siloxanes was obtained from methanol, which showed ideal pattern in the absorption of each impinger step and the least relative standard deviation. Accordingly, it is concluded that methanol is the most suitable solvent for the extraction of siloxanes in the domestic landfill. However, it is considered that solvent suitability can vary depending on the waste components and landfill record in landfills.

The study of characterization of extracted vanadium in waste catalyst for vanadium redox flow battery (폐촉매에서 추출한 바나듐 레독스 흐름전지용 바나듐의 특성 연구)

  • Kang, Ung Il
    • Journal of the Korea Academia-Industrial cooperation Society
    • /
    • v.19 no.10
    • /
    • pp.598-602
    • /
    • 2018
  • This study examined the characteristics of the waste catalyst used in the petroleum refinery operations. The total pore volume, specific surface area, and average pore size of the spent catalyst used in the petroleum refinery operations were 3.96cc/g, 13.81m2/g, and 1.15A, respectively. The weight loss observed in the range from $25^{\circ}C-700^{\circ}C$ for the spent catalysts using TG and DTA was approximately 23 wt. %. EDS analysis of the waste catalyst sample showed that the five major components were vanadium, nickel, manganese, iron, and copper. The extraction system is attractive for liquid-liquid extraction. In this study, Cynex 272 was used to extract vanadium from waste catalyst. The electrochemical characteristics of the extracted vanadium solution were measured by cyclic voltammetry (CV). As a result, an oxidation / reduction peak appeared, indicating the potential of an electrolytic solution.

Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC (HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구)

  • Oh, Bo Young;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
    • /
    • v.43 no.6
    • /
    • pp.663-669
    • /
    • 1999
  • For determination of separated pesticides by using GC and HPLC, liquid-liquid extraction(LLE) and solid phase extraction(SPE) have been carried out to separate and concentrate the organophophorous pesticides such as Diazinon, Fenitrothion, Phosmet, Phosalon and EPN in environmental water samples. ln determination of pesticides by HPLC/UV, SPE has resulted in higher recovery and more precision than LLE, while in determination of pesticides by GC/FPD, vice versa. HPLC/UV after the pretreatment process of sample by solid phase extraction (SPE-HPLC/UV) has suggested the possibility of determination of pesticides ppb level. ln comparison of detection limit, both SPE-HPLC/UV and LLE-GC/FPD are reasonably suitable for analysis of residue pesticides. ln the respect of the rapidity and the solvent required, SPE-HPLC/UV method has proven to be superior to LLE-GC/FPD.

  • PDF