• Title/Summary/Keyword: separation of mixture

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Validation of a Simple HPLC Method for Determination of Nicardipine in Human Plasma and Its Application to Single-dose Pharmacokinetics (인체 혈장 중 니카르디핀의 정량을 위한 HPLC 분석법 검증 및 단일 용량 투여에 의한 약물동태 연구)

  • Im, Ho-Taek;Cho, Sung-Hee;Lee, Heon-Woo;Park, Wan-Su;Rew, Jae-Hwan;Choi, Young-Wook;Yong, Chul-Soon;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.35 no.6
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    • pp.461-465
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    • 2005
  • A simple HPLC method with ultraviolet detection of nicardipine in human plasma was developed and validated. After drug extraction with solid phase extraction (SPE) method, chromatographic separation of nicardipine in plasma was achieved at $30^{\circ}C$ with a $C_{18}$ column and acetonitrile-0.02% phosphate buffer mixture (with 0.02% triethylamine, final pH 7.0), as mobile phase. Quantitative determination was performed by ultraviolet detection at 254 nm. The method was specific and validated with a limit of quantification of 5 ng/mL. The intra- and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification. The applicability of the method was demonstrated by analysis of plasma after oral administration of a single 40 mg dose to 8 healthy subjects. From the plasma nicardipine concentration versus time curves, the mean $AUC_{t}$, was $134.04{\pm}59.72\;ng\;hr/mL$ and $C_{max}$ of $108.65{\pm}69.17\;ng/mL$ reached 1.5 hr after administration. The mean biological half-life of nicardipine was $3.93{\pm}0.82\;hr$. Based on the results, this simple and validated assay method could readily be used in any pharmacokinetic or bioequivalence studies using human.

Quantitative Analysis of Ellagic Acid in Nymphaea tetragona Georgi Root by HPLC-UVD (HPLC-UVD를 이용한 수련(Nymphaea tetragona Georgi)의 Ellagic Acid 정량 분석)

  • Lee, Dong Young;Jeong, Eun Ju;Jeon, Byung Ju;Sung, Sang Hyun
    • Korean Journal of Pharmacognosy
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    • v.45 no.1
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    • pp.84-87
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    • 2014
  • A high performance liquid chromatography (HPLC) method for the quantitation of ellagic acid in Nymphaea tetragona was developed for the quality control of functional cosmetic ingredient, the extract of N. tetragona. Separation and quantitation were successfully achieved with a Kromasil C18 column ($5{\mu}m$, $250mm{\times}4.6mm$, i.d.) by isocratic elution of a mixture of acetonitrile containing 0.1% trifluoroacetic acid and water containing 0.03% phosphoric acid at a flow rate of 1.0 ml/min. The UV detector was used for the detection and the wavelength for quantitation was set at 254 nm. The presence of ellagic acid in the extract was determined by comparison of retention time and spiking with authentic standard. Analytical results showed good linearity ($R^2=0.99996$) in relatively wide concentration ranges. The R.S.D. for precision test was less than 3.0%. Recovery of the compound was 98.55~101.72% with R.S.D values less than 4.0%. In conclusion, this method has been successfully applied to the determination of ellagic acid in N. tetragona.

HORIZON EXPANSION OF THERMAL-HYDRAULIC ACTIVITIES INTO HTGR SAFETY ANALYSIS INCLUDING GAS-TURBINE CYCLE AND HYDROGEN PLANT

  • No, Hee-Cheon;Yoon, Ho-Joon;Kim, Seung-Jun;Lee, Byeng-Jin;Kim, Ji-Hwang;Kim, Hyeun-Min;Lim, Hong-Sik
    • Nuclear Engineering and Technology
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    • v.41 no.7
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    • pp.875-884
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    • 2009
  • We present three nuclear/hydrogen-related R&D activities being performed at KAIST: air-ingressed LOCA analysis code development, gas turbine analysis tool development, and hydrogen-production system analysis model development. The ICE numerical technique widely used for the safety analysis of water-reactors is successfully implemented into GAMMA, with which we solve the basic equations for continuity, momentum conservation, energy conservation of the gas mixture, and mass conservation of 6 species (He, N2, O2, CO, CO2, and H2O). GAMMA has been extensively validated using data from 14 test facilities. We developed a tool to predict the characteristics of HTGR helium turbines based on the throughflow calculation with a Newton-Raphson method that overcomes the weakness of the conventional method based on the successive iteration scheme. It is found that the current method reaches stable and quick convergence even under the off-normal condition with the same degree of accuracy. The dynamic equations for the distillation column of HI process are described with 4 material components involved in the HI process: H2O, HI, I2, H2. For the HI process we improved the Neumann model based on the NRTL (Non-Random Two-Liquid) model. The improved Neumann model predicted a total pressure with 8.6% maximum relative deviation from the data and 2.5% mean relative deviation, and liquid-liquid-separation with 9.52% maximum relative deviation from the data.

Cemento-Ossifying Fibroma in the Fracture Area of Mandibular Body: a Case Report (하악 체부 골절부위에 이환된 백악질 골화성 섬유종: 증례보고)

  • Jung, Tae-Young;Kim, So-Hyun;Jo, Hyun-Joo;Park, Sang-Jun
    • Maxillofacial Plastic and Reconstructive Surgery
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    • v.32 no.5
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    • pp.484-487
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    • 2010
  • Cemento-ossifying fibroma is a true osteogenic neoplasm. It is also called as ossifying fibroma or cementify-ing fibroma. Small lesions seldom cause any symptoms and are detected only on radiographic examination. Large lesions result in a painless swelling of the involved bone. In radiographic features the lesion most often is well defined and unilocular. It may appear completely radiolucent, or more often varying degrees of rdiopacity. It is composed of fibrous tissue that contains a variable mixture of bony trabeculae,cementum-like spherules, or both. Treatment of most lesions generally is enucleation of tumor. However, some lesions which have grown large and destroyed considerable bone, may necessitate surgical resection and bone grafting. This case was the bony lesion that was found by accident in patient with mandibular left body and subcondylar fracture. In radiographic examination, there was a mixed radiolucent and radiopaque lesion in mandibular left body area with fracture line. We treated on mandibular left body and subcondylar fracture and enucleated the lesion on the left body area simultaneously. At surgical exploration, the lesion was well demarcated from the surrounding bone, thus permitting relatively easy separation of the tumor from its bony bed. In histopathologic examination, the lesion contained bony trabeculae and cementum-like spherules within a background of cellular fibrous connective tissue. It finally diagnosed as cemento-ossify-ing fibroma from the result of biopsy.

Simultaneous Determination of Paeoniflorin and Glycyrrhizin in Sayuk-san by HPLC/DAD

  • Lee, Mi-Kyeong;Lee, Ki-Yong;Kim, Seung-Hyun;Jeon, Min-Ji;Cho, Jung-Hee;Oh, Mi-Hyun;Baek, Ju-Hyun;Kim, Hyo-Jin;Sung, Sang-Hyun
    • Journal of Pharmaceutical Investigation
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    • v.39 no.1
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    • pp.23-27
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    • 2009
  • A high performance liquid chromatographic (HPLC) method for the simultaneous determination of marker constituents, paeoniflorin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Sayuk-san (SYS). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, $4.6mm\;I.D.{\times}150mm$) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 mL/min. The diode-array UV/vis detector (DAD) was used for the detection and the wavelength for quantification was set at 230 nm. The presence of paeoniflorin and glycyrrhizin in this decoction was ascertained by retention time, spiking with each authentic standard and UV spectrum. All two compounds showed good linearity ($r^2$>0.996) in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 7.3% and the limits of detection (LOD) were less than 55.7 ng. The mean recovery of each compound was $102.3{\sim}111.1%$ with R.S.D. values less than 4.6%. This method was successfully applied to the determination of contents of paeoniflorin and glycyrrhizin in three commercial products of SYS. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial SYS products.

Functional graphene sheets-TiO2 nanocomposites and their photocatalytic performance for wastewater treatment

  • R. Aitbelale;A. Timesli;A. Sahibed-dine
    • Advances in nano research
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    • v.15 no.4
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    • pp.295-304
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    • 2023
  • In this paper, a powerful photocatalyst based on carbon nanocomposite is developed in order to obtain a new material applicable in water treatment and especially for the discoloration of effluents used in the textile industry. For that, TiO2-graphene nanocomposites have been successfully synthesized by a mixture of Functionalized Graphene Sheet (FGS) and tetrachlorotitanium complexes to form FGS-TiO2 nanocomposite. In the presence of an anionic surfactant, we used a new chemical process to functionalize graphene sheets in order to make them an excellent medium for blocking and preventing the aggregation of TiO2 nanoparticles. The components of these nanocomposites are characterized by means of X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM), which confirms the successful formation of the FGS-TiO2 nanocomposite. It was found that the TiO2 nanoparticles were dispersed uniformly on the graphene plane which possesses better charge separation capability than pure TiO2. The FGS-TiO2 nanocomposites exhibited higher photocatalytic activity compared to pure TiO2 for the removal of three dyes: such as Methylene Blue (MB), Bromophenol Blue (BB) and Alizarin Red-S (AR) in water. The removal process was fast and more efficient with FGS-TiO2 nanocomposite in daylight (in the absence of UV irradiation) compared to pure TiO2 nanoparticles without and under UV in all pH range.

Kinetic Studies on Homopolymerization of $\alpha$-Methylstyrene and Sequential Block Copolymerization of Isobutylene with $\alpha$-Methylstyrene by Living/Controlled Cationic Polymerization (리빙/조절 양이온중합에 의한 알파메틸스티렌 호모중합 및 이소부틸렌과의 블록공중합에 대한 반응속도론 연구)

  • Wu, Yibo;Guo, Wenli;Li, Shuxin;Gong, Huiqing
    • Polymer(Korea)
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    • v.32 no.4
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    • pp.366-371
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    • 2008
  • The controlled/living cationic polymerization of $\alpha$-methylstyrene (${\alpha}MeSt$) and sequential block copolymerization of isobutylene (IB) with ${\alpha}MeSt$ were achieved using 2-chloro-2,4,4-trimethylpentane (TMPCl)/titanium tetrachloride ($TiCl_4$)/titanium isopropoxide ($Ti(OiPr)_4$)/2,6-ditert-butylpyridine (DtBP) initiating system in $CH_3Cl$/hexane(50/50 v/v) solvent mixture at $-80^{\circ}C$. The polymerization rate decreased with increasing $[Ti(OiPr)_4]/[TiCl_4]$ ratio in the homopolymerization of ${\alpha}MeSt$. The effects of $[Ti(OiPr)_4]/[TiCl_4]$ ratios and $PIB^+$ molecular weight on the polymerization rate and blocking efficiency were also investigated. Well-defined poly(isobutylene-b-$\alpha$-methylstyrene)s were demonstrated by $^1H$-NMR and triple detection SEC; refractive index (RI), multiangle laser light scattering (MALLS) and ultraviolet (UV) detectors. Blocking efficiencies for the poly(isobutylene-b-$\alpha$-methylstyrene)s of almost 100% were obtained when ${\alpha}MeSt$ was induced by PIB's of $M_n\;{\geq}\;41000$ at $[Ti(OiPr)_4]/[TiCl_4]=1$. Differential scanning calorimetry (DSC) of the block copolymers showed two glass transition temperatures, thereby demonstrating microphase separation.

A Comparison of Sampling and Analytical Methods for Airborne Isocyanates (공기중 이소시아네이트류의 측정 및 분석방법에 관한 비교연구)

  • 변혜정;윤충식;백남원
    • Journal of Environmental Health Sciences
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    • v.22 no.2
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    • pp.32-42
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    • 1996
  • This study was performed to evaluate accuracy and precision of filter method and impinger method for analyzin airborne isocyanates in mixture (2, 6-TDI, HDI, 2, 4-TDI, MDI). Filter method was performed using the OSHA Method 42 and impinger method using the NIOSH Method 5521. The samples were analyzed by high performance liquid chromatography-ultraviolet detector (HPLC-UVD). After the optimum operating conditions for each method were investigated, samples with various concentration levels were quantified at the conditions. The precision was expressed by the pooled coefficient of variation(C.V.) and the accuracy by overall accuracy. The results are summarized as follows: 1. The optimum condition of filter method was determined at 35/65 ACN/buffer (0.01 M ammonium acetate) in mobile phase. And in case of impinger method, it was at 30/70 ACN/buffer(0.2 M sodium acetate). The effect of concentrations of acetate on the separation of the peaks was not significant, but, the effect of ACN/buffer ratio was significant. 2. The correlation coefficients for the two methods were above 0.9 in all isocyanate compounds. Average recovery efficiencies for 2, 6-TDI, HDI, 2, 4-TDI and MDI in filter method were 92.4%, 102.6%, 87.3% and 101.0%, respectively. Those in impinger method were 106.6%, 106.7%, 99.0% and 103.6%, respectively. As a result, the recovery efficiency of impinger method was higher than those of filter method in analyzing isocyanate compounds. 3. The pooled coefficients of variations of the methods were slightly higher than expected. The overall accuracies of the methods were within $\pm 25%$ for each isocyanate compound. Since these results satisfy NIOSH criteria, the accuracy of the experiment is appropriate. 4. As seen above, impinger method is more efficient than filter method. But, there are many disadvantages in impinger method. Therefore, solid sorbent such as a glass fiber filter must be developed in order to have the high efficiency not less than that of impinger method in the future.

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Quantitation of fructo- and inulo-oligosaccharides by high performance liquid chromatography (High performance liquid chromatography에 의한 fructo 및 inulo올리고당의 정량)

  • Kang, Su-Il;Han, Jong-In;Kim, Kyoung-Youn;Oh, Sun-Jin;Kim, Su-Il
    • Applied Biological Chemistry
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    • v.36 no.4
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    • pp.310-314
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    • 1993
  • High performance liquid chromatographic method using a TSK-gel amide 80 column and isocratic elution with acetonitrile-water (63 :35 ;v/v) mixture was used for the separation and the quantitation of fructo (GF2-GF7)- and inulo-oligosaccharides (F2-F4). Retention time of each standard carbohydrate was highly reproducible. Standardization curves obtained by plotting the peak areas against the amounts of each carbohydrate showed very high coefficient of determination$({\ge}0.9884)$ and similar slopes, and a wide range of y-intercepts. Our results suggest the use of each Pure oligosaccharide for its own standardization curve instead of using a certain carbohydrate as an internal standard.

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Effect of Toluene Added to Casting Solution on Characteristic of Phase Inversion Polysulfone Membrane (상전환 공정에 의한 폴리설폰막의 제조에 있어 제막용액에 첨가된 톨루엔의 영향)

  • Choi, Seung-Rag;Park, So-Jin;Seo, Bum-Kyoung;Lee, Kune Woo;Han, Myeong-Jin
    • Applied Chemistry for Engineering
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    • v.19 no.6
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    • pp.633-639
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    • 2008
  • Polysulfone membranes were prepared via the phase inversion process. Toluene was added as a nonsolvent additive in the casting solution containing a mixture of polysulfone and n-methylpyrrolidone. When prepared via the diffusion-induced process using isopropanol as a precipitation nonsolvent, the solidified membranes revealed a similar asymmetric structure irrespective of the addition of toluene, presenting both a dense skin layer and a sponge-like support layer. The added toluene played a role of enhancing liquid-liquid phase separation of the casting solution, and skin layer thickness of a prepared membrane increased with toluene content in the casting solution. On membrane performance, the solute rejection showed a uniform behavior irrespective of the addition of toluene. However, in spite of the significant increase in dense skin layer thickness, the water permeation through the membrane prepared with 60 wt% toluene revealed five times as much flux, compared with that of the membrane prepared without toluene additive.