• Title/Summary/Keyword: 고성능 액체 크로마토그래피

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Empirical Equation for Resolution if Ibuprofen Enantiomers by Chiral High-Performance Liquid Chromatography (키랄 고성능 액체 크로마토그래피를 이용하 이부프로펜의 분리도에 관한 실험식)

  • 여미순;노경호
    • KSBB Journal
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    • v.18 no.4
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    • pp.261-265
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    • 2003
  • Ibuprofen was analyzed by chiral high performance liquid chromatography. Retention behaviours of the standard mixtures of ibuprofen were investigated to obtain their acceptable resolution. A chromatographic column (3.9 ${\times}$ 300 mm) was packed by Kromasil CHI-TBB packings (10 $\mu\textrm{m}$) and n-hexane was used as a mobile phase with 0.1% acetic acid and tert-butyl methyl ether. Isocratic elution of ibuprofen at 1.0 $m\ell$/min was performed by changing the mobile phase compositions. The experimental variables affecting the resolution were the compositions of mobile phase and chemical buffer (n-hexane and tert-butyl methyl ether). The resolution between the enantiomers were correlated into the several types of empirical equations including linear form, and their agreements between experimental data and calculated values were examined by the regression coefficient.

Bitter Peptides Derived from ${\alpha}_{s1}-and\;{\beta}-Casein$ Digested with Alkaline Protease from Bacillus subtilis (Bacillus subtilis의 염기성 프로테아제로 분해된 ${\alpha}_{s1}$- 및 ${\beta}$-카세인에서 분리된 쓴 맛 펩타이드)

  • Sohn, Kyung-Hyun;Lee, Hyong-Joo
    • Korean Journal of Food Science and Technology
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    • v.20 no.5
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    • pp.659-665
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    • 1988
  • The ${\alpha}_{s1}$-and ${\beta}$-casein were purified by DEAE-cellulose chromatography and digested with alkaline protease from Bacillus subtilis. Bitter fractions from the hydrolyzates were isolated using n-butanol extraction, Sephadex G-25 gel chromatography, and high performance liquid chromatography. Peptide mixtures were separated by reverse-phase octadecyl silica column with linear gradient of 0-80% acetonitrile containing 0.1% trifluoroacetic acid. Major peaks were combined from replicate chromatographies and the bitterness of each peak was evaluated. The bitter-tasting peaks were rechromatograpied until isolated peaks were obtained. Three different bitter peptides(BP-I, BP-II, BP-III) were obtained from the ${\alpha}_{s1}$-casein hydrolyzate. BP-I was eluted at 34% acetonitrile and BP-II, 35%, BP-III, 26%, respectively. Two bitter peptides(BP-IV, BP-V) were isolated from the ${\beta}-casein$ hydrolyzate: BP-IV was eluted at 40% acetonitrile and BP-V, 42%. BP-V was the most hydrophobic peptide in the five bitter peptides. However, BP-I and BP-II tasted more bitter than BP-IV and BP-V.

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Development of Simultaneous Analysis Method for Dimenhydrinate Containing Complex Pharmaceuticals Using RP-HPLC (고성능 역상 액체 크로마토그래피(RP-HPLC)를 이용한 Dimenhydrinate 함유 복합제제의 동시분석법 개발)

  • Keun-Sik Shin;Jin-Young Park;Jae-Ho Sim
    • The Journal of the Convergence on Culture Technology
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    • v.10 no.5
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    • pp.775-780
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    • 2024
  • In this study, a simultaneous analysis method was developed using reversed-phase high-performance liquid chromatography(RP-HPLC) for the main components of motion sickness medication: Dimenhydrinate, Caffeine, Methyl Paraben, and Propyl Paraben. The analysis was conducted after pretreating the four components, utilizing a C18 column with Acetonitrile and H2O as the mobile phase. UV detection was carried out at a wavelength of 254nm. As a result of the experiment, the values of Resolution(Rs) was well over Rs > 1.5, which indicates that the separation of the four components was efficient. Additionally, the symmetry factor of the components was 0.989, 1.120, 1.256, and 1.280, respectively, showing their symmetrical stability. In the stability assessment, the calibration curves for the four components showed excellent linearity with R2 > 0.9991 to 0.9998. Furthermore, the limit of detection(LOD) ranged between 0.017 to 3.060㎍/ml, while the limit of quantification(LOQ) ranged between 0.050 to 9.180 ㎍/ml. The recovery rates range from 98.28% to 101.71%, and repeatability showed precision within the range of 0.447 to 0.550, and robustness confirmed values with %RSD < 2. The quantitative analysis results of this study demonstrated the effectiveness of a simultaneous analysis method for motion sickness medication components.

High Purity Extraction and Simultaneous High-performance Liquid Chromatography Analysis of Curcuminoids in Turmeric (강황에서 curcuminoids의 고순도 추출 및 고성능 액체 크로마토그래피 동시분석)

  • Lee, Kwang-Jin;Ma, Jin-Yeul;Kim, Young-Sik;Kim, Dong-Seon;Jin, Yinzhe
    • Journal of Applied Biological Chemistry
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    • v.55 no.1
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    • pp.61-65
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    • 2012
  • Three major curcuminoids in turmeric (Curcuma longa), curcumin, demethoxycurcumin, and bisdemethoxycurcumin, were efficiently extracted by optimizing extraction condition and simultaneously analyzed and identified using reverse phase high-performance liquid chromatography, thin-layer chromatography, and liquid chromatography-mass spectrometry method. The highest yield of extraction amount 0.279 g, 9.30% was obtained by dipping method with extraction time of 7 h.

Simultaneous Enantiomer Separation of α-Amino Acids and Their Esters as Fluorenylmethoxycarbonyl Derivatives under UV and Fluorescence Detection by High Performance Liquid Chromatography (고성능 액체 크로마토그래피에서 아미노산과 이들 에스테르의 플루오레닐메톡시카르보닐 유도체의 자외선과 형광 검출에서의 동시 광학분리)

  • Islam, Md. Fokhrul;Lee, Wonjae
    • KSBB Journal
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    • v.30 no.4
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    • pp.197-201
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    • 2015
  • Liquid chromatographic enantiomer separation of ${\alpha}$-amino acids and their methyl and ethyl esters as fluorenylmethoxycarbonyl (FMOC) derivatives was performed using a recently developed chiral column (Chiralpak IE) based on polysaccharide derivative under simultaneous UV detection and fluorescence detection. The degree of enantiomer separation of ${\alpha}$-amino acid esters as FMOC derivatives is generally higher than that of the corresponding ${\alpha}$-amino acids. Especially, ${\alpha}$-amino acid methyl esters showed the greatest enantioseparation. As this method developed in this study can be applied to determine the chemical and optical purity of ${\alpha}$-amino acids and esters, it is expected to be quite useful for their chiral separation using Chiralpak IE.

The Pharmacokinetic Study of Josamycin in Flounder by Reversed Phase High Performance Liquid Chromatography (고성능 역상 액체 크로마토그래피를 이용한 넙치에서의 Josamycin의 약물동태에 관한 연구)

  • 오수연;장원철
    • Toxicological Research
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    • v.14 no.4
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    • pp.563-567
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    • 1998
  • This study was conducted to observe the distribution of josamycin, a macrolide antibiotic in flounder. Josamycin was administered orally to the flounder at the dose of 100 mg 1 kg josamycin in flounder. Josamycin in blood and various organs of flounder was analyzed using reversed phase HPLC. In blood kinetics study, Cmax was shown 9.50 $\mu\textrm{g}$/$m\ell$ at 45 min. after treatment and then decreased slowly up to 8th day. Concentration of josamycin in muscle was 0.47$\mu\textrm{g}$/g tissue at 11th day of the treatment and 0.41$\mu\textrm{g}$/g tissue at 7th day for liver. The concentration of josamycin in all the tested organs except gall bladder was decreased as the time passed. On the contrary, josamycin in gall bladder was increased 3.8 times at the day of 5th compared to that of the 1st day aftreatment.

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Determination of Glutathione in Biological Samples by Ion-pairing HPLC/FLD (이온쌍 HPLC/FLD를 이용한 생체 시료중의 Glutathione 농도 분석)

  • Yoo, Jeong-Yeon;Lee, Kyoung-Ok;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.12 no.1
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    • pp.28-33
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    • 1999
  • Glutathione(GSH) in biological samples was determined by high performance liquid chromatographic(HPLC) method with fluorescence detector(FLD) after monobromobimane(MBB) or 4-fluoro-7-sulfobenzofurazan(SBD-F) derivatization. The detection limit of $0.03{\mu}g/mL$ was obtained after MBB derivatization, derivative of MBB was about 200 times more sensitive than that of SBD-F. N-acetylcysteine was used as internal standard and tetrabutylammonium ion as counter ion for better separation. The determination by ion-pairing chromatography after MBB derivatization was characterized by linearity in the range between $0.08{\sim}8.33{\mu}g/mL$ with a good correlation coefficient of 0.998. By precision test appeared relative standard deviation at less than 5% at three different concentrations. This method can be used for the analysis of GSH in plasma and tissue.

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Discrimination of Hanwoo from Holstein and Mixed Beef by DHPLC (변성 고성능 액체 크로마토그래피를 이용한 한우, 젖소 그리고 혼입육의 구분)

  • Ahn, Young-Chang;Cho, Min-Ho;Seo, Jae-Won;Yoon, Il-Kyu;Jung, Duck-Hyun;Lee, Eun-Young;Nam, Youn-Hyoung;Park, Su-Min;Jang, Won-Cheoul
    • Journal of the Korean Chemical Society
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    • v.53 no.6
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    • pp.742-748
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    • 2009
  • In the meat industry, correct breed information in food labeling is required to assure meat quality. Genetic markers provide corroborating evidence to identify breed. We described the development of DNA markers to discriminate between Korean beef cattle (Hanwoo), Holstein, and mixed cow beefs. As most breeds are standardized for coat colour, the melanocortin 1 receptor (MC1R) gene, involved in the regulation of eu/pheomelanins synthesis, has been suggested as marker for breed traceability of products of animal origin. We also designed sex-determining region Y (SRY) gene specific primers for Y chromosome detection. In this study, fragments of MC1R gene and SRY gene were amplified by multiplex-PCR and subjected to digestion by MspA1I restriction endonuclease. Reaction products were analysised by denaturing high performance liquid chromatography (DHPLC). As a result, we identified 6 DHPLC peak types from MC1R gene and SRY gene analysis. DHPLC method showed more sensitive than RFLP method for DNA fragments analysis. Therefore, DHPLC method can apply to identify for Hanwoo, Holstein and mixed beef.

Separation and Determination of Co(II) and Ni(II) Ion as their 4-(2-Pyridylazo) resorcinol Chelates by Reversed-Phase Capillary High-Performance Liquid Chromatography (역상 모세관-고성능 액체 크로마토그래피에 의한 코발트와 니켈 이온의 4-(2-피리딜아조)레조루신올 킬레이트로서의 분리 및 정량)

  • Chung, Yong-Soon;Chung, Won-Seog
    • Journal of the Korean Chemical Society
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    • v.47 no.6
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    • pp.547-552
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    • 2003
  • Separation and determinations of Co(II) and Ni(II) ions as their 4-(2-pyridylazo)resorcinol(PAR) chelates by reversed-phase capillary high-performance liquid chromatography(RP-CpHPLC) were performed. Among many capillary columns, Vydac C4 column was selected and acetonitrile solution was used as mobile phase. The effect of pH and MeCN concentration(%) on the retention factor, k and peak intensity was examined and discussed. As a results, it was found that 22.5% MeCN and pH 5.60 was adequate as mobile phase for the separation of the two metal ions and determination of Co(II) ion, but the mobile phase condition for Ni(II) ion determination was 22.5% MeCN of pH 7.20. Detection limit(D.L., S/N=3) of Co(II) and Ni(II) ions were $2.0{\times}10{-7}$ M(14.9 ppb) and $1.0{\times}10{-6}$ M(59.2 ppb), respectively.

COMPARISON OF MONOMER RELEASE FROM PIT AND FISSURE SEALANT FOLLOWING VARIOUS SURFACE TREATMENT (치면열구전색제의 광중합 후 표면 처리 방법에 따른 미반응 모노머 용리 비교)

  • Lee, Sang-Woo;Lee, Ju-Hyun;Seo, Hyun-Woo;Park, Ho-Won
    • Journal of the korean academy of Pediatric Dentistry
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    • v.33 no.1
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    • pp.70-76
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    • 2006
  • The aim of this study was comparison of effectiveness of surface treatment methods in reducing the oxygen-inhibited layer of a commercially available freshly polymerized, light cured dental sealant($concise^{TM}$, 3M, St Paul, USA). Surface treatment groups were consisted of no treatment(negative control group) and 3 experimental groups according to surface treatment of light-cured sealant. Experimental group I was 10 seconds' exposure to distilled water syringe, group II was 10 seconds' manual application using a cotton pellet wetted with 75% alcohol and group III was 10 seconds' prophylaxis with pumice/water slurry using rubber cup on a slow-speed handpiece. All specimens were immersed in 5ml distilled water and stored at 37c water bath for 10 minutes. All eluates were analyzed by HLPC for identification and quantitive analysis of monomers. The results of this study can be summarized as follows. 1. None of the chromatograms of the tested sealant displayed peaks with the same retention time as that of the standard solution, except for TEGDMA. 2. All surface treatment group had a statistically significant decrease of monomer release in comparison with no treatment group. 3. Removal effects of unreacted monomer in group III was statistically significant in comparison with group I and group II. These results revealed that mechanical method using pumice and rubber cup is the most effective in removing residual monomer and may be valuable to be used effectively in clinic.

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