• Title/Summary/Keyword: High performance Liquid Chromatography

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Determination of Adsorption Isotherms and Separation of L-arabinose and D-ribose in Cation Exchange Chromatography and HPLC (양이온 교환 크로마토그래피와 HPLC에서의 L-arabinose와 D-ribose의 분리 및 등온 흡착곡선 결정)

  • Jeon, Young-Ju;Kim, In-Ho
    • KSBB Journal
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    • v.23 no.1
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    • pp.31-36
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    • 2008
  • The use of L-carbohydrates and their corresponding nucleosides in medicinal application has greatly increased. For example L-ribose has been much in demand as the starting material for curing hepatitis B. High performance liquid chromatography (HPLC) method was studied for the analysis of ribose and arabinose fractions from ion exchange chromatography (IEC). Dowex Monosphere 99 Ca/320 resin was packed in IEC to separate ribose and arabinose under various operating conditions. $NH_{2}$ and sugar HPLC columns were then used to analyze the fractions from the IEC column. Pulse input method (PIM) was also used to measure adsorption isotherms of ribose and arabinose in the Dowex column and HPLC columns. Experimental results and simulations by ASPEN chromatography were compared with fair agreement.

Extraction and Characterization of an Anti-wrinkle Elastase Inhibitor from Rheum undulatum L. (대황(Rheum undulatum L.)으로부터 항주름성 Elastase 저해제의 추출 및 특성)

  • Lee, Jae-Won;Lee, Ji-Su;Lee, Jong-Soo
    • The Korean Journal of Food And Nutrition
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    • v.21 no.2
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    • pp.143-147
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    • 2008
  • To develop a new anti-wrinkle agent from medicinal plants, this study investigated the optimal conditions for extracting elastase inhibitor from Rheum undulatum L. Maximal extraction occurred by using 70% methanol at $50^{\circ}C$ for 24 hr; the elastase inhibitory activity was 60.4%($IC_{50}:6.7{\times}10^3{\mu}g/m{\ell}$). Systematic solvent extraction, thin layer chromatography, silica gel column chromatography, Sephadex LH-20 column chromatography, and reverse-phase high performance liquid chromatography were used in the partial purification of the elastase inhibitor. The compound was soluble in dimethylsulfoxide, methanol, and ethanol, and had maximum absorption spectra at 231.5 nm and 275.5 nm.

Identification of 3-methoxy-4-hydroxybenzoic acid and 4-hydroxybenzoic acid with Antioxidative and Antimicrobial Activity from arachis hypogaea Shell (땅콩껍질에서 항균 및 항산화활성이 있는 3-methoxy-4-hydroxybenzoic acid와 4-hydroxybenzoic acid의 동정)

  • 위지향;박근형
    • KSBB Journal
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    • v.15 no.5
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    • pp.464-468
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    • 2000
  • The methanol extract of Arachis hypogaea shell showed antioxidative and antimicrobial activity. The methanol extract was successively purified by solvent fractionation, silica gel adsorption column chromatography, Sephadex LH-20 column chromatography and octadecylsilane column chromatography. The purified active substances were isolated by high performance liquid chromatography, and were identified as 3-methoxy-4-hydroxybenzoic acid and 4-hydroxybenzoic acid by LC-MS and GC-MS. The amount of 3-methoxy-4-hydroxybenzoic acid and 4-hydroxybenzoic acid were 3.8mg and 9.8 mg per kg of shell, respectively.

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Pharmacokinetic Analysis of Levofloxacin in Healthy Korean Volunteers

  • Kim, Seung-Yong;Chung, Youn-Bok;Pyo, Hee-Soo;Kwon, Oh-Seung
    • Journal of Pharmaceutical Investigation
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    • v.38 no.4
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    • pp.235-240
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    • 2008
  • A sensitive and simple method of determining the plasma levofloxacin (LFX, CAS 100986-85-4) concentrations in human volunteers by liquid-liquid extraction were developed and validated by using a high-performance liquid chromatography/diode array detector. The method was also applied to pharmacokinetic study of LFX. LFX was orally administered to 8 healthy male Korean volunteers at single lowest dose of 200 mg, compared to the published reports in which more than 500 mg of LFX was orally administered. LFX in human plasma was determined. The detection limit of LFX was $0.05\;{\mu}g/mL$. $C_{max}$ value was $2.48{\pm}0.67\;{\mu}g/mL$. $AUC_{0{\to}24\;hr$} and $AUC_{0{\to}{\infty}}$ were $14.52{\pm}3.35\;{\mu}g/mL$ and $16.00{\pm}3.66\;{\mu}g{\cdot}hr/mL$, respectively. The terminal half-life was $6.87{\pm}0.46\;hr$. Our pharmacokinetic parameters were very consistent with that previously reported, showing good correlation between LFX doses and AUC ($r^2=0.995$). This method can be useful for the pharmacokinetics and bioequivalence study with relatively low dose for reducing the main side effects of LFX.

The effect of liposomal cephalexin on the dry period treatment of bovine Staphylococcus aureus mastitis (젖소의 Staphylococcus aureus성 유방염에 대한 liposomal cephalexin 의 건유기 치료효과)

  • Shin, Jin-ho;Han, Hong-ryul
    • Korean Journal of Veterinary Research
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    • v.32 no.2
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    • pp.251-258
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    • 1992
  • Liposomal cephalexin was used m the dry period treatment of bovine mastitis due to Staphylococcus aureus. Liposomes were prepared by stable plurilamellar vesicle(SPLV) process. The shape and size of SPLVs were examined by transmission electron microscopy. The entrapping efficiency and stability of SPLVs were determined by high performance liquid chromatography or liquid scintillation counting. The size of SPLVs ranged from 0.1 to $4.01{\mu}m$ in diameter, with an entrapping efficiency of cephalexin of 25.8 %. The formulation of liposomal cephalexin was used for treatment were SPLV-entrapped cephalexin and free cephalexin with total cephalexin concentration of 250mg per quarters. All quarters were infused intramammarily at the end of lactation period by liposomal cephalexin, free cephalexin, or blank liposome with free cephalexin. The number of quarters cured by liposomal cephalexin(14/15 quarters, 93 %) was significantly higher than that by free cephalexin(7/15 quarters, 46%). or by blank liposome with free cephalexin(8/15 quarters, 53 % ) (p<0.05).

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Optimization of analytical conditions for the determination of nitrosamines in chlorinated tap water by high performance liquid chromatography (액체크로마토그래피를 이용한 수돗물 중 nitrosamine 화합물 분석의 최적화)

  • Han, Ki-Chan;Kim, He-Kap
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.551-559
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    • 2010
  • This study was conducted to establish an analytical method for the determination of seven nitrosamines in chlorinated tap water by precolumn derivatization followed by high performance liquid chromatography coupled with fluorescence detection. The derivatization procedure was optimized for denitrosation and dansylation, and then two extraction methods, liquid-liquid extraction (LLE) with dichloromethane and solid phase extraction (SPE), were compared. The SPE method employing the optimized derivation procedure showed higher extraction recovery (54.4-88.7%) and reproducibility (1.9-19.4%) than the LLE method (51.4-87.7% and 4.2-33.3%, respectively). The method detection limits were between 0.5 and 4.4 ng/L. When chlorinated water samples were collected from two treatment plants and ten household taps, and analyzed for nitrosamines, Nnitrosodimethylamine (NDMA) was the major compound found between 26.1 and 112 ng/L.

Comparison of Preparation Methods for the Quantification of Ginsenosides in Raw Korean Ginseng

  • Hong, Hee-Do;Sim, Eun-Mi;Kim, Kyung-Tack;Rho, Jeong-Hae;Rhee, Young-Kyung;Cho, Chang-Won
    • Food Science and Biotechnology
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    • v.18 no.2
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    • pp.565-569
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    • 2009
  • This study was conducted to evaluate the effects of different preparation methods on the recovery and quantification of ginsenosides in raw Korean ginseng (Panax ginseng C.A. Meyer). Eight major ginsenosides ($Rb_1$, $Rb_2$, $Rb_3$, Rc, Rd, Re, Rf, and $Rg_1$) were analyzed by high performance liquid chromatography (HPLC), after which the recovery and repeatability of the extraction of those ginsenosides using 3 different preparation methods were compared [A. direct extraction (DE) method, hot MeOH extraction/evaporation/direct dissolution; B. solid phase extraction (SPE) method, hot MeOH extraction/evaporation/dissolution/$C_{18}$ cartridge adsorption/MeOH elution; C. liquid-liquid extraction (LLE) method, hot MeOH extraction/evaporation/dissolution/n-BuOH fractionation]. Use of the DE method resulted in a significantly higher recovery of total ginsenosides than other methods and a relatively clear peak resolution. Use of the SPE and LLE methods resulted in clearer peak resolution, but lower ginsenoside recovery than the DE method. The LLE method showed the lowest ginsenoside recovery and repeatability among the 3 methods. Given that the DE method employed only extraction, evaporation, and a dissolution step (avoiding complicate and time consuming purification), this technique may be an effective method for the preparation and quantification of ginsenosides from raw Korean ginseng.

Simultaneous Determination of Amitraz, Bromopropylate, Coumaphos, Cymiazole and 2,4-Dimethylaniline in Korean Honey Samples by High-Performance Liquid Chromatography

  • Ryoo, Jae-Jeong;Kim, Se-Hoon;Jeong, Young-Han;Do, Hwan-Suk;Ryu, Jeong-Eun;Kwon, Hae-Young;Jeong, Ji-Yoon;Park, Hye-Jin;Lee, Soon-Ho;Hong, Moo-Ki;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.29 no.5
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    • pp.1043-1047
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    • 2008
  • Simultaneous determination of amitraz, bromopropylate, coumaphos, cymiazole and 2,4-dimethylaniline in 200 honey samples purchased in Korea was performed by reversed-phase high-performance liquid chromatography with multiple UV detection. 2% Acetone in hexane was used for a liquid-liquid extraction and 20-40% water in acetonitrile solutions were used as mobile phases. The LOD for the analytes varied between 0.4 and 1.5 $\mu$g/L and the recoveries were yielded between 64 and 94%. Relative standard deviation of the repeatability of the method is less than 15%. Amitraz was not present in amount above 10 $\mu$ g/L and one for coumaphos and cymiazole and two for bromopropylate, and three for 2,4-dimethylanilne were detected in amount above 10 $\mu$ g/ L. Levels of the acaricide residues found were less than 50 $\mu$ g/L.

Analysis of tetracyclines in shrimp samples based on a two-step extraction approach prior to high-performance liquid chromatography

  • Thinnakorn Sukkhunthod;Thanakorn Pluangklang;Sumita Boonnab;Sira Sansuk;Phitchan Sricharoen;Maliwan Subsadsana
    • Analytical Science and Technology
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    • v.37 no.4
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    • pp.211-219
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    • 2024
  • This study presents a sensitive and reliable method for determining tetracycline (TC), oxytetracycline (OTC), and chlortetracycline (CTC) residues in shrimp samples. A two-step process involving liquid-liquid extraction (LLE) followed by solid-phase extraction (SPE) was developed prior to HPLC analysis. The target analytes were effectively extracted using EDTA/McIlvaine buffer (pH 4.0): methanol (80:20, %v/v), with subsequent clean-up using a C18 SPE cartridge. HPLC separation was conducted on a C18 column (250 mm × 4.6 mm i.d., 5 ㎛) at 30 ℃, using 0.01 % trifluoroacetic acid (A) and acetonitrile (B) as the mobile phase. A gradient elution protocol was applied, transitioning from 85(A):15(B) %v/v to 70(A):30(B) %v/v at 7 min, with a 5 min hold, followed by adjustment to 85(A):15(B) %v/v for 13-14 min. The detection was performed using photodiode array (PDA) at 365 nm with a flow rate of 1.0 mL/min. The calibration curves exhibited good linearity within a concentration range of 0.4-6.0 ㎍/mL (R2 > 0.995). The limits of detection (LOD) for TC, OTC, and CTC in shrimp were 0.034, 0.029, and 0.021 ㎍/mL, respectively. The limits of quantitation (LOQ) for TC, OTC, and CTC were found to be 0.114, 0.097, and 0.071 ㎍/mL, respectively. Recoveries of TC, OTC, and CTC from spiked shrimp samples ranged from 91.0 % to 95.5 %, 92.4 % to 97.2 %, and 93.3 % to 96.6 %, respectively. This method was successfully applied to the determination of TC, OTC, and CTC residues in shrimp samples sourced from various local markets.

Detection of Undeclared Betamethasone Derivatives in Cosmetic Products Labeled to Contain Zinc Pyrithione as the Active Ingredient (아연피리치온을 유효성분으로 표기한 화장품류에서 미표기 성분인 베타메타손 유도체의 검출)

  • Lee, Jeong-Pyo;Park, Sung-Hwan;Yang, Seong-Jun;Kim, Sun-Mi;Son, Kyung-Hun;Yun, Mi-Ok;Choi, Sang-Sook
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.35 no.1
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    • pp.11-17
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    • 2009
  • Betamethasone propionate, an anti-inflammatory glucocorticosteroid, was detected in cosmetics with no indication on the label of this compound as an ingredient. The product was formulated as a topical spray or shampoo and labeled to contain zinc pyrithione as the active ingredient. A thin-layer chromatographic analysis was carried out on silica gel plates to provide a first indication about the presence of a compound with steroid structure and reactivity; then high-performance liquid chromatography (HPLC) separation allowed the identification of the corticosteroid agent and its quantification. To identify the corticosteroid agent from these commercial samples we collected the fractions suspected to have ketol steroids by prep HPLC and identified the compound as betamethasone propionate by NMR and MS spectrometry. Then we synthesized the standard for the betamethasone 17-propionate and 21-propionate and quantitate the corticosteroids from the sample by HPLC with that standards. By this method we identified the corticosteroid compounds from some commercial cosmetics such as zinc pyrithione sprays. The finding of betamethasone propionate in the products was shown by comparison to an authenticated standard of betamethasone propionate by retention time on reverse-phase HPLC. Two of the tested products contained betamethasone propionate at the levels of 0.005 ${\sim}$ 0.02% and the others were free of betamethasone propionate.