• Title/Summary/Keyword: HPLC analysis

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Preparation and Physicochemical Properties of Soluble Dietary Fiber Extracts from Soymilk Residue at High Temperature (두유박 수용성 식이섬유의 고온 추출물 제조와 이화학적 특성구명)

  • Park, Chun-Ho;Kim, Hyun-Jung;Moon, Tae-Wha
    • Korean Journal of Food Science and Technology
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    • v.29 no.4
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    • pp.648-656
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    • 1997
  • Thermal treatment of soymilk residue was carried out at 140, 150, and $160^{\circ}C$ for possible use as a raw material for dietary fiber, and some physicochemical properties of the extracts were investigated. Soluble dietary fiber(SDF) content of the extracts prepared under optimal conditions was more than 30% suggesting the conversion of insoluble dietary fiber to SDF. The main sugar components of the extracts were glucose, galactose, and arabinose. Analysis of the moelcular weight distribution by high performance size exclusion chromatography revealed that the proportion of high molecular weight fraction decreased and that of middle-sized polymer increased as the extraction temperature increased. The viscosity of aqueous solution of the extracts decreased with an increase in extraction temperature, but showed no trend as pH changed. The solubility increased with extraction temperature showing the highest at $160^{\circ}C$. The extract at $140^{\circ}C$ had the biggest calcium-binding capacity, which correlated with the changes in viscosity.

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Bioequivalence Evaluation of Two Brands of Zolpidem Tartrate 10 mg Tablets(Zanilo and Stilnox) in Healthy Male Volunteers

  • Ryu, Ju-Hee;Lee, Heon-Woo;Lee, Hyun-Su;Kang, Il-Mo;Seo, Ji-Hyung;Kang, Jin-Yang;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.36 no.5
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    • pp.343-348
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    • 2006
  • The purpose of the present study was to evaluate the bioequivalence of two zolpidem tartrate tablets, Stilnox tablet(Sanofi-aventis Korea, reference product) and Zanilo tablet(ChoDang Pharm Co., Ltd., Korea, test product), according to the guidelines of Korea Food and Drug Administration(KFDA). After adding an internal standard(cimetropium), 250 ${\mu}L$ plasma samples were extracted using 1.3 mL of ethyl acetate. Extracted compounds were analyzed by HPLC with triple-quadrupole mass spectrometry. This method for determination of zolpidem is proved accurate and reproducible with the limit of quantitation of 1 ng/mL in human plasma. Twenty-four healthy male Korean volunteers received each medicine at the zolpidem tartrate dose of 10 mg in a $2{\times}2$ crossover study. There was one-week washout period between the doses. Plasma concentrations of zolpidem were monitored for over a period of 8 hr after the administration. $AUC_{0-t}$(the area under the plasma concentration-time curve) was calculated by the linear trapezoidal rule. $C_{max}$(maximum plasma drug concentration) and $T_{max}$(time to reach $C_{max}$) were compiled from the plasma concentration-time data. Analysis of variance was carried out using logarithmically transformed $AUC_{0-t}$ and $C_{max}$. No significant sequence effect was found for all of the bio-availability parameters indicating that the crossover design was properly performed. The 90% confidence intervals for the log transformed data were acceptable range of log 0.8 to log 1.25(e.g., log 0.92-log 1.06 for $AUC_{0-t}$, log 0.96-log 1.13 for $C_{max}$). The major parameters, $AUC_{0-t}$ and $C_{max}$ met the criteria of KFDA for bioequivalence indicating that Zanilo tablet is bioequivalent to Stilnox tablet.

Bioequivalence of RoxithrinTM Tablet to RulidTM Tablet (Roxithromycin 150 mg) (루리드 정(록시스로마이신 150 mg)에 대한 록시스린 정의 생물학적동등성)

  • Joung, Sun-Koung;Lee, Yun-Young;Cho, Tae-Seob;Kim, Ho-Hyun;Lee, Ye-Rie;Lee, Kyung-Ryul;Lee, Hee-Joo
    • Journal of Pharmaceutical Investigation
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    • v.34 no.3
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    • pp.209-214
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    • 2004
  • A bioequivalence study of $Roxithrin^{TM}$ tablet (Kukje Pharma. Ind. Co., Ltd.) to $Rulid^{TM}$ tablet (Han Dok Pharma. Ind. Co., Ltd.) was conducted according to the guidelines of Korea Food and Drug Administration (KFDA). Twenty four healthy male Korean volunteers received each medicine at the roxithromycin dose of 300 mg in a $2{\times}2$ crossover study. There was a one-week wash-out period between the doses. Plasma concentrations of roxithromycin were monitored by a high-performance liquid chromatography for over a period of 36 hours after drug administration. $AUC_t$ (the area under the plasma concentration-time curve from time zero to 36 hr) was calculated by the linear trapezoidal rule method. $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were compiled from the plasma concentration-time data. Analysis of variance was carried out using logarithmically transformed $AUC_t$ and $C_{max}$. No significant sequence effect was found for all of the bioavailability parameters indicating that the cross-over design was properly performed. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for $Roxithrin^{TM}/Rulid^{TM}$ were 1.00 - 1.13 and 0.98 - 1.10, respectively. These values were within the acceptable bioequivalence intervals of 0.80 - 1.25. Thus, our study demonstrated the bioequivalence of $Roxithrin^{TM}$ and $Rulid^{TM}$ with respect to the rate and extent of absorption.

Pharmacokinetic and Bioequivalence Study of Zolpidem Tartate in Healthy Volunteers

  • Park, Jun-Sung;Myung, Ja-Hye;Wang, Hun-Sik;Koo, Ja-Seong;Cho, Won-Kyung;Cha, Kwang-Ho;Park, Hee-Jun;Kim, Min-So;Kim, Jeong-Soo;Hwang, Sung-Joo
    • Journal of Pharmaceutical Investigation
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    • v.41 no.3
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    • pp.191-196
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    • 2011
  • In this study simple and sensitive high performance liquid chromatographic method using a commercially available column, was developed and validated for the determination of zolpidem tartrate in human plasma. The developed method with suitable validation was applied to a bioequivalence study of two different kinds of zolpidem tartrate. Two different formulations containing 10 mg of zolpidem tartate (CAS : 99294-93-6) were compared in 24 healthy male volunteers in order to compare the bioavailability and prove the bioequivalence. The study was performed in an open, single dose randomized, 2-sequence, cross-over design in 24 healthy male volunteers with a one-week washout period. Blood samples for pharmacokinetic profiling were drawn at selected times during 12 h. The mean $AUC_{0-12h}$, $C_{max}$, $T_{max}$ and $T_{1/2}$ were $676.6{\pm}223.4$ $ng{\cdot}h{\cdot}mL^{-1}$, $177.4{\pm}34.2$ $ng{\cdot}mL^{-1}$, and $0.8{\pm}0.4$ and $3.5{\pm}2.1$, respectively, for the test formulations, and $640.7{\pm}186.6$ $ng{\cdot}h{\cdot}mL^{-1}$, $193.0{\pm}64.5$ $ng{\cdot}mL^{-1}$, and $0.9{\pm}0.4$ and $2.7{\pm}0.9$, respectively, for the reference formulation. Both primary target parameters $AUC_{0-12h}$ and $C_{max}$ were log-transformed and tested parametrically by analysis of variance (ANOVA). 90% confidence intervals of $AUC_{0-12h}$ and $C_{max}$ were in the range of acceptable limits of bioequivalence (80-125%). Based on these results, the two formulations of zolpidem tartate are considered to be bioequivalent.

Establishment of analytical method of methiozolin and dissipation in golf course's green (Methiozolin의 분석법 개발 및 골프장 그린에서의 잔류소실특성)

  • Jo, Hyeong-Wook;Hwang, Kyu-won;Hwang, Ki-Hwan;Moon, Joon-Kwan
    • Journal of Applied Biological Chemistry
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    • v.59 no.4
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    • pp.331-336
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    • 2016
  • Analytical methods for methiozolin in soil, water and turfgrass were established and dissipation patterns of methiozolin in soil and turfgrass were elucidated. Analysis was done using a high performance liquid chromatography with an ultra violet detector at the wavelength of 280 nm after extraction with acetone, liquid-liquid partition with dichloromethane, and a solid phase extraction purification. Limit of determination and Limit of quantitation were 1.0, 0.5, 1.0 ng, and 0.001, 0.1, 0.01 mg/kg for water, turfgrass, and soil, respectively. Recovery rates of methiozolin from soil, water, and turfgrass were ranged 87.5~111.3, 92.8~97.4, and 78.2~98.5 %, respectively. The turfgrass and soil samples were collected at 0, 1, 4, 7, 14, 30, 45, and 60 after spray on green area in golf course. Residues of methiozlolin were not translocated to lower soil layer but detected only in turfgrasses and root area of turfgrass. Half-lives of methiozolin in turfgrass were 10.7 days and 8.8 days in soil from root area.

Protective effects of red ginseng according to steaming time on HCl/ethanol-induced acute gastritis (염산/에탄올로 유도된 급성 위염 동물모델에서 증숙시간에 따른 홍삼의 보호 효과)

  • Lee, Joo Young;Kwon, O Jun;Noh, Jeong Sook;Roh, Seong-Soo
    • Journal of Applied Biological Chemistry
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    • v.59 no.4
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    • pp.365-372
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    • 2016
  • The objective of the present study was to evaluate the protective effect of red ginseng (RG) according to steaming time on 150 mM HCl/60 % ethanol induced gastric ulcer models in mice. The sample was divided into 3 groups-G (dried ginseng), RG 4 (steamed 4 h and dried ginseng), RG 6 (steamed 6 h and dried ginseng), and determined through in vitro experiments, such as 1,1-diphenyl-2-picrylhydrazyl and 2,2'-azinobis-3-ethyl-benzothiazoline-6-sulfonic acid radical scavenging activity, HPLC analysis, total polyphenol, and flavonoid contents. In vitro experiment results were depended on steaming hours. Based on the results, we chose two samples (G, RG 6) and conducted in vivo experiments. Mice were divided into 5 groups: Nor (normal group), Con (acute gastritis mice treated with distilled water), G (gastris induced by HCl/Ethanol treated with 100 mg/kg G), RG 6 (gastris induced by HCl/ethanol treated with 100 mg/kg RG 6), and SC (gastris induced by HCl/Ethanol treated with 10 mg/kg sucralfate). In our results revealed that RG 6 suppressed elevated reactive oxygen species, and inflammatory related makers, such as cyclooxygenase-2, inducible nitric oxide synthase, tumor necrosis factor alpha, and interleukin-1 beta. In addition, gastric lesion area was improved. These results suggest that RG 6 protects the stomach by attenuating oxidative stress and inflammatory response under gastric ulcer conditions. Therefore, RG 6 should be a potential therapeutic agent for the treatment of acute gastric ulcer.

Characteristics of Seasonal Distributions of Fine Particles ($PM_{2.5}$) and Particle-Associated Polycyclic Aromatic Hydrocarbons in Urban, Metropolitan and Industrial Complex Sites (중소도시, 대도시 및 산업지역에서 채취한 미세분진 ($PM_{2.5}$)과 입자상 다환방향족탄화수소의 계절적인 분포 특성)

  • Kim He-Kap;Jung Kyung-Mi;Kim Tae-Sik
    • Environmental Analysis Health and Toxicology
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    • v.21 no.1 s.52
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    • pp.45-56
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    • 2006
  • This study was conducted to investigate seasonal distributions of fine particles ($PM_{2.5}$) and associated polycyclic aromatic hydrocarbons (PAHs) at three cities. $PM_{2.5}$ samples were collected on glass fiber filters at urban (Chuncheon), metropolitan (Seoul), and industrial complex sites (Ulsan) from September, 2002 to February, 2004 using the Andersen FH 95 Particulate Sampler. About five 24-hour samples were collected from each site per season. The filters were analyzed for mass and six selected PAHs concentrations. $PM_{2.5}$ concentrations were the highest either in winter or spring, which could be attributed to the increase of fossil fuel combustion in winter or the transport of yellow sand to the Korean peninsula from China in spring, respectively. Regional $PM_{2.5}$ concentrations were higher in the order of Seoul>Chuncheon>Ulsan without statistical difference among cities. The filters were extracted using dichloromethane in an ultrasonicator and analyzed for six PAHs (anthracene, fluoranthene, pyrene, benzo[a]anthracene, chrysene, and benzo[a]pyrene) with HPLC. Total PAHs concentrations were statistically different among seasons in each site, and the highest concentrations were observed in winter at each sampling site. For total samples collected, the median total PAHs concentrations in Chuncheon ($4.6ng/m^3$) and Seoul ($4.4ng/m^3$) were approximately two times higher than that in Ulsan ($2.1ng/m^3$). Chrysene was a component found in the highest proportion among total PAHs at each site. Carcinogenic risks calculated based on the BaP toxic equivalency factors (TEFs) over the whole sampling period were higher in the order of Chuncheon>Seoul>Ulsan. This study suggests that the atmosphere of Chuncheon is contaminated with particulate matter and PAHs at the levels equivalent to those of Seoul and that an appropriate measure needs to be taken to mitigate human health risks from inhalation exposure to airborne fine particles.

PHENOLIC ANTIOXIDANT CONTENT OF OLIVE OILS AND THEIR POTENTIAL IN THE PREVENTION OF CANCER

  • Owen Robdrt W;Spiegelhalder Bertold;Haubner Roswitha;Wurtele Gerd;Giacosa Attilio;Bartsch Helmut
    • Proceedings of the Korean Society of Food Science and Nutrition Conference
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    • 2001.12a
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    • pp.95-109
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    • 2001
  • The traditional (European) Mediterranean diet is characterized by an abundance of plant foods such as bread, pasta, vegetables, salad, legumes, fruit, nuts; olive oil as the principal source of fat; low to moderate amounts offish, poultry, dairy products and eggs; only small amounts of red meat; low to moderate amounts of wine, normally consumed with meals. This diet is low in saturated fatty acids, rich in carbohydrate and fibre, and has a high content of monounsaturated fatty acids (MUFA). These are primarily derived from olive oil. Despite a wealth of general knowledge concerning the major classes of compounds present in olives and olive oil, detailed knowledge of the phenolic antioxidant content has been lacking. Therefore the aim of the study was to evaluate the phenolic antioxidant content in a range of olive and seed oils. While seed oils were devoid, on average, the olive oils contained $196{\pm}19mg/kg$ total phenolics as judged by HPLC analysis, but the value for extravirgin ($232{\pm}15 mg/kg$) was significantly higher than that of refined virgin olive oil ($62{\pm}12mg/kg$; P<0.0001). Appreciable quantities of simple phenols (hydroxytyrosol and tyrosol) were detected in olive oils, with significant differences between extravirgin ($41.87{\pm}6.17$) and refined virgin olive oils ($4.72{\pm}2.15$; P<0.01). The major linked phenols were secoiridoids and lignans. Although extravirgin contained higher concentrations of secoiridoids ($27.72{\pm}6.84$) than refined olive oils ($9.30{\pm}3.81$) this difference was not significant. On the other hand the concentration of lignans was significantly higher (P<0.001) in extravirgin ($41.53{\pm}3.93$) compared to refined virgin olive oils ($7.29{\pm}2.56$). All classes of phenolics were shown to be potent antioxidants. In future epidemiolgic studies, both the nature and source of olive oil consumed should be differentiated in ascertaining cancer risk.

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Effect of hydrothermal processing on ginseng extract

  • Ryu, Jebin;Lee, Hun Wook;Yoon, Junho;Seo, Bumjoon;Kwon, Dong Eui;Shin, Un-Moo;Choi, Kwang-joon;Lee, Youn-Woo
    • Journal of Ginseng Research
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    • v.41 no.4
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    • pp.572-577
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    • 2017
  • Background: Panax ginseng Meyer is cultivated because of its medicinal effects on the immune system, blood pressure, and cancer. Major ginsenosides in fresh ginseng are converted to minor ginsenosides by structural changes such as hydrolysis and dehydration. The transformed ginsenosides are generally more bioavailable and bioactive than the primary ginsenosides. Therefore, in this study, hydrothermal processing was applied to ginseng preparation to increase the yields of the transformed ginsenosides, such as 20(S)-Rg3, Rk1, and Rg5, and enhance antioxidant activities in an effective way. Methods: Ginseng extract was hydrothermally processed using batch reactors at $100-160^{\circ}C$ with differing reaction times. Quantitative analysis of the ginsenoside yields was performed using HPLC, and the antioxidant activity was qualitatively analyzed by evaluating 2,2'-azino-bis radical cation scavenging, 2,2-diphenyl-1-picrylhydrazyl radical scavenging, and phenolic antioxidants. Red ginseng and sun ginseng were prepared by conventional steaming as the control group. Results: Unlike steaming, the hydrothermal process was performed under homogeneous conditions. Chemical reaction, heat transfer, and mass transfer are generally more efficient in homogeneous reactions. Therefore, maximum yields for the hydrothermal process were 2.5-25 times higher than those for steaming, and the antioxidant activities showed 1.6-4-fold increases for the hydrothermal process. Moreover, the reaction time was decreased from 3 h to 15-35 min using hydrothermal processing. Conclusion: Therefore, hydrothermal processing offers significant improvements over the conventional steaming process. In particular, at temperatures over $140^{\circ}C$, high yields of the transformed ginsenosides and increased antioxidant activities were obtained in tens of minutes.

Bioactivity-guided isolation of ginsenosides from Korean Red Ginseng with cytotoxic activity against human lung adenocarcinoma cells

  • Yu, Jae Sik;Roh, Hyun-Soo;Baek, Kwan-Hyuck;Lee, Seul;Kim, Sil;So, Hae Min;Moon, Eunjung;Pang, Changhyun;Jang, Tae Su;Kim, Ki Hyun
    • Journal of Ginseng Research
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    • v.42 no.4
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    • pp.562-570
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    • 2018
  • Background: Lung cancer is the leading cause of cancer-related death worldwide. In this study, we used a bioactivity-guided isolation technique to identify constituents of Korean Red Ginseng (KRG) with antiproliferative activity against human lung adenocarcinoma cells. Methods: Bioactivity-guided fractionation and preparative/semipreparative HPLC purification were used with LC/MS analysis to separate the bioactive constituents. Cell viability and apoptosis in human lung cancer cell lines (A549, H1264, H1299, and Calu-6) after treatment with KRG extract fractions and constituents thereof were assessed using the water-soluble tetrazolium salt (WST-1) assay and terminal deoxyribonucleotidyl transferase-mediated dUTP nick end labeling (TUNEL) staining, respectively. Caspase activation was assessed by detecting its surrogate marker, cleaved poly adenosine diphosphate (ADP-ribose) polymerase, using an immunoblot assay. The expression and subcellular localization of apoptosis-inducing factor were assessed using immunoblotting and immunofluorescence, respectively. Results and conclusion: Bioactivity-guided fractionation of the KRG extract revealed that its ethyl acetate-soluble fraction exerts significant cytotoxic activity against all human lung cancer cell lines tested by inducing apoptosis. Chemical investigation of the ethyl acetatesoluble fraction led to the isolation of six ginsenosides, including ginsenoside Rb1 (1), ginsenoside Rb2 (2), ginsenoside Rc (3), ginsenoside Rd (4), ginsenoside Rg1 (5), and ginsenoside Rg3 (6). Among the isolated ginsenosides, ginsenoside Rg3 exhibited the most cytotoxic activity against all human lung cancer cell lines examined, with $IC_{50}$ values ranging from $161.1{\mu}M$ to $264.6{\mu}M$. The cytotoxicity of ginsenoside Rg3 was found to be mediated by induction of apoptosis in a caspase-independent manner. These findings provide experimental evidence for a novel biological activity of ginsenoside Rg3 against human lung cancer cells.