• Title/Summary/Keyword: Fluorescence method

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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
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    • v.36 no.5
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    • pp.331-338
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    • 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.

Bioequivalence of Cadilan Tablet 12.5 mg to Dilatrend® Tablet 12.5 mg (Carvedilol 12.5 mg) (딜라트렌 정 12.5밀리그람(카르베딜롤 12.5밀리그람)에 대한 카딜란 정 12.5밀리그람의 생물학적동등성)

  • Kim, Se-Mi;Shin, Sae-Byeok;Kim, Ju-Hwan;Kwon, In-Ho;Kim, Yong-Hee;Lee, Sang-No;Cho, Hea-Young;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.38 no.6
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    • pp.413-419
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    • 2008
  • Carvedilol, is a nonselective $\beta$-blocking agent and it also has vasodilating properties that are attributed mainly to its blocking activity at ${\alpha}_1$-receptors. The purpose of the present study was to evaluate the bioequivalence of two carvedilol tablets, $Dilatrend^{(R)}$ tablet 12.5 mg (Chong Kun Dang Pharmaceutical Co., Ltd.) and Cadilan tablet 12.5 mg (KyungDong Pharmaceutical. Co., Ltd.), according to the guidelines of the Korea Food and Drug Administration (KFDA). The release of carvedilol from the two carvedilol formulations in vitro was tested using KP VIII Apparatus II method with pH 4.5 dissolution medium. Thirty two healthy male subjects, $25.00{\pm}3.09$ years in age and $70.71{\pm}11.35\;kg$ in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After a single tablet containing 12.5 mg as carvedilol was orally administered, blood samples were taken at predetermined time intervals and the concentrations of carvedilol in serum were determined using HPLC with fluorescence detector. The dissolution profiles of two formulations were similar in the tested dissolution medium. The pharmacokinetic parameters such as $AUC_t$, $C_{max}$ and $T_{max}$ were calculated and ANOVA test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$, $C_{max}$ and untransformed $T_{max}$. The results showed that the differences between two formulations based on the reference drug, $Dilatrend^{(R)}$ tablet 12.5 mg, were 4.66%, 8.33% and -7.45% for $AUC_t$, $C_{max}$ and $T_{max}$, respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log 0.8 to log 1.25 (e.g., $\log\;0.9823{\sim}\log\;1.1042$ and $\log\;1.0132{\sim}\log\;1.1875$ for $AUC_t$ and $C_{max}$, respectively). Thus, the criteria of the KFDA bioequivalence guideline were satisfied, indicating Cadilan tablet 12.5 mg was bioequivalent to $Dilatrend^{(R)}$ tablet 12.5 mg.

A Study on Chemical Composition and Firing Temperature of White Wares from the Guyre-2ri Kiln Sites, Wonju (원주 귀래2리 가마터 출토 백자의 화학조성과 소성온도 연구)

  • Lee, Byeong Hoon;So, Myoung-Gi
    • Journal of Conservation Science
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    • v.30 no.3
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    • pp.249-261
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    • 2014
  • This study aims to examine production technique of white wares from the Guyre-2ri 1st and 2nd kiln sites, Wonju, Gangwon Province and characteristics of the used materials, and to find a correlation among materials of the excavated white wares. X-ray fluorescence sequential spectroscopy(XRF), X-ray diffraction(XRD), Dilatometer and Inductively coupled plasma mass spectrometry(ICP-MS), Inductively coupled plasma automic emission spectrometer(ICP-AES) were applied to determine the chemical composition, crystalline phase of samples, firing temperatures, trace elements and rare earth elements. White wares from the Guyre-2ri kiln sites contained high contents of coloring oxides and fluxes. Though firing temperature of each sample was different, they were mostly fired at a temperature below $1200^{\circ}C$ and some of them experienced a low temperature of $1000^{\circ}C{\pm}20^{\circ}C$ and a high temperature above $1200^{\circ}C$. When analyzing body crystalline phases of the white wares using the XRD method, quartz and mullite were extracted from all the samples, and the proportions were similar to each other. When analyzing the excavated white wares using the Seger formula, also, all the samples showed similar clay sources and production techniques. Moreover, the white wares were made of host rocks of the same geological origin, according to the result of rare earth elements analysis.

Analysis on the Microbial Community Structure of Red Granule in the Anaerobic Ammonium Oxidation Reactor (혐기성 암모늄 산화 반응기 내 붉은색 입상슬러지의 미생물 군집구조 분석)

  • Bae, Hyo-Kwan;Park, Kyung-Soon;Chung, Yun-Chul;Jung, Jin-Young
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.10
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    • pp.1055-1064
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    • 2006
  • Extremely slow growing anammox(anaerobic ammonium oxidation) bacteria were cultivated using a combination of UASB(Upflow Anaerobic Sludge Blanket) reactor seeded with anaerobic granular sludge and carbon-fiber cultivating reactor. After 180 days of continuous cultivation, average nitrogen removal rate showed 0.54 kg $N/m^3-day$ when 0.6 kg $N/m^3-day$ of nitrogen loading was applied. The black granule was changed to brown and red granule as continuous operation, and the red granule was highly dependant on the high anammox activity. Microbial community structure of red granule in the UASB reactor was analyzed by molecular methods such as gene cloning, phylogenetic tree analysis, and FISH(Fluorescence In Situ Hybridization) method. As a result of gene cloning and phylogenetic tree analysis, 5 kinds of phylum were found to be Planctomycetes, Proteobacteria, Acidobacteria, Chlorobi and Chloroflexi. 13 clones were matched to anammox bacteria among 51 clones in the red anammox granule. In-silico test which used cloning information and FISH probe of the AMX368 was conducted to detect the presence of anammox bacteria in the red anammox granule. As a result of in-silico test only one clone was exactly matched to AMX368 but 11 clones was mutated one base among 18 bases representing all 12 clones are anammox bacteria. A filamentous Chloroflexi might be related to the granulation of anammox bacteria. As a result of FISH analysis, anammox bacteria was abundant in the red anammox granule.

Bioequivalence Test of Rebamipide 100 mg Tablets (레바미피드 100 mg 정제의 새울학적동등성)

  • Kim, Se-Mi;Cho, Hea-Young;Kang, Hyun-Ah;Lee, Yong-Bok
    • Korean Journal of Clinical Pharmacy
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    • v.18 no.1
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    • pp.38-44
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    • 2008
  • Rebamipide, ($\pm$)-2-(4-chlorobenzoylamino)-3-[2(1H)-quinolinon-4-yl] propionic acid, is used for mucosal protection, healing of gastroduodenal ulcers, and treatment of gastritis. It works by enhancing mucosal defense, scavenging free radicals and temporarily activating genes encoding cyclooxygenase-2. The purpose of the present study was to evaluate the bioequivalence of two rebamipide tablets, $Mucosta^{(R)}$ (Korea Otsuca Pharmaceuticals Co., Ltd.) and Mustar (Korean Drug Co., Ltd.), according to the guidelines of the Korea Food and Drug Administration (KFDA). The release of rebamipide from the two rebamipide formulations in vitro was tested using KP VIII Apparatus II method with pH 6.8 dissolution medium. Twenty six healthy male subjects, $23.46{\pm}2.63$ years in age and $66.62{\pm}8.97\;kg$ in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After a single tablet containing 100 mg as rebamipide was orally administered, blood samples were taken at predetermined time intervals and the concentrations of rebamipide in serum were determined using HPLC with fluorescence detector. The dissolution profiles of two formulations were similar in the tested dissolution medium. The pharmacokinetic parameters such as $AUC_t$, $C_{max}$ and $T_{max}$ were calculated, and ANOVA test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$, $C_{max}$ and untransformed $T_{max}$. The results showed that the differences between two formulations based on the reference drug, $Mucosta^{(R)}$ were -5.08, 3.52 and -9.71 % for $AUC_t$, $C_{max}$ and $T_{max}$, respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log 0.8 to log 1.25 (e.g., log 0.84$\sim$log 1.07 and log 0.90$\sim$log 1.17 for $AUC_t$ and $C_{max}$, respectively). Thus, the criteria of the KFDA bioequivalence guideline were satisfied, indicating Mustar tablet was bioequivalent to $Mucosta^{(R)}$ tablet.

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Enhancement of Immune Activities of Canavalia gladiata & Arctium lappa complexes in immobilization stress mouse model. (부동화 스트레스 유도 마우스 모델에서 도두(刀豆), 우방근(牛蒡根) 복합물의 면역증진 작용)

  • Lee, Ji-eun;Roh, Seong-Soo;Kim, Han-Young;Kim, Kun-hoae;Kim, Seung-Hyung
    • The Korea Journal of Herbology
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    • v.32 no.1
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    • pp.1-13
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    • 2017
  • Objective : Soybeans of Canavalia gladiata(CG) and root of Arctium lappa(AL) have been reported to have anti-inflammatory, antioxidant effect. However, the immunoregulatory mechanisms of its combinational prescription remain a matter of considerable debate. In the current study, we investigated whether CG and AL and its combinational prescription(CG+AL) regulate immune system using chronic immobilization-stress mouse model. Methods : C57BL/6J mice fixed for 2 hours into immobilization tube after CG, AL, CG+AL oral administration after 2 hours daily for 21 days. After every experiment has ended the C57BL/6J mice were sacrificed on 22 days. The production of Serotonin and Cortisol, lgA were observed by ELISA method, The proportion of immune cells such as T/B cell and macrophage, NK cell were measured by FACS. Then, Real-time PCR was performed to measure the mRNA expression of Inflammatory cytokines(IL-1beta, IL-6, TNF-a) and T cell activation cytokines(IL-2, IL-10, IFN-gamma, IL-12p35 / p40). Result : When chronic immobilization-stress mouse model were treated with CG+AL(1:4), the expression of mRNA were significantly decreased at the Inflammatory cytokines(IL-1beta, IL-6, TNF-a). While, the levels of mRNA were significantly increased at immune T cell activation cytokines. Additionally, CG+AL(1:4) combinational prescription group enhanced immune cells such as T/B cell and macrophage, NK cell. Furthermore, the Immuno-fluorescence result of brain tissue can confirm that CG+AL(1:4) group significantly increased the BDNF expression. Conclusion : These result suggest that CG+AL(1:4) combinational prescription has Immune System enhancement via stress-mediated immunocyte.

Rapid Screening of Naturally Occurring Radioactive Nuclides (238U, 232Th) in Raw Materials and By-Products Samples Using XRF

  • Park, Ji-Young;Lim, Jong-Myoung;Ji, Young-Yong;Lim, Chung-Sup;Jang, Byung-Uck;Chung, Kun Ho;Lee, Wanno;Kang, Mun-Ja
    • Journal of Radiation Protection and Research
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    • v.41 no.4
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    • pp.359-367
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    • 2016
  • Background: As new legislation has come into force implementing radiation safety management for the use of naturally occurring radioactive materials (NORM), it is necessary to establish a rapid and accurate measurement technique. Measurement of $^{238}U$ and $^{232}Th$ using conventional methods encounter the most significant difficulties for pretreatment (e.g., purification, speciation, and dilution/enrichment) or require time-consuming processes. Therefore, in this study, the applicability of ED-XRF as a non-destructive and rapid screening method was validated for raw materials and by-product samples. Materials and Methods: A series of experiments was conducted to test the applicability for rapid screening of XRF measurement to determine activity of $^{238}U$ and $^{232}Th$ based on certified reference materials (e.g., soil, rock, phosphorus rock, bauxite, zircon, and coal ash) and NORM samples commercially used in Korea. Statistical methods were used to compare the analytical results of ED-XRF to those of certified values of certified reference materials (CRM) and inductively coupled plasma mass spectrometry (ICP-MS). Results and Discussion: Results of the XRF measurement for $^{238}U$ and $^{232}Th$ showed under 20% relative error and standard deviation. The results of the U-test were statistically significant except for the case of U in coal fly ash samples. In addition, analytical results of $^{238}U$ and $^{232}Th$ in the raw material and by-product samples using XRF and the analytical results of those using ICP-MS ($R^2{\geq}0.95$) were consistent with each other. Thus, the analytical results rapidly derived using ED-XRF were fairly reliable. Conclusion: Based on the validation results, it can be concluded that the ED-XRF analysis may be applied to rapid screening of radioactivities ($^{238}U$ and $^{232}Th$) in NORM samples.

Alteration of Endogenous Growth Substances in Cold-moist Stratified Seeds of Ginkgo biloba L. (냉습적(冷濕積)에 따른 은행나무종자내(種子內) 생장조정물질(生長調整物質)의 변화(變化))

  • Lee, Kyong Jae;Yim, Kyong Bin
    • Journal of Korean Society of Forest Science
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    • v.38 no.1
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    • pp.1-12
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    • 1978
  • This study has intended to disclose the change of some chemical compositions of Ginkgo seeds which were acquired the treatment of cold-moist-stratification after collection. As check sample, the room-stored seeds were used. With the reasons that when the seeds not stratified were sown the delay of field germination has usually been resulted, the effectiveness of stratificaation in respect to alteration of chemical composition is to be investigated. The increase and decrease of growth promoting and inhibiting substances were investigated by means of chromatography method followed by rice seedling test or wheat coleoptile straight-growth test. The results obtained are summarized as follows; 1. In the untreated seeds, the zone of growth inhibitors on paper chromatograph were observed without regard to the tissue differences, embryo, endosperm and seedcoat. 2. Due to stratification, the amount of inhibitor has decreased in the embryo and seed coat, but growth promoters was decreased as compared with the check materials 3. The indications of results appear that each portion of the embryo, endosperm, and seedcoats of Ginkgo biloba L. contains the growth in hibitor taking part in germination dormancy. 4. It was presumed that hastening germination was influenced by decreasing of inhibitors in the embryo and seed coats rather than by increasing of promoters. 5. Gibberellin was detected at Rf 0.26 under the UV-lamp and the abscisic acid was detected at Rf 0.62, Rf 0.70, and Rf 0.78 and showed purple, gray, blue fluorescence respectively under the UV-lamp.

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Influence of Polycyclic Aromatic Hydrocarbons Formation in Sesame Oils with Different Roasting Conditions (참깨의 볶음 조건이 참기름 중 polycyclic aromatic hydrocarbons 생성에 미치는 영향)

  • Seo, Il-Won;Nam, He-Jung;Shin, Han-Seung
    • Korean Journal of Food Science and Technology
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    • v.41 no.4
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    • pp.355-361
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    • 2009
  • Polycyclic aromatic hydrocarbons (PAHs) are environmental carcinogenic compounds that arise by several means including food processing methods such as smoking and direct drying and cooking. This study examined the concentration of PAHs in sesame oils with various roasting temperatures (190, 220 and $250^{\circ}C$), methods (direct heating vs. indirect hot air heating), and times (5, 10, 15, 20 and 25 min). The PAHs in the sesame oils were analyzed using liquid-liquid extraction and solid-phase clean up (Florisil), followed by HPLC with fluorescence detection. According to the results, mean levels of total PAHs increased when the sesame oils were roasted at increasing temperatures and times. The sesame oil roasted at $250^{\circ}C$ for 25 min had the highest mean value of total PAHs (4.66 ${\mu}g$/kg). The results of this study suggest that the indirect hot air roasting method decreased PAH formation during sesame oil processing.

Studies on the Optical and the Electrical Characterization of Organic Electroluminescence Devices of Europium Complex Fabricated with PVD(Physical Vopor Deposition) Technique (진공 증착법에 의하여 제작한 Europium complex 유기 박막 전기발광소자의 광학적.전기적 특성에 관한 연구.)

  • Lee, Myeong-Ho;Lee, Han-Seong;Kim, Yeong-Gwan;Kim, Jeong-Su
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.48 no.5
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    • pp.285-295
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    • 1999
  • Electroluminescent(EL) devices based on organic materials have been of great interest due to their possible applications for large-area flat-panel displays. They are attractive because of their capability of multi-color emission, and low operation voltage. An approach to realize such device characteristics is to use active layers of lanthanide complexes with their inherent extremely sharp emission bands in stead of commonly known organic dyes. In general, organic molecular compounds show emission due to their $\pi$-$\pi*$ transitions resulting in luminescence bandwidths of about 80 to 100nm. Spin statistic estimations lead to an internal quantum efficiency of dye-based EL devices limited to 25%. On the contrary, the fluorescence of lanthanide complexes is based on an intramolecular energy transfer from the triplet of the organic ligand to the 4f energy states of the ion. Therefore, theoretical internal quantum efficiency is principally not limited. In this study, Powders of TPD, $Eu(TTA)_3(phen) and AlQ_3$ in a boat were subsequently heated to their sublimation temperatures to obtain the growth rates of 0.2~0.3nm/s. Organic electrolumnescent devices(OELD) with a structure of $glass substrate/ITO/Eu(TTA)_3(phen)/AI, glass substrate/ITO/TPD/Eu(TTA)_3(phen)/AI and glass substrate/ITO/TPD/Eu(TTA)_3(phen)/AIQ_3AI$ structures were fabricated by vacuum evaporation method, where aromatic diamine(TPD) was used as a hole transporting material, $Eu(TTA)_3(phen)$ as an emitting material, and Tris(8-hydroxyquinoline)Aluminum$(AlQ_3)$ as an electron transporting layer. Electroluminescent(EL) and current density-voltage(J-V) characteristics of these OELDs with various thickness of $Eu(TTA)_3(phen)$ layer were investigated. The triple-layer structure devices show the red EL spectrum at the wavelength of 613nm, which is almost the same as the photoluminescent(PL) spectrum of $Eu(TTA)_3(phen)$.It was found from the J-V characteristics of these devices that the current density is not dependent on the applied field, but on the electric field.

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