• Title/Summary/Keyword: liquid column

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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.

Studies on the Composition of Protein and Lipid from Korean Walnut (Juglans regia L.) (한국산 호도의 단백질 및 지질의 조성에 관한 연구)

  • Choi, Cheong;Sung, Tae-Soo;Cha, Woen-Suep;Son, Cyu-Mok
    • Applied Biological Chemistry
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    • v.29 no.3
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    • pp.318-323
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    • 1986
  • We empolyed gel filtraction, polyacrylamide gel electrophoresis, amino acid autoanalyzer, thin layer chromatography for determining protein and lipid composition in walnut. The walnut contained 22.18% of crude protein and 64.23% of crude lipid. Glutamic acid (38.60%) was the major amino acid in soluble protein, followed by arginine and aspartic acid. The sodium dodecyl sulfate polyacrylamide gel electrophoresis analysis showed 12 band in soluble protein of walnut, and collection rate of main protein fraction purified by Sephadex G-150 was 60.67%. The molecular weight for the main protein was estimated to be 43,000. The lipid fraction obtained by silicic acid column chromatography were mainly composed of about 93.05% neutral lipid, whereas compound lipid was only 7.0% level. Among the neutral lipid by thin layer chromatography, triglyceride was 82.05%, sterol ester and free fatty acid were 3.86% and 4.80%, repectively. The predominant fatty acids of total and neutral lipids were linoleic acid $(64.48{\sim}69.98%)$ and oleic acid $(13.89{\sim}15.36%)$. The major fatty acids of triglyceride separated from neutral lipid were linolenic acid (69.98%).

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Utilization of [6]-gingerol as an origin discriminant marker influencing melanin inhibitory activity relative to its content in Pinellia ternata (반하(Pinellia ternata)에서의 [6]-gingerol 함량과 멜라닌 저해 활성에 영향을 미치는 원산지 판별 마커로의 활용)

  • An, Ju Hyeon;Won, Hyo Jun;Seo, Soo-Kyung;Kim, Doo-Young;Ku, Chang-Sub;Oh, Sei-Ryang;Ryu, Hyung Won
    • Journal of Applied Biological Chemistry
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    • v.59 no.4
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    • pp.323-330
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    • 2016
  • Pinellia ternata Breitenbach, the natural medicinal plant of the Araceae family, is a perennial plant originated from the East Asia, but also widely distributed in Europe and North America. Its tuber is used as traditional medicine for treatment of various diseases such as vomiting, inflammation, and traumatic injury. Pharmacological studies revealed that P. ternata possesses anticonvulsant, anti-tumor, insecticidal, and cytotoxic activities. Despite being well-known as the useful medicinal plant, there is no reliable, standardized method for origin discrimination. Ultra performance liquid chromatography-photodiode array detector and quadrupole time of flight-mass spectrometry based metabolite-profiling was applied to explore significant metabolite for origin discrimination between Korean and Chinese P. ternata. One compound was isolated from Korean P. ternata using repeated ODS column chromatography by bioactivity guided fractionation, and determined as [6]-gingerol according to the results of spectroscopic data including nuclear magnetic resonance and MS. This compound was selected as cosmeceutical biomarker by fingerprints, and it was associated to melanin inhibitory effect determining its origin authenticity. Furthermore, the calibration curve of biomarker was prepared using validated method for the comparison of content between Korean and Chinese P. ternata. This is the report to address the selection and successful validation of the discriminant metabolite for confirmation of Korean P. ternata.

A Study on the Lipid Components in Oyster Mushroom (느타리버섯의 지방성분(脂肪成分)에 관한 연구(硏究))

  • Kwon, Yong-Ju;Uhm, Tai-Boong
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.13 no.2
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    • pp.175-180
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    • 1984
  • Lipids in oyster mushroom (Pleurotus florida) were extracted by the mixture of chloroform-methanol (2: 1, v/v) and fractionated into neutral lipids, glycolipids and phospholipids by silicic acid column chromatography. Components and fatty acid composition of each fraction were deter- mined by thin-layer and gas-liquid chromatographies. Fresh oyster mushroom contained 0.5% total lipid in which the contents if neutral lipids, glycolipids and phospholipids were 33.8%, 19.7% and 45. 6%, respectively, Triglycerides(38.2%), free fatty acids (20%) and free sterol (10%) were the major components among the neutral lipids. Diglycerides, monoglycerides, sterol esters and three unidentified neutral lipids were the minor components. Major components of glycolipids were steryl glycosides(35.9%) and esterified steryl glycosides (23.7%). Digalactosyl diglycerides, mono-galactosyl diglycerides and two unknown components were also present. Of the phospholipids, phosphatidyl cholines and serines (48.2%), and phosphatidyl ethanolamines(44.4%) were the major components. On the other hand, the major fatty acids of neutral lipids we.e linoleic, palmitoleic, oleic and palmitic acid. Linoleic and palmitic acid were the predominant fatty acids of both glycolipids and phospholipids.

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Distribution and Migration Characteristics of Explosive Compounds in Soil at Military Shooting Ranges in Gyeonggi Province (경기도 북부지역 군용 사격장 토양에 존재하는 화약물질 분포 및 이동 특성 조사)

  • Bae, Bumhan;Park, Jieun
    • Journal of the Korean GEO-environmental Society
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    • v.15 no.6
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    • pp.17-29
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    • 2014
  • A remedial investigation was conducted at five military training ranges in northern Gyeonggi province to collect information necessary for the design of on-site treatment facilities for the abatement of explosive compounds release to the environment. These information includes (i) identification of dominant explosive compounds in each range, (ii) discharge/migration routes, and (iii) contaminant distribution in particle size fraction and settling velocity of the soils. The results of investigation showed that TNT and RDX are the major contaminants but the extent of contamination varied depending on the types of military training practices and topography of the site. RDX was also detected in the subsurface soil and in the nearby stream within the training ranges, suggesting release of contaminants to streams. The median concentrations of explosives in the surface soil were less than 20 mg/kg despite several 'hot spots' in which explosives concentrations often exceeds several hundred mg/kg. The average clay contents in the soil of target area was less than 5 % compared to 12 % in the control, indicating loss of smaller particles by surface runoff during rainfall due to lack of vegetative land cover. Analysis of explosive compounds and particle size distribution showed that the amount of explosive compounds in soil particles smaller than 0.075 mm was less than 10 % of the total. Settling column tests also revealed that the quantity of explosive compounds in the liquid phase of the effluent was greater than that in the solid phase. Therefore, pre-treatment of particulate matter in surface runoff of shooting range with a simple settling basin and subsequent effluent treatment with planted constructed wetlands as polishing stage for explosives in the aqueous phase would provide the shooting ranges with a self-standing, sustainable, green solution.

Studies on the Lipid and Fatty Acid Compositions of Ark-Shell, Anadara broughtonii (피조개 지질 및 지방산 조성에 관한 연구)

  • 문숙임
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.21 no.4
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    • pp.436-442
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    • 1992
  • The present study was designed to analyze the lipid and fatty acid compositions of ark shell, Anadara broughtonii. The crude lipid was extracted by Bligh and Dyer's method, and then fractionated by TLC and quantitatively analyzed by TLC scanner. Lipid extracted from ark shell was fractionated into neutral and polar lipid by column chromatography with silicic acid. The fatty acid composition of lipid fractions were determined by gas liquid chromatography. Total lipid content of ark shell was 0.83% base on wet weight. The content of unsaponifiable matter was 20.19%, and iodine value was 156.13. The main components of total lipids were triglyceride, diglyceride, hydrocarbon, and sterol ester. The fatty acid composition of total lipid chiefly consisted of $C_{17 : 0}$, $C_{16 : 0}$, $C_{18 : 1}$ and $CT_{16 : 1}$. The main fatty acids of neutral lipid were $C_{16 : 0}$, $C_{18 : 1}$, $C_{22 : 1}$, $C_{18 : 0}$ and $C_{16 : 1}$. The major fatty acids of polar lipid were $C_{16 : 0}$, $C_{18 : 2}$, $C_{20 : 5}$ and $C_{22 : 6}$. In total lipid fractionation, saturated acid contents were high in all (SA>MA> PA), in neutral lipid fractionation, menoenoic acid contents were high in all (MA > SA> PA), and in polar lipid fractionation, saturated acid con-tents were high in all (SA> PA> MA).

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Absorption Characteristics of Carbon Dioxide by Water-lean Diethylenetriamine Absorbents Mixed with Physical Solvents (물리 흡수제를 포함한 디에틸렌트리아민(Diethylenetriamine) 저수계 흡수제에서의 이산화탄소 흡수 특성)

  • Lee, Hwa Young;Seok, Chang Hwan;You, Jong-Kyun;Hong, Yeon Ki
    • Clean Technology
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    • v.24 no.1
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    • pp.50-54
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    • 2018
  • In this work, N-methyl-2-pyrrolidone (NMP) was added into diethylenetriamine (DETA) aqueous solution for high $CO_2$ loading via phase splitting of absorbents during $CO_2$ absorption. Immiscible two phases were formed in the range of more than 30 wt% of NMP in 2 M DETA + NMP + water absorbents because of low solubility of DETA-carbamate in NMP solution. As the composition of NMP in the absorbents increased, the difference of $CO_2$ loading between each phase increased and the volume of bottom phase decreased. In $CO_2$ absorption in packed column by 2 M DETA + NMP + water absorbents, the absorption rate decreased in the range of more than 40 wt% of NMP. It is due to the increasing of mass transfer resistance in liquid film of absorbents at the high concentration of NMP. DETA + NMP + water absorbent is expected as the promising one for reducing the regeneration energy of absorbents according to volume reduction of $CO_2-rich$ phase.

A Study of Liquid Chromatographic Detection Method for Thiocarbamates by Using Photochemical Reaction (광화학 반응을 이용한 티오카바메이트류의 액체 크로마토그래피 검출법에 관한 연구)

  • Dai Woon Lee;Young Hun Park;Yong Wook Choi
    • Journal of the Korean Chemical Society
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    • v.37 no.4
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    • pp.453-461
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    • 1993
  • Detection method was developed using a simply designed photochemical reactor made of teflon coil and low pressure mercury lamp. This method of UV photolysis of analytes followed by UV, fluorescence and electrochemical detection was found to be useful for four thiocarbamates. Analytes eluting from the column are irradiated with a high flux of 254 nm UV light, so that they change to either fluorescent active forms or highly electrochemically sensitive products. Appling this technique to the UV detection, thiocarbamates were converted into long wavelength absorbing products upon UV irradiation. In fluorescence detector four thiocarbamates are not detected at nonirradiated condition but fluorescence signals of MPTC, CPTC photolysates are appeared after irradiation with UV light. The electrochemical detection for the determination of thiocarbamates was enhanced up to 5∼20 fold signal after UV irradiation, compared to that of the nonirradiated. The detection limit of thiocarbamates on electrochemical detector was 13.3∼0.02 ng under pH 7.0, ionic strength $0.5{\times}10^{-2}$ M, phosphate buffer solution. Adducts produced by reaction of photolysates and OPA-MERC in the reaction coil were monitored at 425 nm with fluorescence detector, and one of the photolysates was primary amine.

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Antioxidative Constituents from Fruit of Sorbaria sorbifolia var. stellipila MAX. (쉬땅나무(Sorbaria sorbifolia var. stellipila MAX.) 열매의 항산화 활성 성분)

  • Park, Jong-Hyuk;Kwon, Jin-A;Yang, Yoon-Jung;Han, Hyo-Sang;Han, Min-Woo;Lee, Young-Il;Kim, In-Su;Lee, Jong-Ill;Kang, Se-Chan
    • Korean Journal of Plant Resources
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    • v.24 no.4
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    • pp.337-342
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    • 2011
  • The purpose of this study was to evaluated the antioxidative constituents and their activities of the 80% methanolic extracts from fruit of Sorbaria sorbifolia var. stellipila MAX. The isolation of active compound was performed in three steps: solvent partition, open column chromatography, and high-performance liquid chromatography (HPLC). The solvent fractions were tested for their antioxidant activities by oxygen radical absorbance capacity (ORAC). The antioxidant activity of 80% methanolic extracts by various solvent partitions was in the order of 80% MeOH (1.68 ${\pm}$ 0.027), n-hexane (1.02 ${\pm}$ 0.036), $CH_2Cl_2$ (0.95 ${\pm}$ 0.025), EtOAc (1.98 ${\pm}$ 0.065), n-BuOH (1.94 ${\pm}$ 0.054) and Water (1.28 ${\pm}$ 0.032). Therefore, the results indicated that the potential antioxidant activities and functional values were observed significantly at EtOAc fraction from fruit of S. sorbifolia, flavonoid compound isolated.

Determination of 10${\alpha}$-Methoxy-9,10-dihydrolysergol (MDL), Main Metabolite of Nicergoline, in Human Plasma by HPLC-MS and Applicability to Oral Bioavailability in Korean Healthy Male Volunteers (HPLC-MS를 이용한 생체시료 중 니세르골린의 주대사체인 10${\alpha}$-Methoxy-9,10-dihydrolysergol(MDL)의 분석 및 이를 이용한 한국인 성인 남성에 대한 생체이용률 응용)

  • Lim, Hyon-Kyun;Yoo, Sun-Dong;Kim, Kyeong-Ho;Han, Sang-Beom;Youm, Jeong-Rok
    • YAKHAK HOEJI
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    • v.51 no.2
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    • pp.133-139
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    • 2007
  • A simple and sensitive HPLC-MS method for quantitation of 10${\alpha}$-methoxy-9,10-dihydrolysergol (MDL), the main metabolite of nicergoline, in human plasma was developed and the bioavailability parameters of MDL was assessed in Korean healthy male volunteers. Clomipramine was used as an internal standard. MDL and internal standard in plasma sample were extracted using ethyl acetate. A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 10 mM ammonium acetate-acetonitrile (10 : 90, v/v). The reconstituted samples were injected into a Zorbax SB-C8 column (2.1${\times}$150 mm,5 ${\mu}$m) at a flow-rate of 0.3 ml/min. Using MS with selected ion monitoring (SIM) mode, MDL and clomipramine were detected without severe interference from human plasma matrix. MDL produced a protonated molecular ion ([M+H]$^+$) at m/z 287. Internal standard produced a protonated molecular ion ([M+H]$^+$) at m/z 315. A linear relationship for MDL was found in the range of 2.5${\sim}$100 ng/ml. The lower limit of quantitation (LLOQ) was 2.5 ng/ml with acceptable precision and accuracy. The intra- and inter-day validation for all coefficients of variation (R.S.D.%) were found less than 15%. Main pharmacokinetic parameters of 30 mg of nicergoline were revealed as follows: AUC$_t$ 321.1${\pm}$64.5 ng${\cdot}$hr/ml, C$_{max}$, 51.2${\pm}$25.3 ng/ml, T$_{max}$ 3.6${\pm}$1.5 hr, K$_{el}$ 0.12${\pm}$0.07 hr$^{-1}$ and t$_{1/2}$ 7.6${\pm}$3.4 hr. Inter subject variations and race differences were shown in comparison with the published data in the literature.