• 제목/요약/키워드: glacial acid

검색결과 42건 처리시간 0.024초

사람 혈장 중 부메타니드의 HPLC 분석법 검증 및 단일 용량 투여에 의한 약물동태 연구 (Determination of Bumetanide in Human Plasma by a Validated HPLC Method and Its Application to Single-dose Pharmacokinetics)

  • 박혜영;곽혜선;전인구
    • Journal of Pharmaceutical Investigation
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    • 제35권1호
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    • pp.51-55
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    • 2005
  • A high-performance liquid chromatographic method was employed for the determination of bumetanide in human plasma. After addition of internal standard (IS, naproxen) and acidification of the plasma with 1 M hydrochloric acid, the drug and IS were extracted into dichloromethane. The organic phase was back-extracted into 1 M sodium bicarbonate solution and 50 ${\mu}l$ of the aqueous phase was injected onto a reversed-phase C18 column with a mobile phase consisting of methanol: water: glacial acetic acid = 65 : 35 : 1. The samples were detected utilizing a fluorescence detector (excitation wavelength 235 nm, emission wavelength 405 nm). The method was specific and validated with a lower limit of 5 ng/mL. Intra- and inter-day precision and accuracy were acceptable for all quality control samples including the lower limit of quantification. The applicability of the method was demonstrated by analysis of plasma after oral administration of a single 2 mg dose to 24 healthy subjects. From the plasma bumetanide concentration vs. time curves, the mean AUC was $246.5{\pm}73.8\;ng{\cdot}hr/mL$ and $C_{max}$ of $132.1{\pm}40.9$ ng/mL reached 1.2 hr after administration. The mean biological half-life of burnet ani de was $1.1{\pm}0.2$hr. Based on the results, this simple and validated assay method could readily be used in any pharmacokinetic or bioequivalence studies using humans.

HPLC Determination of Tolperisone in Human Plasma

  • Bae Jung-Woo;Park Young-Seo;Sohn Uy-Dong;Myung Chang-Sun;Ryu Byung-Kwon;Jang Choon-Gon;Lee Seok-Yong
    • Archives of Pharmacal Research
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    • 제29권4호
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    • pp.339-342
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    • 2006
  • A simple high performance liquid chromatographic (HPLC) method was developed for the determination of tolperisone in human plasma. Tolperisone and internal standard (chlorphenesin) were isolated from 1 mL of plasma using 8 mL of dichlormethane. The organic phase was collected and evaporated under nitrogen gas. The residue was then reconstituted with 300 mL aliquot of mobile phase and a 100 mL aliquot was injected onto the $C_{18}$ reverse-phased column. The mobile phase, $45\%$ methanol containing $1\%$ glacial acetic acid and $0.05\%$ 1-hexanesulfonic acid was run at a flow rate of 1 mL/min. The column effluent was monitored using UV detector at 260 nm. The retention times for tolperisone and the internal standard were approximately 7.1 and 8.4 min, respectively. The standard curve was linear with minimal intra-day and inter-day variability. The quantification limit of tolperisone in human plasma was 10 ng/ mL. The proposed method has been applied to the determination of pharmacokinetic profile of tolperisone in Koreans. The T max of tolperisone in Koreans $(0.94{\pm}0.42\;h)$ was not significantly differ from that reported in Europeans (0.5-1 h), but the mean half-life in Koreans $(1.14{\pm}0.27\;h)$ was shorter than that in Europeans $(2.56{\pm}0.2\;h)$. The proposed HPLC method is simple, accurate, reproducible and suitable for pharmacokinetic study of tolperisone.

Quantification of Karanjin, Tannin and Trypsin Inhibitors in Raw and Detoxified Expeller and Solvent Extracted Karanj (Pongamia glabra) Cake

  • Panda, A.K.;Sastry, V.R.B.;Kumar, A.;Saha, S.K.
    • Asian-Australasian Journal of Animal Sciences
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    • 제19권12호
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    • pp.1776-1783
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    • 2006
  • Despite being a rich source of protein (28-34%), karanj (Pongamia glabra) cake is found to be bitter in taste and toxic in nature owing to the presence of flavonoid (karanjin), tannin and trypsin inhibitor, thereby restricting its safe inclusion in poultry rations. Feeding of karanj cake at higher levels (>10%) adversely affected the growth performance of poultry due to the presence of these toxic factors. Therefore, efforts were made to detoxify karanj cake by various physico-chemical methods such as dry heat, water washing, pressure cooking, alkali and acid treatments and microbiological treatment with Sacchraromyces cerevisiae (strain S-49). The level of residual karanjin in raw and variously processed cake was quantified by high performance liquid chromatography and tannin and trypsin inhibitor was quantified by titrametric and colorimetric methods, respectively. The karanjin, tannin and trypsin inhibitor levels in such solvent and expeller pressed karanj cake were 0.132, 3.766 and 6.550 and 0.324, 3.172 and 8.513%, respectively. Pressure-cooking of solvent extracted karanj cake (SKC) substantially reduced the karanjin content at a cake:water ratio of 1:0.5 with 30-minute cooking. Among chemical methods, 1.5% (w/w) NaOH was very effective in reducing the karanjin content. $Ca(OH)_2$ treatment was also equally effective in karanjin reduction, but at a higher concentration of 3.0% (w/w). A similar trend was noticed with respect to treatment of expeller pressed karanj cake (EKC). Pressure cooking of EKC was effective in reducing the karanjin level of the cake. Among chemical methods alkali treatment [2% (w/w) NaOH] substantially reduced the karanjin levels of the cake. Other methods such as water washing, dry heat, HCl, glacial acetic acid, urea-ammoniation, combined acid and alkali, and microbiological treatments marginally reduced the karanjin concentration of SKC and EKC. Treatment of both SKC and EKC with 1.5% and 2.0% NaOH (w/w) was the most effective method in reducing the tannin content. Among the various methods of detoxification, dry heat, pressure cooking and microbiological treatment with Saccharomyces cerevisiae were substantially effective in reducing the trypsin inhibitor activity in both SKC and EKC. Based on reduction in karanjin, in addition to tannin and trypsin inhibitor activity, detoxification of SKC with either 1.5% NaOH or 3% $Ca(OH)_2$, w/w) and with 2% NaOH were more effective. Despite the effectiveness of pressure cooking in reducing the karanjin content, it could not be recommended for detoxification because of the practical difficulties in adopting the technology as well as for economic considerations.

Cytotoxic Effect and Constituent Profile of Alkaloid Fractions from Ethanolic Extract of Ficus septica Burm. f. Leaves on T47D Breast Cancer Cells

  • Nugroho, Agung Endro;Akbar, Fiki Fatihah;Wiyani, Anggie;Sudarsono, Sudarsono
    • Asian Pacific Journal of Cancer Prevention
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    • 제16권16호
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    • pp.7337-7342
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    • 2015
  • The study aimed to investigate the profile of alkaloids in two ethyl acetate soluble fractions, namely fractions A and B from an ethanolic extract of Ficus septica leaves and cytotoxic effect on T47D breast cancer cells. Preparation of both fractions involved maceration of leaves with 70% (v/v) ethanol, filtration with $Al_2O_3$, precipitation with 0.1 N HCl, Mayer reagent, and 0.1 N NaOH, and also partition with ethyl acetate. Qualitative thin layer chromatography (TLC) was conducted to determine the profile of alkaloids in the two fractions, using alkaloid specific reagents such as Dragendorff, sodium nitrite, and Van Urk-Salkowski. Cytotoxic effects of both fractions on T47D cells were evaluated using MTT assay with a concentration series of 1.56; 3.12; 6.25; 12.5; 25 and $50{\mu}g/mL$. The TLC test showed that fractions A and B contained alkaloids with Rx values of 0.74 and 0.80 for fraction A and 0.74, 0.84, 0.92 for fraction B with regard to yohimbine using the mobile phase of n-buthanol:glacial acetic acid:distilled water (3:1:1 v/v/v). Moreover, an indole alkaloid was detected with Rx values of 0.80 and 0.84, respectively. Fractions A and B exhibited high cytotoxic effects on T47D cells with IC50 values of 2.57 and $2.73{\mu}g/mL$, respectively. In conclusion, overall the results of this study showed that fractions of Ficus septica contain alkaloids including indole alkaloid or its derivatives and possess a cytotoxic effect on T47D cells. This research supports the idea that alkaloids in F. septica have anticancer activity.

종격동경을 이용한 식도절제수술 -1례- (Esophagectomy with Operating Mediastinoscope)

  • 윤용한;이두연;이성수
    • Journal of Chest Surgery
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    • 제31권11호
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    • pp.1110-1115
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    • 1998
  • 식도절제와 식도와 위의 문합 혹은 식도와 대장의 문합등의 수술은 통상적으로 식도절제를 위한 개흉절개와, 식도 및 주위 림프절 절제, 광범위한 개복수술과 위 혹은 대장의 박리 등을 포함하고 있다. 또한 박리된 위 혹은 대장은 경부절개후 경부식도에 문합하게 된다. 1978년 Orringer 와 Sloan 등이 개흉술을 하지 않고 식도절제술을 최초로 시행한 이래 흉강내시경과 종격동경등을 이용한 여러 가지 수술방법이 개발되었다. 반면에 종격동 내시경을 이용한 식도박리(endoscopic microsurgical dissection of the oesophagus : EMDO) 1989년 이들 수술수기 개발자인 Buess, Kimfmuller, Naruhn과 Melzer 등에 의해 EMDO로 명명되었으며 Buess와 Becker에 의해서 임상에 응용되었다. 본 증례는 150cc의 빙초산을 먹은 후 식동협착(esophageal striture) 로 진단 받은 20세된 여자환자에서 종격동경(Operating Mediastinoscope)을 이용하여 식도를 박리 하면서 동시에 위와 식도를 문합할수 있게 박리하고 GIA 90을 이용하여 위문부와 식도부위를 절제한 후 점막이 보존되어있는 상부식도 부위에서 식도를 절제하고 위를 1이용하여 경부에서 식도와 위를 문합하였다. 수술 후 특이한 합병증 없이 수술 후 17일째 퇴원하였으며 현재 별다른 문제없이 외래 추적관찰중이다.

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Sol-gel 방법에 의한 $LaAlO_3$ 박막의 제조 (Preparation of $LaAlO_3$ thin Films by Sol-gel Method)

  • 김혜진;김병주;이희균;홍계원
    • Progress in Superconductivity
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    • 제9권1호
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    • pp.85-90
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    • 2007
  • Lanthanum aluminate($LaAlO_3$) film has been prepared on single crystal and metal substrates by dip coating method. Lanthanum acetate and aluminum were prepared via ligand exchange starting from lanthanum nitrate hexahydrate and aluminum nitrate hexahydrate in acetate glacial acetic acid solution after being refluxed. Coating solution was obtained by diluting the gel with methanol and 2-methoxyethanol to adjust the total cation concentration to 0.67 M. Precursor coated film was prepared by dip-coating with a speed of 25 mm/min on various substrates such as $LaAlO_3$ (001), MgO(001), $SrTiO_3$(001) single crystal, LMO/MgO/Ni-alloy. Thin films have been obtained by heat treating the precursor film at various temperatures from $600^{\circ}C{\sim}900^{\circ}C$ and various heating rate from $0.83^{\circ}C/min{\sim}1.25^{\circ}C/min$ under $Ar/O_2$ mixture containing 1000ppm oxygen. The films have been characterized by scanning electronic microscopy (SEM) and X-ray diffraction (XRD). XRD analysis for the prepared film showed that $LaAlO_3$ thin films with a preferred orientation of (100) plane parallel to substrate surface were obtained at $800^{\circ}C(1.11\;^{\circ}C/min)$ on LMO/MgO/Ni-alloy substrate, but the intensity decreased with the increase of heat treatment temperature.

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견직물의 초란각액 처리 조건에 따른 연구(I) - 물성 및 태 변화를 중심으로 - (Development of Eco-friendly Textiles by Studying the effect of the Natural Chorangak Liquid Treatment of Silk Fabrics - Focusing on the Mechanical Properties & the Hand -)

  • 이정주;김기연
    • 한국생활과학회지
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    • 제22권1호
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    • pp.131-140
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    • 2013
  • Eco-friendly and health-functional clothing is now becoming the target of the worldwide hot trends. The purpose of this study is to develop an eco-friendly textiles to decrease environmental pollution and to be harmless for human health by investigating how the natural chorangak liquid treatment affects the changes of mechanical properties and the hand of silk fabrics according to different treatment conditions. Treatment was varied with various temperatures ($85^{\circ}C$, $90^{\circ}C$, $95^{\circ}C$) for 90 seconds after degumming. The results were as follows: 1) The natural chorangak liquid is the most effective at the ratio of glacial acid 200ml with eggshell 20g minimizing the time limit and sludge reduction. Its treatment of silk fabrics is optimized at $90^{\circ}C$ for 90 seconds with 25% conc. after degumming when considering tenacity and elongation. 2) After the treatment, tenacity and elongation of specimen are increased compared with those of degummed silk fabrics. 3) After analyzing the effect of the treatment on the characteristic values of basic mechanical properties of silk fabrics, mechanical properties (tensile, bending, shearing, compression, surface) are overall improved. The properties of thickness and weight are increased as well. 4) Based on the clear analysis on effects of the treatment on the mechanical properties and the hand of silk fabrics, the level of THV was enhanced from good to excellent. Therefore, chorangak liquid can be utilized satisfactorily as a new finishing agent for developing eco-friendly textiles.

Genomic DNA Extracted from Ancient Antarctic Glacier Ice for Molecular Analyses on the Indigenous Microbial Communities

  • Lee, Sang-Hoon;Bidle, Kay;Falkowski, Paul;Marchant, David
    • Ocean and Polar Research
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    • 제27권2호
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    • pp.205-214
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    • 2005
  • From ancient Antarctic glacier ice, we extracted total genomic DNA that was suitable for prokaryotic 16S rDNA gene cloning and sequencing, and bacterial artificial chromosome (BAC) library and end-sequencing. The ice samples were from the Dry Valley region. Age dating by $^{40}Ar/^{39}Ar$ analysis on the volcanic ashes deposited in situ indicated the ice samples are minimum 100,000-300,000 yr (sample DLE) and 8 million years (sample EME) old. Further assay proved the ice survived freeze-thaw cycles or other re-working processes. EME, which was from a small lobe of the basal Taylor glacier, is the oldest known ice on Earth. Microorganisms, preserved frozen in glacier ice and isolated from the rest of the world over a geological time scale, can provide valuable data or insight for the diversity, distribution, survival strategy, and evolutionary relationships to the extant relatives. From the 16S gene cloning study, we detected no PCR amplicons with Archaea-specific primers, however we found many phylotypes belonging to Bacteria divisions, such as Actinobacteria, Acidobacteria, Proteobacteria $({\alpha},\;{\beta},\;and\;{\gamma})$, Firmicutes, and Cytophaga-Flavobacterium-Bacteroid$. BAC cloning and sequencing revealed protein codings highly identical to phenylacetic acid degradation protein paaA, chromosome segregation ATPases, or cold shock protein B of present day bacteria. Throughput sequencing of the BAC clones is underway. Viable and culturable cells were recovered from the DLE sample, and characterized by their 16S rDNA sequences. Further investigation on the survivorship and functional genes from the past should help unveil the evolution of life on Earth, or elsewhere, if any.

겔의 수열합성법에 의한 다공성 구형 $BaTiO_3$ 미분체의 제조 (Manufacture of $BaTiO_3$ Powders by Gel-hydrothermal Method)

  • 김용렬
    • 한국응용과학기술학회지
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    • 제22권4호
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    • pp.306-314
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    • 2005
  • In this study, spherical $pre-BaTiO_3$ particles are prepared by gelation and aging process in autoclave without catalysts. The (Ba-Ti) gel used as a starting material was prepared by aging mixtures of titanyl acylate with barium acetate aqueous solution([glacial acetic acid (AcOH)]/[titanium isopropoxide (TIP)] 4, [barium acetate]/[TIP] 1) at $45^{\circ}C$ for 48hrs. XRD and SEM results for the (Ba-Ti) gel sample at aging process showed that the gel was formed via aggregation of the fine particles. It seems to be the primary particles of bulk (Ba-Ti) gel amorphous, but the spatial arrangement of barium and titanium in the (Ba-Ti) gel is similar to that in crystalline $BaTiO_3$ particles. From XRD and FT-IR. spectroscopy analysis it was found that the crystal structure of the prepared particles continuously transformed from amorphous to tetragonal as the calcination temperature increased, and crystallized spherical cubic and tetragonal $BaTiO_3$ powder obtained at the very low calcination temperature between $500^{\circ}C$ and $900^{\circ}C$ after 1hrs of heat treatment respectively. According to BET analysis result, final particle have pore structure of ink bottle shape which is produced by aggregation of fine spherical particles with surface area of $280m^2/g$ and average pore size of 130nm.

Synthesis and Antitumor Evaluation of Acyclic 1-[${\omega}$-(N^I-2-chloroethyl-N^I-nitrosoureido)alkyl]thymidine Nucleoside Analogues

  • Kim, Jack-C.;Kim, Young-Hyun;Park, Jin-Il;Kim, Seon-Hee;Choi, Soon-Kyu
    • Archives of Pharmacal Research
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    • 제20권3호
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    • pp.259-263
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    • 1997
  • In the preparation of acyclic thymidine nucleoside analogues, $K_2CO_3$(or NaH) treated thymine in DMSO was alkylated with .omega.-chloroalkyl nitrite (Cl-(CH_2)n-CN; n=1, 2, 3, 4) to provide an isomeric mixture of 1-(${\omega}$-cyanoalkyl)thymine (2a-d) and 1,3-bis(${\omega}$-cyanoalkyl)thymine in approximately 5:1 ratios. Reduction of the cyano function 2a-d with $NaBH_{4}/CoCl_{2}$ center dot$ 6H_{2}O$gave the corresponding 1-(${\omega}$aminoalkyl)thymine (3a-d). The newly formed primary amino function in 3a-d was directly reacted with 2-chloroethylisocyanate to afford the 1-[.omega.($N^{I}$-2-chloroethylureido) alkyl]thymine (4a-d) in good yields. Nitrosation of 1-[5-($ N^{I}-2$-chloroethylureido)pentyl] thymine (4d) with glacial acetic acid and dry $NaNO_{2}$-powder in anhydrous $CH_{2}Cl_{2}$gave two types of regioisomeric nitrosoureas, 1-[5-($N^{I}$--chloroethyl-$N^{I}$--nitrosoureido)pentylithymine (5d) and 1-[5-($N^{I}-2$-chloroethyl-N-nitrosoureido)pentyllthymine in approximately 5 :1 ratios. The in vitro cytotoxicity of the synthesized compounds (2a-d, 3a-d, 4a-d and 5a-d) against three cell lines (K-562, P-388 and FM-3A) are measured as $IC^{50}$ values. Compounds 3b and 4c showed moderate activities against all three cell lines, and all other compounds were found to be not active.

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