• 제목/요약/키워드: Analytical Chromatography

검색결과 1,121건 처리시간 0.026초

Potential for Dependence on Lisdexamfetamine - In vivo and In vitro Aspects

  • Yun, Jaesuk;Lee, Kwang-Wook;Eom, Jang-Hyeon;Kim, Young-Hoon;Shin, Jisoon;Han, Kyoungmoon;Park, Hye-Kyung;Kim, Hyung Soo;Cha, Hye Jin
    • Biomolecules & Therapeutics
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    • 제25권6호
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    • pp.659-664
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    • 2017
  • Although lisdexamfetamine is used as a recreational drug, little research exists regarding its potential for dependence or its precise mechanisms of action. This study aims to evaluate the psychoactivity and dependence profile of lisdexamfetamine using conditioned place preference and self-administration paradigms in rodents. Additionally, biochemical techniques are used to assess alterations in the dopamine levels in striatal synaptosomes following administration of lisdexamfetamine. Lisdexamfetamine increased both conditioned place preference and self-administration. Moreover, after administration of the lisdexamfetamine, dopamine levels in the striatal synaptosomes were significantly increased. Although some modifications should be made to the analytical methods, performing high performance liquid chromatography studies on synaptosomes can aid in predicting dependence liability when studying new psychoactive substances in the future. Collectively, lisdexamfetamine has potential for dependence possible via dopaminergic pathway.

Isolation and Partial Characterization of Phytotoxic Mycotoxins Produced by Sclerotinia sp., a Potential Bioherbicide for the Control of White Clover(Trifoliorum repens)

  • Hong, Yeon-Kyu;Lee, Bong-Choon;Jung, Won-Kwon;Bae, Soon-Do;Park, Sung-Tae;Uhm, Jae-Youl
    • The Plant Pathology Journal
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    • 제20권1호
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    • pp.52-57
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    • 2004
  • Sclerotinia sp. (isolate BWC98-105) causes stem blight and root rot in Leghum sp., and is presently being evaluated as a potential mycoherbicide for the control of Trifoliorium repens. Bioassays have shown that Sclerotinia sp. produces phytotoxic substance which is biologically active against T. repens. Two biologically active compounds, designated as compoundsI and II, were produced in vitro from the culture filtrate of BWC98-105 isolate Sclerotium sp. Compounds I and II were purified by means of liquid-liquid extraction and $C_{18}$ open column chromatography (300 ${\times}$ 30 mm, i.d). To determine the purity, the purified compounds were analyzed by RP-HPLC. The analytical RP-HPLC column was a TOSOH ODS-120T (150 ${\times}$ 4.6 mm i.d, Japan), of which the flow rate was set at 0.7 mL/min using the linear gradient solvent system initiated with 15 % methanol to 85 % methanol for 50 min with monitoring at 254 nm. Under these RP-HPLC conditions, compounds I and II eluted at 3.49 and 4.13 min, respectively. Compound II was found to be most potent and host specific. However, compound I had a unique antibiotic activity against phytopathogenic bacteria like bacterial leaf blight (Xanthomonas oryzae) on rice, where it played a less important role in producing toxicity on T. repens. No toxin activity was detected in the water fraction after partitioning with several organic solvents. However, toxin activity was detected in the ethyl acetate and butanol fractions. In the leaf bioassay using compound II, the disease first appeared within 4-5 h as water soaked rot, which subsequently developed into well-defined blight affecting the whole plant.

속단(Dipsaci Radix) 중 Asperosaponins 및 Iridoid glycosides의 LC-ESI-MS에 의한 동시분석 (Simultaneous Determination of Asperosaponins and Iridoid Glycosides from Dipsaci Radix by Using LC-ESI-MS Spectrometry)

  • 조황의;손인섭;김선춘;손건호;우미희;문동철
    • 생약학회지
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    • 제43권2호
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    • pp.137-146
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    • 2012
  • Dipsaci Radix (Dipsacaceae) has been used as a tonic, an analgesic, anti-inflammatory and anti-complement agents in traditional herbal medicine for the therapy of low back pain, knee pain, rheumatic arthritis, traumatic hematoma, and bone fractures. A high-performance liquid chromatography-electrospray ionization-mass spectrometric method (HPLC-ESI-MS) was developed for the simultaneous quantitation method of the five compounds from the herbal drug: asperosaponin VI and asperosaponin XII (terpene glycosides), sweroside, loganin and dipsacus A(iridoid glycosides). HPLC separation of the analytes was achieved on a C18 column ($150{\times}2.0$ mm i.d., 5 ${\mu}m$) using the aqueous methanol containing 5 mM ammonium acetate with gradient flow of the mobile phase. Detection of the analytes was performed by positive ion electrospray ionization, and selected ion monitoring was used for data acquisition using m/z corresponding molecular adduct ion, $[M+NH_4]^+$ and $[M+H]^+$. Calibration graphs showed good linearity ($r^2$=0.9997) over the wide range of the analytes; intra- and inter-day precisions (RSD, %) were within 9.1% and the accuracy between 94.0-111.0%. Recoveries of the analytes through the assay procedure were in the range of 93.7-110.8%. Analytical results of the herbal drugs of Dipsaci Radix (17 samples) show wide distribution of the five marker compounds and clear difference of the species from Phlomidis Radix (4 samples). The developed method would provide a practical guide for the quality control of the herbal drug.

LC-ESI-MS/MS를 이용한 평위산 주요 성분의 함량 분석 (Quantitative Determination of the Marker Components in Pyungwi-San Using LC-ESI-MS/MS)

  • 서창섭;신현규
    • 생약학회지
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    • 제49권3호
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    • pp.270-277
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    • 2018
  • Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

Characterization and Application of a Novel Thermostable Glucoamylase Cloned from a Hyperthermophilic Archaeon Sulfolobus tokodaii

  • Njoroge, Rose Nyawira;Li, Dan;Park, Jong-Tae;Cha, Hyun-Ju;Kim, Mi-Sun;Kim, Jung-Wan;Park, Kwan-Hwa
    • Food Science and Biotechnology
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    • 제14권6호
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    • pp.860-865
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    • 2005
  • A gene for a putative glucoamylase, stg, of a hyperthermophilic archae on Sulfolobus tokodaii was cloned and expressed in Escherichia coli. The recombinant glucoamylase (STGA) had an optimal temperature of $80^{\circ}C$ and was extremely thermostable with a D-value of 17 hr. The pH optimum of the enzyme was 4.5. Being different from fungal glucoamylases, STGA hydrolyzed maltotriose (G3) most efficiently. Gel permeation chromatography and sedimentation equilibrium analytical ultracentrifugation analysis showed that the enzyme existed as a dimer. STGA was stable enough to hydrolyze liquefied com starch to glucose in 4 hr at $90^{\circ}C$ with a yield of95%. Comparison of the $k_{cat}$ values for the hydrolysis and the reverse reaction at $75^{\circ}C$ and $90^{\circ}C$ indicated that glucose production by STGA was more efficient at $90^{\circ}C$ than $75^{\circ}C$. Therefore, STGA showed great potential for application to the industrial glucose production process due to its high thermostability.

추출방법에 의한 아니스의 휘발성 성분 조성 비교 (A Comparison of Different Extraction Methods for the Volatile Components of Anise(Pimpinella anisum L.))

  • 권영주;장희진;곽재진;김옥찬;최영현;이재곤
    • Applied Biological Chemistry
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    • 제40권2호
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    • pp.144-147
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    • 1997
  • 식물체의 향기성분을 분리하는데 사용되는 몇가지 방법을 비교하기 위해서 headspace(purge & trap)법, simultaneous distillation extraction(SDE)법, steam distillation법, 용매추출법 등으로 분리된 휘발성 성분의 조성차이를 분석하여 각각의 사용된 방법들의 특징을 비교하였다. 휘발성 성분 분석시료로는 Anise(Pimpinella anisum L.)씨앗을 사용하였으며 분리된 휘발성분중 GC/MSD를 이용하여 43종의 성분을 확인하였다. Headspace (purge & trap)법에서는 휘발성이 강한 2-butanol, pentanal, 3-hexen-1-ol 등과 같은 alcohol류 및 aldehyde류 성분들을 주요성분으로 확인할 수 있었으며, 용매추출에서는 비점이 높은 성분들인 myristic acid, oleic acid 등의 acid류 성분들과 ethyl hexadecanoate, ethyl octadecanoate 등과 같은 ester 화합물들이 주요성분으로 확인되었다. SDE법과 steam distillation법에서 추출된 성분의 조성은 유사하였으며 terpene 화합물들이 주요성분으로 확인되었다. Anise의 주성분인 anethole은 SDE법, headspace(purge & trap)법으로 추출하였을때 가장 많이 추출되었다.

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HPLC-tandem Mass Spectrometric Analysis of the Marker Compounds in Forsythiae Fructus and Multivariate Analysis

  • Cho, Hwang-Eui;Ahn, Su-Youn;Son, In-Seop;Hwang, Gyung-Hwa;Kim, Sun-Chun;Woo, Mi-Hee;Lee, Seung-Ho;Son, Jong-Keun;Hong, Jin-Tae;Moon, Dong-Cheul
    • Natural Product Sciences
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    • 제17권2호
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    • pp.147-159
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    • 2011
  • A high-performance liquid chromatography-electrospray ionization-tandem mass spectrometric method was developed to determine simultaneously eight marker constituents of Forsythiae fructus, and subsequently applied it to classify its two botanical origins. The marker compounds of Forsythia suspensa were phillyrin, pinoresinol, phillygenin, lariciresinol and forsythiaside; those of F.viridissima were arctiin, arctigenin and matairesinol. Separation of the eight analytes was achieved on a phenyl-hexyl column (150${\times}$2.0 mm i.d., 3 ${\mu}M$) using gradient elution with the mobile phase: (A) 10% acetonitrile in 0.5% acetic acid, (B) 40% aqueous acetonitrile. A few fragment ions specific to the types of lignans, among the product ions generated by collisonally induced dissociation (CID) of molecular ion clusters, such as [M-H]$^-$ or [M+OAc]$^-$ were used not only for fingerprinting analysis but for the quantification of each epimer by using multiple-reaction monitoring mode. It was shown good linearity ($r^2{\geq}$ 0.9998) over the wide range of all analytes; intra- and inter-day precisions (RSD, %) were within 9.14% and the accuracy ranged from 84.3 to 115.1%. The analytical results of 40 drug samples, combined with multivariate statistical analyses - principal component analysis (PCA) and hierarchical cluster analysis (HCA) - clearly demonstrated the classification of the test samples according to their botanical origins. This method would provide a practical strategy for assessing the authenticity or quality of the herbal drug.

Solid SCR용 암모니아 저장물질인 Calcium Ammine Chloride의 합성방법 및 물질분석 연구 (A Study on Synthetic Method and Material Analysis of Calcium Ammine Chloride as Ammonia Transport Materials for Solid SCR)

  • 신종국;윤천석;김홍석
    • 한국자동차공학회논문집
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    • 제23권2호
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    • pp.199-207
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    • 2015
  • Solid materials of ammonia sources with SCR have been considered for the application of lean NOx reduction in automobile industry, to overcome complex problems of liquid urea based SCR. These solid materials produce ammonia gas directly with proper heating and can be packaged by compact size, because of high volumetric ammonia density. Among ammonium salts and metal ammine chlorides, calcium ammine chloride was focused on this paper due to low decomposition temperature. In order to make calcium ammine chloride in lab-scale, simple reactor and glove box was designed and built with ammonium gas tank, regulator, and sensors. Basic test conditions of charging ammonia gas to anhydrous calcium chloride are chosen from equilibrium vapor pressure by Van't Hoff plot based on thermodynamic properties of materials. Synthetic method of calcium ammine chloride were studied for different durations, temperatures, and pressures with proper ammonia gas charged, as a respect of ammonia gas adsorption rate(%) from simple weight calculations which were confirmed by IC. Also, lab-made calcium ammine chloride were analyzed by TGA and DSC to clarify decomposition step in the equations of chemical reaction. To understand material characteristics for lab-made calcium ammine chloride, DA, XRD and FT-IR analysis were performed with published data of literature. From analytical results, water content in lab-made calcium ammine chloride can be discovered and new test procedures of water removal were proposed.

한국전통간장의 맛과 향에 관여하는 주요 향미인자의 분석(III) -향기성분 분석 - (Analysis of Significant Factors in the Flayer of Traditional Korean Soy Sauce (III) - Aroma Compound Analysis -)

  • 박현경;손경희;박옥진
    • 한국식생활문화학회지
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    • 제12권2호
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    • pp.173-182
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    • 1997
  • This study was carried out in order to investigate effective aroma components of Korean traditional soy sauce. Volatile aroma compounds were extracted by solvent extraction, TMS esterification of methyl acetate extracts and SDE, and analyzed by GC/MSD. 140 voltile aroma compounds were detected by three different extraction methods. Most abundant volatile compounds were acids and phenols and identified aldehydes, hydrocarbons, ketones, furans, furanone, alcohols, esters, nitrogen compounds, sulfur compounds and thiazoles, too. In the analytical sensory evaluation of soy sauce aroma, there were significant differences between each soy sauce sample in all test item. To sum up, Sweet odor was high in Kyupjang. Nutty odor and traditional soy sauce odor were similarly high in Kyupjang and high concentration soy sauce. Kyupjang had high score in overall odor preference than Chungiangs. The result of multiple regression of soy sauce odor characteristics and gas chromatography pattern demonstrated that offensive and sour odor was affected by octadecanoic acid. Contributive compounds to sweet odor were 1,2-benzenedicarboxylic acid and 3,6-dioxa-2,7-disilacotane. Benzoic acid 4-methyl ethyl ester and nonacotane were identified as major compounds of nutty odor. Contribu live variables of traditional soy sauce odor were benzoic acid 4-methyl ethyl ester and 9,12-octadecadienoic acid. The main factors of odor preference were 3-methyl pentanoic acid, acetic acid, 2,6-dimethyl heptadecane and 3,6-dioxa-2,7-disilacotane.

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혼합폐플라스틱의 열분해로부터 생성된 고분자성분의 열적분해 (Thermal Degradation of High Molecular Components Obtained from Pyrolysis of Mixed Waste Plastics)

  • 오세천;류재훈;곽현;배성열;이경환
    • 공업화학
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    • 제19권2호
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    • pp.191-198
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    • 2008
  • 혼합폐플라스틱의 열분해로부터 얻어진 고분자성분의 열적분해 특성에 대한 연구를 TGA와 GC-MS를 이용하여 수행하였다. 열적분해의 속도론적 연구는 $10{\sim}50^{\circ}C/min$ 사이의 여러 가열속도에서 비등온 질량감소 기술을 이용하여 수행하였으며 활성화 에너지 및 반응차수 등과 같은 속도 상수들에 대한 정보를 얻기 위하여 문헌에 제시된 여러 가지의 속도론 해석 방법을 이용하여 질량감소 곡선 및 그 미분 값을 해석하였다. 또한 회분식 열분해 반응기를 이용하여 반응온도 및 반응시간에 따른 액상 생성물의 수율변화를 고찰하였으며 GC-MS를 이용하여 반응온도의 증가에 따른 액상 생성물의 특성연구를 수행하였다.