• 제목/요약/키워드: chromatography test

검색결과 737건 처리시간 0.033초

A study of test method for impurities(related compounds) in pharmaceutical products

  • Ko, Yong-Seok;Jang, Seung-Jae;Kang, Chan-Soon;Choi, Bo-Kyung;Kim, Hye-Soo;Kim, Eun-Jung;Cho, Myoeng-Sin;Hong, Chong-Hui;Kim, Sang-Hyun
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.280.1-280.1
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    • 2003
  • The high-performance liquid chromatography method was performed for test method development of related compounds in pharmaceuticals. Using reverse-phase column and gradient elution of 1 % acetonitrile-acetonitrile: H20:triethylamine (70:30:0.5), lansoprazole, 2-hydroxybenzimidazole, 2-mercaptobenzimidazole, lansoprazole sulfone, lansoprazole sulfide could be individually identified and quantitated. (omitted)

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Production of selenium peptide from yeast

  • 김영옥;김은기
    • 한국생물공학회:학술대회논문집
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    • 한국생물공학회 2002년도 생물공학의 동향 (X)
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    • pp.208-210
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    • 2002
  • Baker's yeast was cultured with $Na_2SeO_3$. Selenium compounds in yeast were extracted and analyzed by size exclusion chromatography. Selenium was broadly distributed in the fraction of protein. For the inhibition test of MMP-l induction, selenium containing compounds was fractioned by ultrafiltration

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HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법 (Simultaneous analysis of sulfonamides in beef and pork by high performance liquid chromatography and electrospray ionization mass spectrometry)

  • 정봉수;박준조;금모래;김인경;박병옥;한정희
    • 한국동물위생학회지
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    • 제27권1호
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    • pp.17-29
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    • 2004
  • A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$\^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

비임상시험관리기준 시스템에서 고성능액체크로마토그래피 분석법 정확도 검증의 필요성 (Necessity of high-performance liquid chromatography validation in good laboratory practice systems)

  • 양수빈;김창열
    • 한국응용과학기술학회지
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    • 제41권2호
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    • pp.172-187
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    • 2024
  • 비임상시험관리기준에서 독성시험 전 분석법 밸리데이션은 농도 설정 및 시료 제조 측면에서 중요하다. 시험기관에서는 의뢰받은 시험물질 2종에 대한 밸리데이션을 고성능액체크로마토그래피를 이용하여 수행한 결과 특이성, 시스템 적합성, 직선성, 일내 재현성, 균질성, 안정성, 농도분석, 품질관리를 판정 기준에 만족하는 분석방법을 확립 및 검증하였다. 하지만 의뢰기관의 시험성적서상 표준물질 함량은 시험기관의 결과보다 1.34배, 1.17배 높은 결과로 나타나 비임상시험관리기준에 적합한 분석법 밸리데이션을 통한 결과 도출이 신뢰성과 안정성 확보 측면에서 중요함을 확인하였다.

C 반응성 단백질이 사람 Macrophage 탐식 기능에 미치는 영향 (Modulation of Human Macrophage Phagocytic Activity by C-reactive Protein)

  • 김용호;강신원
    • 대한의생명과학회지
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    • 제4권1호
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    • pp.35-42
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    • 1998
  • 치료목적으로 채취한 사람 복수에서 C반응성 단백질 (CRP)을 분리 정제하여 사람 대식세포 탐식활성에 미치는 영향에 대하여 연구하였다. CRP는 p-diazonium phenyl-phosphoryl choline 혹은 C-polysaccharide coupled sepharose 4B와 hydroxylapatite affinity chromatography법으로 분리 정제 시켰다. 대식 세포는 ficoll hypaque 밀도 원심 구배법으로 분리시킨 다음 부착법으로 정제시키고 탐식 시험을 이용하여 확인하였다. CRP가 대식 세포의 시험 관내 미생물 탐식 활성에 미치는 영향은 촉진 혹은 억제시키는 경향을 보였다. 즉, CRP와 대식세포 미생물 탐식능과의 관계는 반응시킨 시간, 반응계에 가해준 CRP량, 미생물ㆍ탐식세포 및 CRP상호간 반응시킨 순서에 따라서 다르게 나타났다. 대식세포의 시험관내 탐식활성에 미치는 CRP 자극의 특성은 한계자극 특성을 보였다.

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사상균의 Naringin 분해효소에 관한 연구(제3보) Aspergillus niger S-1의 naringin 용해화효소의 특성과 여름밀감의 탈고미에 대하여 (Studies on Naringinase of Mold. (Part 3) Naringin solubilizing enzyme of Aspergillus niger S-1 and removing of bitter taste from chinese citron.)

  • 기우경
    • 한국미생물·생명공학회지
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    • 제2권2호
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    • pp.111-117
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    • 1974
  • \circled1 분리선별한 Naringinase 생산균인 S-1 SP, 은 Aspergillus niger 이었다. \circled2 Naringinase중 정제된 naringin 용해화 효소를 aceton과 ammonium sulfate에 의해 결정화하였다. \circled3 Naringin용해화 효소와 naringenin 생성효소가 DEAE-sephadex A-50 column chromatography에 의해 분리되었다. \circled4 Naringin 용해화 효소에 의해 분해된 물질이 Thin layer chromatography에의해 확인되었으며 이물질은 ethylacetate 추출법에 의해 naringin분리 정량이 가능하였다. \circled5 Crude naringinase를 여름밀감 과즙과 병조림 탈고미에 이용하여 ethylacetate 추출법에 의해 naringin을 정량하고 식미시험 결과와 비교하였다. 본 연구에 많은 조언을 해 주신 경북대학교 농화학과 서정훈 박사님께 감사를 드립니다.

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참기름의 특이성분함량(特異成分含量)과 순도결정(純度決定)에 관(關)한 연구(硏究) (제(第) 1 보(報)) -Sesamin 및 관련(關聯)Sterol를 중심(中心)으로- (Studies on the Contents of Special Components and Estimation of Purity in Sesame oil -I : Contents of Sesamin and Sterols-)

  • 노일협;이문선
    • Journal of Nutrition and Health
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    • 제16권2호
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    • pp.107-114
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    • 1983
  • There has been no specific test available for identifying the sesame oil among common edible oils. As the contents of sesamin and the ratio of sterols allowed the estimation for the genuine sesame oil, the author investigated to establish some instrumental methods for verification of genuine sesame oil and its distribution in the market. The sesame oil was saponified and the sesamin and sterols were isolated from the unsaponiable fraction by Florisil column chromatography. The individual components were determined by gas- chromatography and sesamin standard (purified sesamin) was obtained by silicagel column chromatography. The gas- chromatographic condition using Flame Ionization Detector supported on 10% OV-101 with di-(2-ethylhexyl) sebacate as an internal standard was suitable, and quantitation of sesamin and sterols, including campesterol, stigmasterol and ${\beta}-sitosterol$ was carried out. The results of this study showed that contents of sesamin in genuine sesame oil were 0.3-0.5% and the ratio of stigmasterol to compesterol was 0.3-0.6 and ${\beta}-sitosterol$ to campesterol 3.0-3.8. The 50 samples from the markets in Seoul were composed of 70% genuine sesame oil, and others were mixed with palm oil, rape seed oil and soybean oil.

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밀리미터 스케일 촉매 연소기에서의 수소-공기 예혼합 가스의 촉매 연소 특성 (Catalytic Combustion Characteristics of Hydrogen-Air Premixture in a Millimeter Scale Monolith Coated with Platinum)

  • 최원영;권세진
    • 한국연소학회지
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    • 제10권1호
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    • pp.20-26
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    • 2005
  • In the present study, catalytic combustion of hydrogen-air premixture in a millimeter scale monolith coated with Pt catalyst was investigated. As the combustor size decreases, the heat loss increases in proportion with the inverse of the scale of combustion chamber and combustion efficiency decreases in a conventional type of combustor. Combustion reaction assisted by catalyst can reduce the heat loss by decreasing the reaction temperature at which catalytic conversion takes place. Another advantage of catalytic combustion is that ignition is not required. Platinum was coated by incipient wetness method on a millimeter scale monolith with cell size of $1{\times}1mm$. Using this monolith as the core of the reaction chamber, temperatures were recorded at various locations along the flow direction. Burnt gas was passed to a gas chromatography system to measure the hydrogen content after the reaction. The measurements were made at various volume flow rate of the fuel-air premixture. The gas chromatography results showed the reaction was complete at all the test conditions and the reacting species penetrated the laminar boundary layer at the honeycomb and made contact with the catalyst coated surface. At all the measuring locations, the record showed monotonous increase of temperature during the measurement duration. And the temperature profile showed that the peak temperature is reached at the point nearest to the gas inlet and decreasing temperature along the flow direction.

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Head Space Gas Chromatography를 이용한 MTBE-Methanol, MTBE-n-Heptane, n-Heptane-Methanol계의 기액평형 (Vapor-Liquid Equilibria for the Systems of MTBE-Methanol, MTBE-n-Heptane, n-Heptane-Methanol by Using Head Space Gas Chromatography)

  • 이주동;이태종;박소진
    • 공업화학
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    • 제5권4호
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    • pp.706-713
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    • 1994
  • $45^{\circ}C$$65^{\circ}C$의 등온하에서 MTBE-methanol, MTBE-n-heptane, methanol-n-heptane 각 이성분계에 대한 등온 기액 평형 데이타를 head space gas chromatography(H.S.G.C.)를 이용해서 측정하였다. 이들중에 MTBE-methanol계와 methanol-n-heptane계에서 최소공비점이 발견되었으며, 특히 methanol-n-heptane계에서는 불용영역의 존재로 인한 불균일 최소공비점을 나타내었다. 각각의 실험 데이타들은 과잉 Gibbs 에너지 모델에 합치시켜서 그 상관관계를 알아보았으며, Redlich-Kister의 적분법에 의한 열역학적 일치성 시험도 수행하였다.

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Determination of Acaricides in Honey by Solid-Phase Extraction and Gas Chromatography / Mass Spectrometry

  • Hong, Joo-Yeon;Jung, Ok-Sang;Ryoo, Jae-Jeong;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • 제30권1호
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    • pp.61-66
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    • 2009
  • An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.