• 제목/요약/키워드: Chromatographic assay

검색결과 120건 처리시간 0.024초

First Derivative Spectrophotometric and Gas-Liquid Chromatographic Determination of Caffeine in Foods and Pharmaceuticals III. Simultaneous assay of caffeine and some antihistaminics

  • Abdel-Moety, Ezzat M.;El-Tarras, Mohamed F.;El-Zeany, Badr-Eldin A.;Kelani, Khadiga O.
    • Archives of Pharmacal Research
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    • 제13권3호
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    • pp.215-220
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    • 1990
  • Two different, derivative spectrophotometric and gas-liquid chromatographic, procedures for direct quantitation of caffeine and some commonly dispensed antihistaminics in bulk forms, in their laboratory prepared mmixtures and in dosage formulations, have been investigated. The limit, sensitivity reproducibility and accuracy of each method were studied for each individual drug substance and in some usual pharmaceutical formulations.

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혈장중 Acebutolol 및 그 Acetyl 대사체의 HPLC 분석 (High Performance Liquid Chromatographic Assay of Acebutolol and its Acetyl Metabolite in Plasma)

  • 백채선
    • Journal of Pharmaceutical Investigation
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    • 제23권3호
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    • pp.133-137
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    • 1993
  • A high-performance liquid chromatographic assay using ion-pair reverse-phase system was developed for the separation of acebutolol and acebutolol acetyl metabolite in plasma. A ion-pair reversephase system consisting of an ODS-bonded silica column and a mixture of 20% $CH_3CN$, 0.1% $H_3PO_4$, 0.035 M heptanesulfonic acid and 0.005 M tetrabutylammonium hydrogen sulfate as the mobile phase were used. Triamterene was employed as an internal standard. Based on 0.2 ml of plasma, the detection limits were 10.4 ng/ml for acebutolol and 10.3 ng/ml of acebutolol acetyl metabolite at the signal-to-noise ratio of 3:1.

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형광 크로마토그래피에 의한 콜레스테롤 측정법의 개발 (Development of Total Cholesterol Detection System by Fluorescence Chromatography)

  • 오상욱
    • 한국식품위생안전성학회지
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    • 제24권2호
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    • pp.148-153
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    • 2009
  • 본 연구에서는 심혈관계 질환의 표지인자인 콜레스테롤의 농도를 새롭게 개발한 형광 크로마토그라피 방법에 의하여 측정 하고자 시도하였다. 개발된 측정 시스템은 크로마토그라피 스트립이 들어 있는 카트리지, 발색제 AEC, 콜레스테롤 옥사데이즈 (Cholesterol Oxidase, CO), 콜레스테롤 에스트라아제(Cholesterol Esterase, CE), 호스래 디쉬페록시다아제 (Horseradish peroxidase, HRP)를 포함하는 효소혼합 수용액, 그리고 형광 판독기로 구성되어 었다. 콜레스테롤 농도 변화에 따른 형광 세기 변화로 얻은 상관계수 r= 0.968로 측정 가능한 농도 범위에서 신뢰할 만한 직선성 관계를 제시하여 주었다. 회복률과 Hitachi 747 검사기기와 비교 테스트에서는 각각 106.5-94%와 상관관계 r = 0.939 (p<0.001)로 비교적 높은 유의성을 보여주었다. 따라서 본 연구에서 개발된 새로운 콜레스테롤 농도 측정법은 빠른 반응 시간 (8분)과 적은 시료량 ($5\;{\mu}l$)을 사용하기에 시료를 실험실로 운반할 필요없이 클리닉에서 측정 가능한 준현장검사 플랫폼형으로 개발되었으며 기존의 고가의 자동화 장비를 사용하는 생화학적 진단방식 대체용으로의 응용이 기대된다.

Development of Geno-chromatographic Assay System for Salmonella species

  • 김석하;오홍일;조정환;백세환
    • 한국생물공학회:학술대회논문집
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    • 한국생물공학회 2001년도 추계학술발표대회
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    • pp.827-828
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    • 2001
  • 이 실험은 특정 DNA를 검출 할 수 있는 새로운 방법을 제시하고 개발하려는 것이다. 이것은 geno-chromatography 분석방법이라고 하여 DNA capture probe를 membrane상에 고정하고 PCR을 통하여 증폭된 특정 유전자를 hybridization 반응을 이용하여 탐지하는 것이다. 이러한 개념을 식중독균의 일종인 Salmonella 균의 탐지에 적용하여 그 분석시스템의 성능을 확인 할 수 있었다.

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혈장중 Ofloxacin의 HPLG분석 (High Performance Liquid Chromatographic Assay of Ofloxacin in Plasma)

  • 백채선;김영수
    • 한국임상약학회지
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    • 제10권1호
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    • pp.38-41
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    • 2000
  • A high-performance liquid chromatographic method with fluorometric detection was evaluated for analysis of ofloxacin in plasma. Biological fluids (plasma, $200\;{\mu}L$) were prepared for assay by protein precipitation with chlorofurm. The detection of ofloxacin and triamterene as an internal standard were performed at 358 nm for excitation and 495 nm for emission. The HPLC separation was carried out on Ultrasphere ODS column (4.6 mm${\times}25\;cm,\;5\;{\mu} m$) with acetonitrile $(45\%)$-phosphoric acid $(1.5\%)\;containing\;0.3\%$ sodium laurylsulfate as the mobile phase. The flow-rate was 1.0 mL/min. The calibration graphs were linear from 3.0 to 80 ng/mL with r=0.998. The minimal detectable concentration in plasma was 1.5 ng/mL. The proposed technique is reproducible, selective, reliable and sensitive.

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A Dilute-and-Shoot LC-MS/MS Method for Screening of 43 Cardiovascular Drugs in Human Urine

  • Pham, Thuy-Vy;Lee, Gunhee;Mai, Xuan-Lan;Le, Thi-Anh-Tuyet;Nguyen, Thi Ngoc Van;Hong, Jongki;Kim, Kyeong Ho
    • Mass Spectrometry Letters
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    • 제12권1호
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    • pp.1-10
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    • 2021
  • A simple, specific, and economical LC-MS/MS method was investigated for the screening of 43 prescribed antihypertensive and related drugs in human urine. The urine samples were simply prepared by diluting and mixing with internal standard before directly introduced to the LC-MS/MS system, which is fast, straightforward, and cost-effective. Fractional factorial, Box-Behnken, and I-optimal design were applied to screen and optimize the mass spectrometric and chromatographic factors. The analysis was carried out on a triple quadrupole mass spectrometer system utilizing multiple reaction monitoring with positive and negative electrospray ionization method. Chromatographic separation was performed on a Thermo Scientific Accucore RP-MS column (50 × 3.0 mm ID., 2.6 ㎛) using two separate gradient elution programs established with the same mobile phases. Chromatographic separation was performed within 12 min. The optimal method was validated based on FDA guideline. The results indicated that the assay was specific, reproducible, and sensitive with the limit of detection from 0.1 to 50.0 ㎍/L. The method was linear for all analytes with coefficient of determination ranging from 0.9870 to 0.9981. The intra-assay precision was from 1.44 to 19.87% and the inter-assay precision was between 2.69 and 18.54% with the recovery rate ranges from 84.54 to 119.78% for all drugs measured. All analytes in urine samples were stable for 24 h at 25℃, and for 2 weeks at -60℃. The developed method improves on currently existing methods by including larger number of cardiovascular medications and better sensitivity of 12 analytes.

혈장중 비스테로이드성 소염진통제의 HPLC분석 (High Performance Liquid Chromatographic Assay of Non-steroidal Anti-inframmatory Drugs in Plasma)

  • 백채선
    • 한국임상약학회지
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    • 제5권2호
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    • pp.71-74
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    • 1995
  • A high performance liquid chromatographic method has been developed for the simultaneous analysis of non-steroidal anti-inflammatory drugs in plasma. The simultaneous determination of ibuprofen, fenoprofen and ketoprofen is performed by RP-HPLC with UV detection. The chromatographic system consisted of Spherisorb octyl column$(5{\mu}m)$ ; the mobile phase was $acetonitrile\;-\;0.5\%$ phosphoric acid(55 : 45, v/v) and the detection wavelength was 230nm. Tolmetin was employed as an internal standard. The method described is rapid and simple with sensitivity limits of $2.0{\mu}g/ml$ ibuprofen, $0.5{\mu}g/ml$ fenoprofen and $0.3{\mu}g/ml$ ketoprofen and is suitable for routine clinical and pharmacokinetic studies.

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Legionella Pneumophila 검출을 위한 효소면역측정 스트립 센서 (An Enzyme-linked Immunosorbent Assay Strip Sensor for the Detection of Legionella Pneumophila)

  • 김영기;박소정
    • 공업화학
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    • 제25권5호
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    • pp.544-547
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    • 2014
  • 본 연구에서는 효소면역 분석법(enzyme-linked immunosorbent assay)과 면역크로마토그래픽 기법을 결합하여 Legionella pneumophila 검출을 위한 면역스트립을 제작하였다. 면역스트립은 4종의 멤브레인을 이용하여 제작하였다. 니트로셀룰로오스 멤브레인은 포획항체를 고정화하여 신호 발생을 일으키기 위해 사용되었고, 두 종류의 유리섬유 멤브레인은 각각 중합체 패드와 시료주입 패드로 사용되었다. 셀룰로오스 멤브레인은 모세관 현상으로 시료흐름을 유도하는 흡수 패드로 이용하였다. 샌드위치 면역반응과 효소반응에 의해 30 min 이내에 생성된 발색신호는 정성 및 정량 분석이 가능하였다. 분석조건 하에서 육안에 의한 정성 검출뿐 아니라, $1.3{\times}10^3-1.3{\times}10^6CFU/mL$ 범위의 L. pneumophila 농도를 디지털카메라와 자체 제작된 소프트웨어를 이용하여 정량적으로 분석할 수 있었다.

High Performance Liquid Chromatographic Assay of a New Fluoroquinolone, LB20304, in the Plasma of Rats and Dogs

  • Seo, Mi-Kyeong;Jeong, Yi-Na;Kim, Hoon-Joo;Kim, In-Chull;Lee, Yong-Hee
    • Archives of Pharmacal Research
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    • 제19권6호
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    • pp.554-558
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    • 1996
  • High-performance liquid chromatographic method was developed for the determination or LB 20304 (compound 1) in the plasma of rats and dogs. The analyte was deproteinized with 1 volume of methanol and 1/2 volume of 10% zinc sulfate, and the supernatant was injected onto a reversed-phase HPLC column. The mobile phase was a mixture of 24 parts of acetonitrile and 76 parts of 0.1% trifluoroacetic acid. The flow rate was 1 ml/min, and the effluent was monitored by fluorescence detector at an excitation wavelength of 337 nm and an emission wavelength of 460 nm. The retention time of compound 1 was 6.3 min. The assay of compound 1 was linear over the concentration range of 0.2-100.mu.g/ml in the plasma of rats and dogs. The lower limit of quantification was 0.2.mu.g/ml using 100.mu.l of plasma with a 97-99% accuracy and a 12-14% precision. In the 0.5, 5, and 50.mu.g/ml quality control samples, the intra- and inter-day accuracy were 88-95% and 88-97%, whereas intra- and interday precision were 0.5-6.6% and 0.2-9.3%, respectively, in the plasma of rats and dogs. The recoveries were 68-71% independent of concentration and species in the plasma. No interferences from endogenous substances were observed. Taken together, the above HPLC assay method by deproteinization and fluorescence detection was suitable for the determination of compound 1 in the preclinical pharmacokinetics.

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