• 제목/요약/키워드: Analytical determination

검색결과 1,487건 처리시간 0.021초

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
    • /
    • 제13권3호
    • /
    • pp.215-220
    • /
    • 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.

  • PDF

Studies on the Colorimetric Determination of Drugs with Phosphomolybdic Acid. I. Colorimetric Determination of Ampicillin with Phosphomolybdic acid

  • Lee, Wang-Kyu;Yoo, Byung-Tai;Kang, Gil-Jong
    • 약학회지
    • /
    • 제18권3호
    • /
    • pp.190-196
    • /
    • 1974
  • A new colorimetric method established for the determination of ampicillin was based on the reductions of phosphomolybdic acid by ampicillin to be resutled in a molybdenum blue which showed a mezimal absorbance at 770nm. The pH effects on a molybodenum blue solution was dependent significantly on temeprature, but the wave-length shift was not effected by the molybdenum blue.

  • PDF

Spectrophotometric and Kinetic Determination of Some Sulphur Containing Drugs in Bulk and Drug Formulations

  • Walash, M.I.;El-Brashy, A.M.;Metwally, M.S.;Abdelal, A.A.
    • Bulletin of the Korean Chemical Society
    • /
    • 제25권4호
    • /
    • pp.517-524
    • /
    • 2004
  • Two simple and sensitive spectrophotometric methods were developed for the determination of carbocisteine, penicillamine, ethionamide and thioctic acid in bulk and in their pharmaceutical preparations using alkaline potassium permanganate as an oxidizing agent. The first one involves determination of ethionamide and thioctic acid by spectrophotometric investigation of the oxidation reaction of the two drugs. The second method involves determination of carbocisteine and penicillamine by kinetic studies of the oxidation reaction of these two drugs at room temperature for a fixed time of 20 minutes. The absorbance of the colored manganate ions was measured at 610 nm in both methods. 1-10 ${\mu}$g/mL of ethionamide and thioctic acid could be etermined by the spectrophotometric method with detection limits of 0.11 and 0.089 ${\mu}$g/mL for the two drugs respectively. 2-10 ${\mu}$g/mL of carbocisteine and penicillamine could be determined by the kinetic method with detection limits of 0.14 and 0.21 ${\mu}$g/mL respectively. The two methods were successfully applied for the determination of these drugs in their dosage forms.

Validation of an analytical method for cyanide determination in blood, urine, lung, and skin tissues of rats using gas chromatography mass spectrometry (GC-MS)

  • Shin, Min-Chul;Kwon, Young Sang;Kim, Jong-Hwan;Hwang, Kyunghwa;Seo, Jong-Su
    • 분석과학
    • /
    • 제32권3호
    • /
    • pp.88-95
    • /
    • 2019
  • This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

중성자 방사화분석법과 원자질량분석법을 이용한 침전물 시료속에 존재하는 미량원소들의 화학종 분류 및 분석 (The chemical speciation and analysis of trace elements in sediment with neutron activation analytical method(NAA) and atomic mass spectrometry)

  • 남상호;김재진;정용삼;김선하
    • 분석과학
    • /
    • 제16권5호
    • /
    • pp.358-367
    • /
    • 2003
  • 이 연구는 먼저 침전물 속에 major 원소 (Al, Ca, K, Fe, Mg)를 측정하기위해 ICP-MS를 이용하여 분석방법을 개발하였다. Cool ICP-MS로 major원소를 분석한 결과 Normal ICP-MS보다 더 좋은 분석 결과를 얻었다. 또한 그 결과를 NAA의한 분석 결과와 비교해 보았다. NAA는 고체시료의 비파괴 미량분석법이며 침전물 속에 major원소들에 대한 측정 결과는 ICP-MS보다 더 좋은 결과를 얻었다. 또한 침전물 속에 minor 원소 (Cr, Ce, U, Co, Pb, As, Se)를 측정하기 위해 ICP-MS를 이용하여 분석방법을 개발하였다. 표준 검정곡선으로 분석한 결과 모체방해효과 때문에 정확도가 좋지 않았다. 그래서 ICP-MS를 이용하여 내부표준물법으로 minor 원소들을 분석했을 때 결과값이 향상됨을 알 수 있었다. 그 결과를 NAA분석법과 비교해도 ICP-MS를 이용한 방법이 더 좋은 결과였음을 알 수 있었다. 두 가지의 분석방법은 침전물 속에 존재하는 minor 원소를 충분히 측정할 수 있다. 그러므로 NAA 분석법이 모체가 복잡한 환경시료를 분석하는데 중요한 역할을 하며, ICP-MS 또한 NAA 분석법으로는 분석 할 수 없는 납을 검출할 수 있기 때문에 환경시료를 분석하는데 두 분석법은 상호 보완할 수 있는 중요한 분석법이다.

원자흡광분광법에 의한 식물체 중의 게르마늄 분석법 개선 (Improvement of Analytical Method for Determination of Germanium in Plant by Atomic Absorption Spectrometry)

  • 한성수;임요섭;김일광
    • 분석과학
    • /
    • 제10권3호
    • /
    • pp.179-186
    • /
    • 1997
  • 본 연구는 식물체 중 게르마늄을 분석할 때 기존의 방법보다 분석효율이 높고 간편하여 분해시간이 짧게 걸리는 방법을 찾고자 실험을 수행하였다. 시료 분해시 분해액은 $HNO_3+HClO_4+H_2SO_4$의 혼합산을 10 : 4 : 1(v/v)의 비율로 혼합 사용하였을 때 분해 소요 일수는 4~5일이었고, 회수율은 98% 이상이었다. 분해 후 최종 일정 부피로 맞추어 주기 위한 용액은 0.1M acetic acid-sodium acetate가 좋았으며, 아르곤 연료를 사용한 탄소봉원자화기부착 원자흡광분광광도계의 검출 한계는 0.02ppm이었다. 이와 같은 결과들은 식물체 중 게르마늄 분석에 있어서 전술한 실험 목적에 부합되는 결과였다.

  • PDF

식이보충제로 사용되는 히알루론산의 분석법에 대한 불확도 산정 (Measurement Uncertainty for Analytical Method of Hyaluronic Acid Used as a Dietary Supplement)

  • 박상욱;김형범;김광준;이원재
    • KSBB Journal
    • /
    • 제32권1호
    • /
    • pp.54-62
    • /
    • 2017
  • This study aimed to estimate the measurement uncertainty related to determination of hyaluronic acid used as a dietary supplement by high-performance liquid chromatography. According to the guidelines of the Association of Official Analytical Chemists, the analytical processes for determination of hyaluronic acid were performed. And the measurement uncertainty obtained during the analytical processes were expressed in accordance with mathematical/ statistical guidances of GUM (Guide to the Expression of Uncertainty in Measurement) & EURACHEM (Focus for Analytical Chemistry in Europe) for the analytical operations. For the uncertainty in measurement produced based on this analytical method, the expanded uncertainty was calculated by using the relative standard uncertainty between analytical results and sources of uncertainty in measurement (sample weight, final volume, extraction volume, standard solution, matrix and instrument etc). In the results of 95% confidence interval, it was calculated that the uncertainty in measurement was $57.75{\pm}8.76{\mu}g/kg$ (k=2.0). Therefore, it showed that the measurement uncertainty obtained by this analytical method influences on 15.2% of the contents of hyaluronic acid as the analytical results.

Determination of Selenium and Tellurium by HG-AAS in Foods

  • Cha, Ki-Won;Park, Sang-Ho;Park, Kwang-Won
    • 분석과학
    • /
    • 제8권4호
    • /
    • pp.419-425
    • /
    • 1995
  • A method has been investigated for the determination of selenium and tellurium in Ginseng, Ganoderma and Garlic using hydride generation atomic absorption spectrometry(HG-AAS). The concentration effects of hydrochloric acid and sodium tetrahydroborate on the hydride generation for the determination of selenium and tellurium were investigated. The method of sample decomposition was also investigated using various mineral acids, such as nitric, perchloric and sulfuric acid in the closed system, and foreign ion effects containing in the samples were studied. The calibration curves of selenium and tellurium were obtained in the range of 0~40 ppb. The detection limits(S/N=2) of selenium and tellurium are 0.1 and 0.2 ppb. Analytical data of selenium and tellurium in Garlic, Ganoderma and Ginseng are 289, 296 and 198 ng/g for selenium and 146, 127 and 110 ng/g for tellurium, respectively.

  • PDF

Determination of trace elements in food reference materials by instrumental neutron activation analysis

  • Cho, K.H.;Zeisler, R.;Park, K.W.
    • 분석과학
    • /
    • 제18권6호
    • /
    • pp.520-528
    • /
    • 2005
  • Two biological Certified Reference Materials (CRMs), KRISS 108-04-001 (oyster tissue) and 108-05-001 (water dropwort stem), were prepared by Korea Research Institute of Standards and Science (KRISS)during FY '01. The certified values of these materials had been determined by Isotope Dilution Mass Spectrometry (IDMS) for six elements (Cd, Cr, Cu, Fe, Pb and Zn). Additional analytical works are now progressing to certify the concentrations of a number of the environmental and nutrimental elements in these CRMs. The certified values in a CRM are usually determined by using a single primary method with confirmation by other method(s) or using two independent critically-evaluated methods. Instrumental Neutron Activation Analysis (INAA) plays an important role in the determination of certified values as it can eliminate the possibility of common error sources resulting from sample dissolution. In this study INAA procedure was used in determination of 23 elements in these two biological CRMs to acquire the concentration information and the results were compared with KRISS certified values.