• Title/Summary/Keyword: Analytical chemistry method

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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
    • Analytical Science and Technology
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    • v.32 no.3
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    • pp.88-95
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    • 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.

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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    • v.13 no.3
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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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Simultaneous Determination of Abamectin and Milbemectin Residues in Fruits

  • Lee, Young-Deuk;Kwon, Chan-Hyeok
    • Journal of Applied Biological Chemistry
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    • v.43 no.2
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    • pp.94-100
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    • 2000
  • An analytical method was developed to determine abamectin and milbemectin residues in apple, pear, and citrus using HPLC with ultraviolet absorption detection. Abamectin and milbemectin were extracted with methanol from apple, pear, and citrus samples. The extract was diluted with saline water and dichloromethane partition was followed to recover the compounds from the aqueous phase. Florisil column chromatography and aminopropyl solid-phase extraction were employed as cleanup methods to remove most of co-extractives from the sample extract. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate abamectin and milbemectin residues in sample extracts at the wavelength of 245 nm. Recoveries of abamectin and milbemectin from fortified samples ranged 80.4~90.3% and 90.9~96.8%, respectively. Relative standard deviations of the analytical method were less than 10% for both acaricides. Detection limit of the analytical method was 0.003 mg/kg sample for all the analytes. The proposed method was reproducible and sensitive enough to evaluate terminal residues of abamectin and milbemectin in apple, pear, and citrus.

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Studies on the Terpenoids in the Volatile Constituents of Liaoning Schisandra Chinensis Baillon

  • Hou, Dongyan;Zhang, Weihua;Hui, Ruihua
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.505-509
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    • 1995
  • The terpenoids in the volatile constituents of Liaoning Shcisandra Chinesis Baillon have been determined by the analytical method of GC/MS. Thirty terpenoids molecular structure were characterized. They are 11.89% monterpenes, 4.60% monoterpene oxides, 58.74% sesquiterpene hydrocarbons, and 1.62% oxygen-containing sesquiterpenoids in the total volatile constituents quantified by chromatograph. Among them, the sesquiterpene make up the characteristic constituents. Every terpenoid constituent percent content was obtained using area normalization method of HP-59970 chemstation.

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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
    • YAKHAK HOEJI
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    • v.18 no.3
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    • pp.190-196
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    • 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.

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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
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    • v.25 no.4
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    • pp.517-524
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    • 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.

Determination of Gold by Flame Atomic Absorption Spectrophotometry using a New Chelating Agent (새로운 킬레이트 시약을 이용한 금의 원자흡수광도법 정량)

  • Lee, Jin-Sik;Uesugi, Katsuya;Thoru, Nagahiro;Choi, Won-Hyung;Kim, Kyung-Tae;Choi, Sung-Yung
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.391-396
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    • 1995
  • A rapid preconcentration method based on solvent extraction is described for the determination of gold by flame atomic absorption spectrophotometry. Trace amounts of gold was extracted as a new chelating agent, 3-thiophenaldehyde-4-phenyl-3-thiosemicarbazone from pH 4.0 in diisobutyl ketone. The method is simple, fast, free from the effect of many interfering ions and has a high sensitivity and a good precision. Gold is quantitatively separated and concentrated from the elements in standard sample, and the value of the recovery was 91.7 and 108.3% by the proposed method.

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