scholarly journals Derivative UV Spectrophotometric Analysis of Some Pharmaceutically Important Halogenated 8-Hdroxyquinoline Derivatives via Their Pd (II)-Complexes

2000 ◽  
Vol 68 (3) ◽  
pp. 297-307 ◽  
Author(s):  
Rizk M. ◽  
Belal F. ◽  
Ibrahim F. ◽  
Ahmed S. ◽  
Sheribah Z.A.
Keyword(s):  
Linear Correlation ◽  
Limit Of Detection ◽  
Reference Method ◽  
Dosage Forms ◽  
Uv Spectra ◽  
Spectrophotometric Analysis ◽  
Zero Order ◽  
First Order ◽  
Tablet Formulations ◽  
Selective Analysis

A derivative UV-spectrophotometric method was developed for the analysis of two halogenated 8-hydroxyquinoline derivatives; iodochlorohyroxyquin (I) (Clioquinol) and diiodohydroxyquin (II) (iodoquinol). The proposed method depends on the formation of Pd II-ligand complexes in methanol-acetonitrile mixture, which exhibits an UV-spectra with an appreciable value of ε. Zero order (0D), first order (1D) and fourth order (4D) derivative measurements were applied for the quantitative analysis of the drugs. A linear correlation was established between absorbance and concentration for the 0D mode in the range 2-14µg ml-1 and 2-18 µg ml-1 for (I) and (II) with average % recoveries of 99.83 ± 1.04 and 99.9 ± 0.64 respectively. Also a linear correlation was obtained between the trough of the peak and concentration for 1D mode in the range of 0.16-0.8 µgml-1 for both dmgs with average % recoveries of 100.23 ± 1.04 and 100.18 ± 1.14 for (I) and (II) respectively. Besides, the 1D mode was successfully applied for the analysis of binary mixture containing both (II) and metronidazole (III) in tablet formulations. The average % recoveries were 99.42 ± 0.358 and 98.81 ± 0.973 for (II) and (III) respectively. In the 4D mode, a linear correlation was attained between the amplitude of the peak and concentration in the range 0.1-0.8 µgml-1 for (I) and (II), with average % recoveries of 99.6 ± 0.84 and 100.06 ± 0.98. The limit of detection (LOD) was 2.1 µg ml-1 and 2.3 µg ml-1 for (I) and (II) respectively. The suggested method was successfully applied for accurate, sensitive and selective analysis of the studied drugs in bulk and single or combined dosage forms with average % recoveries of 99.74 ± 0.480–99.84 ± 0.515 and 99.44 ± 0.71–100.58 ± 1.06 for (1D) and (4D) respectively. The results obtained were favorably compared to those given by a reference method.

scholarly journals Derivative Spectrophotometric Analysis of 4-Quinolone Antibacterials in Formulations and Spiked Biological Fluids by Their Cu(II) Complexes

2001 ◽  
Vol 84 (2) ◽  
pp. 368-375 ◽  
Author(s):  
Mohammed Rizk ◽  
Fathalla Belal ◽  
Fawiza Ibrahim ◽  
Soad Ahmed ◽  
Zeinab A Sheribah
Keyword(s):  
Aqueous Medium ◽  
Linear Correlation ◽  
Analytical Procedure ◽  
Biological Fluids ◽  
Reference Method ◽  
Spectrophotometric Analysis ◽  
Third Order ◽  
Selective Determination ◽  
Average Percentage

Abstract A derivative UV-spectrophotometric analytical procedure was developed for determination of three 4-quinolone antibacterials: norfloxacin (NFX), ciprofloxacin (CFX), and sparfloxacin (SFX). The method depends on the complexation of Cu(II) with the studied compounds in aqueous medium. A third order, measurement was applied for their quantification. A linear correlation was established between the amplitude of the peak and concentration for all the studied drugs in the range of 15–80, 35–120, and 200–700 ng/mL, with minimum detectability (S/N = 2) of 1.0, 1.3, and 5.1 ng/mL for NFX, CFX, and SFX, respectively. The method was successfully applied for accurate, sensitive, and selective determination of the studied drugs in bulk and tablets formulation with average percentage recoveries of 99.22 ± 0.55 to 100.33 ± 1.60. The results obtained were favorably compared with those of the reference method. The method was also used to determine sparfloxacin in spiked human plasma and urine. The results obtained were satisfactory, accurate, and precise.

scholarly journals DEVELOPMENT AND VALIDATION OF DIFFERENTIAL PULSE POLAROGRAPHIC ANALYSIS OF FENOFIBRATE IN PURE AND PHARMACEUTICAL DOSAGE FORMS USING DROPPING MERCURY ELECTRODE

2016 ◽  
Vol 8 (10) ◽  
pp. 284
Author(s):  
Abdul Aziz Ramadan ◽  
Hasna Mandil ◽  
Reham Abu-saleh
Keyword(s):  
Limit Of Detection ◽  
Mercury Electrode ◽  
Reference Method ◽  
Differential Pulse ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Polarographic Analysis ◽  
Relative Standard ◽  
Dropping Mercury Electrode

<p><strong>Objective: </strong>An easy, fast, accurate and sensitive differential pulse polarographic analysis for determination of fenofibrate (FEN) in pure and pharmaceutical dosage forms using dropping mercury electrode (DME) was applied.</p><p><strong>Methods: </strong>The method involves the electrochemical reduction of fenofibrate at DME by differential pulse polarographic analysis (DPPA). Different buffer solutions were used over a wide pH range (1.0–10.0). The best definition of the analytical signals was found in lithium perchlorate trihydrate buffer at pH 6.0 containing 24% (v/v) acetonitrile at-994 to-1025mV (versus Ag/AgCl).</p><p><strong>Results: </strong>Under optimized conditions the peak current (I<sub>p</sub>) is linear over the range 0.0361-3.608 μg/ml. The DPPA was used successfully for the determination of FEN in pure and pharmaceutical dosage forms. The relative standard deviation did not exceed 2.1% for the concentration of FEN 0.0361 μg/ml. Regression analysis showed a good correlation coefficient (R<sup>2</sup>= 0.9994) between Ip and concentration at the mentioned range. The limit of detection (LOD) and the limit of quantification (LOQ) was to be 0.0025 and 0.0076 μg/ml, respectively. The proposed method was validated for linearity, precision and accuracy, repeatability, sensitivity (LOD and LOQ), robustness and specificity with an average recovery of 99.8-100.6%.</p><p><strong>Conclusion: </strong>The developed method is applicable for the determination of FEN in pure and different dosage forms with the assay of marketed formulations 99.8-104.0% and the results are in good agreement with those obtained by square-wave voltammetry (SWV) reference method.</p><p><strong>Keywords: </strong>Differential pulse polarographic analysis, Fenofibrate, Pharmaceutical formulations</p>

scholarly journals FIRST-ORDER ULTRAVIOLET DERIVATIVE SPECTROPHOTOMETRIC METHODS FOR DETERMINATION OF RESERPINE IN ANTIHYPERTENSION TABLET

2012 ◽  
Vol 12 (3) ◽  
pp. 268-272 ◽  
Author(s):  
Latifah K Darusman ◽  
Mohamad Rafi ◽  
Wulan Tri Wahyuni ◽  
Rizna Azrianiningsari
Keyword(s):  
Limit Of Detection ◽  
Low Cost ◽  
Reference Method ◽  
Ml Estimation ◽  
Mean Values ◽  
First Order ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Limit Of Quantitation

A new ultraviolet derivative spectrophotometry (UVDS) method has been developed for determination of reserpine in antihypertension tablets. A first-order UVDS based on the measurement of the distance between peaks to baseline (DZ) at the wavelength of 312 nm was used. Evaluation of analytical performance showed that accuracy as percentage recovery was 99.18-101.13%, precision expressed as relative standard deviation (RSD) was 1.91% and linear correlation was also obtained 0.9998 in the range of 10-50 µg/mL. Estimation of limit of detection and limit of quantitation was 0.8868 µg/mL and 2.6874 µg/mL, respectively. As a reference method, HPLC methods from United States Pharmacopiea (USP) were used. Commercially tablets available were analyzed by the two methods. The content of reserpine in tablets was found 0.2260±0.0033 mg by UVDS and 0.2301±0.0051 mg by the USP methods. The result obtained from the two methods was compared statistically using F-test and t-test and showed no significant differences between the variance and mean values of the two methods at 95% confidence level. This method was faster, easier, low cost and gave result as well as the reference method published by USP.

QUANTITATIVE DETERMINATION OF DEFERASIROX IN BULK AND PHARMACEUTICAL FORMULATION BY UV SPECTROPHOTOMETRIC METHOD

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (02) ◽  
pp. 27-32
Author(s):  
G. M Marathe ◽  
◽  
V. V. Pande ◽  
P. H. Patil ◽  
R. E. Mutha ◽  
...  
Keyword(s):  
Detection Limit ◽  
Quantitative Determination ◽  
Spectrophotometric Method ◽  
Dosage Forms ◽  
Zero Order ◽  
Pharmaceutical Dosage Forms ◽  
Pharmaceutical Tablet ◽  
Quantitation Limit ◽  
Tablet Formulations

A simple, fast and reliable zero order spectrophotometric method was developed for determination of deferasirox in bulk and pharmaceutical dosage forms. Beer’s law was obeyed in concentration range of 2–12 µ/ml deferasirox at 245.6 nm wavelength. The correlation coefficient was found to be (r2 = 0.999), precision (repeatability % RSD 1.29), percentage recovery 100.054±0.271. The detection limit (DL) and quantitation limit (QL) were 0.247 µg/ml and 0.75 µg/ml respectively. The proposed method was found to be simple, accurate, precise, reproducible and gave an acceptable recovery of the analyte, which could be directly and easily applied to analysis of bulk and pharmaceutical tablet formulations of deferasirox.

scholarly journals Differential Pulse Polarographic Behavior and Quantification of the Flucloxacillin in Pure and Pharmaceutical Dosage Forms Using a Static Mercury Drop Electrode

2018 ◽  
Vol 15 (2) ◽  
pp. 6235-6247
Author(s):  
Abdul Aziz Ramadan ◽  
Hasna Mandil ◽  
Reham Abu Saleh
Keyword(s):  
Limit Of Detection ◽  
Reference Method ◽  
Differential Pulse ◽  
Dosage Forms ◽  
Calibration Graph ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Mercury Drop Electrode ◽  
Relative Standard

Differential pulse polarographic analysis (DPPA) by using static mercury drop electrode (SMDE) for quantification of flucloxacillin (FLUX) in pure and pharmaceutical dosage forms was studied. The optimum conditions for the polarographic signal were determined and a study was made of the different parameters affecting the electrochemical process. The best definition of the analytical signals was found in Britton–Robinson buffer (0.06 M) at pH 4.0 . Under the optimum conditions, liner calibration graph, Ip=f(CFLUX) was obtained in the concentration ranges of 0.1 mM (0.0494 ?g.mL-1) to 26 mM (12.8414 ?g.mL-1) at -940 to -1000 mV (versus Ag/AgCl) with relative standard deviations (RSD) did not exceed 2.4% for the concentrations of FLUX (0.0494 ?g.mL-1). Regression analysis showed a good correlation coefficient (R2=9998) between Ip and concentration over the mentioned range. The limit of detection (LOD) and the limit of quantification (LOQ) were to be 0.0040 and 0.0120 ?g.mL-1, respectively. The proposed method was validated for linearity, precision and accuracy, repeatability, sensitivity (LOD and LOQ), robustness and specificity. The developed method is applicable for the determination of FLUX in pure and different dosage forms in presence a same amount of amoxicillin (AMOX) with average recovery of 99.4 to 102.2 % and the results are in good agreement with those obtained by the HPLC reference method.  

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

Kinetics of catalytic reduction of nitrogen oxide by carbon monoxide on CuO/Al2O3 catalyst

1983 ◽  
Vol 48 (11) ◽  
pp. 3202-3208 ◽  
Author(s):  
Zdeněk Musil ◽  
Vladimír Pour
Keyword(s):  
Carbon Monoxide ◽  
Nitrogen Oxide ◽  
Rate Equation ◽  
Catalytic Reduction ◽  
Zero Order ◽  
Spectroscopic Measurements ◽  
First Order ◽  
Ir Spectroscopic ◽  
Kinetics Of ◽  
Al2o3 Catalyst

The kinetics of the reduction of nitrogen oxide by carbon monoxide on CuO/Al2O3 catalyst (8.36 mass % CuO) were determined at temperatures between 413 and 473 K. The reaction was found to be first order in NO and zero order in CO. The observed kinetics are consistent with a rate equation derived from a mechanism proposed on the basis of IR spectroscopic measurements.

scholarly journals Detection of Exosomes Using Total Internal Reflected Imaging Ellipsometry

Biosensors ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 164
Author(s):  
Haoyu Liu ◽  
Wei Liu ◽  
Gang Jin
Keyword(s):  
Limit Of Detection ◽  
Biological Fluids ◽  
Surface Proteins ◽  
Surface Markers ◽  
Functional Roles ◽  
Disease Biomarkers ◽  
First Order ◽  
Imaging Ellipsometry ◽  
Interaction Kinetics ◽  
Membrane Bound

Exosomes are a kind of membrane-bound phospholipid nanovesicle that are secreted extensively in a variety of biological fluids. Accumulating evidence has indicated that exosomes not only communicate with cells, but also perform functional roles in physiology and pathology. In addition, exosomes have also elicited a great deal of excitement due to their potential as disease biomarkers. Therefore, requirements for sensitive methods capable of precisely and specifically determining exosomes were needed. Herein, we not only develop a sensing surface to capture exosomes but also compare two surface proteins on exosomes, which are appropriate for detecting exosome surface markers by total internal reflected imaging ellipsometry (TIRIE). Protein G and antibody were immobilized on a thin layer of golden substrate to form the biosensing surface. The bio-interaction between antibodies and exosomes was recorded by the TIRIE in real time. The distance between exosomes adhered on a surface was 44 nm ± 0.5 nm. The KD  of anti-CD9 and exosome was lower than anti-CD63 and exosome by introducing pseudo-first-order interaction kinetics, which suggested that CD9 is more suitable for exosome surface markers than CD63. The limit of detection (LOD) of TIRIE was 0.4 μg/mL. In conclusion, we have proposed a surface for the detection of exosomes based on TIRIE, which can make the detection of exosomes convenient and efficient.

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