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

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.

2009 ◽  
Vol 15 (2) ◽  
pp. 77-81 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagaraju Rajendraprasad ◽  
Basavaiah Vinay

Two simple, rapid, reliable and cost-effective methods based on titrimetry in non-aqueous medium are described for the determination of olanzapine in pharmaceuticals. In these methods, the drug dissolved in the glacial acetic acid was titrated with the acetous perchloric acid with visual and potentiometric end point detection, crystal violet being used as the indicator for visual titration. The methods are applicable over 1-15 mg range of olanzapine. The procedures were applied to determine olanzapine in pharmaceutical products and the results were found to be in a good agreement with those obtained by the reference method. Associated pharmaceutical materials did not interfere. The precision results, expressed by inter-day and intra-day relative standard deviation values, were satisfactory, higher than 2%. The accuracy was satisfactory as well. The methods proved to be suitable for the analysis of olanzapine in bulk drug and in tablets. The accuracy and reliability of the methods were further ascertained by recovery studies via a standard addition technique with percent recoveries in the range 97.51-103.7% with a standard deviation of less than 2%.


2021 ◽  
Vol 87 (12) ◽  
pp. 11-16
Author(s):  
E. I. Shinko ◽  
O. V. Farafonova ◽  
T. N. Ermolaeva

Conditions for the preparation of carbon nanomaterials for embedding into the discerning layer of a piezoelectric immunosensor are described. The effect of the oxidation method, temperature, and the duration of treatment of nanomaterials with an oxidizing agent on the surface concentration of active functional groups is demonstrated. It is shown that the use of carboxylated carbon nanotubes (CNT) increases the efficiency of their binding to biomolecules and increases the stability of the discerning layer of a piezoelectric sensor when measurements are carried out in liquid media. Conditions for the determination of antibiotics using piezoelectric immunosensors modified with carbon nanomaterial were studied including the choice of immunoreagent concentrations and assessment of the selectivity of antibiotic determination. The CNT-based piezoelectric immunosensors providing rapid, highly sensitive, and selective determination of the analyte at the MRL level and below it in food products and biological fluids are proposed.


2020 ◽  
Vol 36 (1(103)) ◽  
pp. 113-125
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica

2-Nitroanisole is a colourless or slightly yellowish liquid. This substance is mainly used in the production of o-anisidine (2-methoxyaniline), which is directly or indirectly used for the production of more than 100 azo dyes. 2-Nitroanisole may cause cancer to humans. The aim of this study was to develop a method for determining concentrations of 2-nitroanisole in workplace air in the range from 1/10 to 2 of maximum admissible concentration (MAC) values. The developed method is based on the adsorption of 2-nitroanisole on a silica gel, extraction with methanol and chromatographic analysis of the resulting solution. The tests were performed using a liquid chromatograph (HPLC) 1200 series of Agilent Technologies with a diode array detector (DAD). Determinations were performed using an Ultra C18 column (25 cm × 4.6 mm, dp = 5 µm). The procedure was validated according to Standard No. EN 482. The method can be used to determine 2-nitroanisole in workplace air in the concentration range from 0.16 to 3.2 mg/m3, i.e., from 1/10 to 2 MAC values. In that range, the obtained calibration curve was linear, as evidenced by the regression coefficient of 1. The overall accuracy of the method was about 5.3% and its relative total uncertainty was 23%. This method enables selective determination of 2-nitroanisole in workplace air in the presence of other compounds, such as methanol, o-anisidine, 3-nitroanisole, 4-nitroanisole and 1-chloro-2-nitrobenzene. The method for determining 2-nitroanisole has been recorded in the form of an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.


2000 ◽  
Vol 68 (3) ◽  
pp. 297-307 ◽  
Author(s):  
Rizk M. ◽  
Belal F. ◽  
Ibrahim F. ◽  
Ahmed S. ◽  
Sheribah Z.A.

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.


1972 ◽  
Vol 18 (9) ◽  
pp. 996-1000 ◽  
Author(s):  
A R Pettigrew ◽  
G S Fell

Abstract A colorimetric procedure for determination of small amounts of cyanide and thiocyanate, involving the synthesis of a pyridine dyestuff by the reaction of pyridine and an aromatic amine, has been simplified for the estimation of thiocyanate alone in biological fluids. Replacement of benzidine with p-phenylenediamine in the colorimetric reaction has both improved the precision of the analytical procedure and avoided a carcinogenic hazard. This method has been used to follow the decrease in plasma thiocyanate associated with abstinence from cigarette smoking, and its subsequent increase upon resumption. It has also been used to measure the plasma and urinary thiocyanate concentrations of patients suffering from the particular toxic amblyopias—tobacco amblyopia and Leber’s hereditary optic atrophy— believed to be associated with cyanide toxicity, and to follow the increased thiocyanate concentrations that accompany significant improvements in the patients’ vision brought about by various treatments.


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