scholarly journals Azocoupling Reaction Of Cephalosporin Antibiotics With 8-Hydroxyquinoline And Its Application In The Analysis Of Medicinal Products

2020 ◽  
Vol 15 (3) ◽  
pp. 144-155
Author(s):  
O. Kostiv ◽  
O. Korkuna ◽  
M. Ornat
Keyword(s):  
Quality Control ◽  
Spectrophotometric Determination ◽  
Azo Compounds ◽  
Optimal Conditions ◽  
Medicinal Products ◽  
Final Volume ◽  
Auxiliary Substance ◽  
Cephalosporin Antibiotics ◽  
High Standards

Methods for spectrophotometric determination of cephalosporin antibiotics ceftazidime and ceftriaxone using azocoupling reactions with 8-hydroxyquinoline have been developed. Optimal conditions for the diazotization of antibiotics in hydrochloric acid (CHCl = 12 M) and subsequent azocoupling with 8-hydroxyquinoline in alkaline medium (0.16 M NaOH in the final volume) were established. The of azocopling products of violet and light red colors are formed, which are characterized by absorption maxima at 553 nm (ε553 = 6.31·103 M-1 cm-1) and 550 nm (ε550 = 1.45·104 M-1 cm-1) for ceftazidime and ceftriaxone, respectively. Stoichiometric ratios of the azo compounds components were determined using continuous variations methods and in both cases are 1:1. Sensitive methods of spectrophotometric determination of ceftazidime (LOD = 1.81∙10-6 M) and ceftriaxone (LOD = 5.92·10-7 M) have been developed. The selectivity of cephalosporin antibiotics spectrophotometric determination in the presence of auxiliary substance (sodium carbonate) has been investigated. The elaborated methods has been approved during the analyses of model solutions and the single component drug. The recommended procedure is well suited for the ceftazidime and ceftriaxone assay in medicine to assure high standards of quality control.

scholarly journals SPECTROPHOTOMETRIC DETERMINATION OF ANTIOXIDANT SODIUM METABISULPHITE CONTENT IN PREPARED MEDICINAL FORMS OF VETERINARY MEDICINAL PRODUCTS

2020 ◽  
Vol 21 (2) ◽  
pp. 189-198
Author(s):  
H. Yu. Teslyar ◽  
M. Ya. Smolinska ◽  
I. Ya. Kotsyumbas ◽  
N. M. Chyhyn ◽  
N. G. Rohulia ◽  
...  
Keyword(s):  
Spectrophotometric Determination ◽  
Storage Time ◽  
Analytical Signal ◽  
Veterinary Drugs ◽  
Biologically Active Substances ◽  
Biologically Active ◽  
Optimal Conditions ◽  
Sodium Metabisulphite ◽  
Active Substances

An analytical method for the quantitative determination of antioxidant sodium metabisulphite in veterinary drugs has been proposed by spectrophotometric method. Based on the literature data, the optimal conditions of the analytical reaction were selected experimentally. The dependence of the value of the analytical signal on the temperature of the reaction medium, concentration of p-rosaniline and duration of the reaction was investigated to establish the optimal conditions of the analytical reaction and obtain a stable analytical signal. The stability of the colored analytical form in time was also checked and the linear dependence of the value of the analytical signal on the concentration of sodium metabisulphite was investigated. The analytical reaction at room temperature is optimal. The maximum analaytical signal is achieved by carrying out the analytical reaction for 10 minutes and then practically does not change for an hour. To achieve the maximum analytical signal, it is necessary to use a 20-fold excess of dye relative to sodium metabisulphite. The analytical signal remains stable only for the first hour, then gradually begins to decrease. Metrological characteristics of the method of determination of metabisulphite in veterinary drugs are calculated, the limits of spectrophotometric determination are 0.33 – 2.50 μg/ml. The correctness of the developed method was checked on model solutions by the method of "introduced-found" method of comparison in the presence of various biologically active substances that are part of drugs together with sodium metabisulphite. The content of sodium metabisulphite in veterinary drugs of domestic and foreign production at different intervals of their storage time was established. It is shown that the content of sodium metabisulphite in drugs decreases during their storage time, until complete disappearance, which directly affects the content of the active substance, because in the absence of antioxidant oxidative processes with biologically active substances begin to take place.

HPLC Tests in Quality Control under the Market Surveillance Program for Medicinal Products Containing Amlodipine and Valsartan

2021 ◽  
Vol 17 ◽  
Author(s):  
Dessislava Ilieva-Tonova ◽  
Ivanka Pencheva ◽  
Assena Serbezova
Keyword(s):  
Quality Control ◽  
Surveillance Program ◽  
Medicinal Products ◽  
Market Surveillance ◽  
Multi Stage ◽  
Quality Assurance Process ◽  
Significant Difference ◽  
Assurance Process ◽  
Determination Of Impurities

Background: Quality is one of the three main characteristics of medicinal products. The quality assurance process is multi-stage: during the manufacturing, quality control is the commitment of the manufacturer, but after medicinal products become part of the distribution and pharmacy network, analytical quality control is carried out within the program for Market Surveillance. There are different approaches in conducting quality control of medicinal products under the Market Surveillance Program. Aim: The aim of the study is to compare the results obtained under two approaches: individual testing and testing by groups with the same active substance. Methods: In this study, comparative tests for assay and purity were carried out within two groups of medicinal products from the antihypertensive group containing Amlodipine besilate and Valsartan. Analyses were performed in accordance with the available pharmacopoeial monographs, as well as those from literature sources. Results: The results from the assay tests show a significant difference in the same product tested. Analytical methods for the determination of impurities also show different results when analyzing the same medicinal product. Conclusion: Considering the performed analytical tests, the obtained results can be used to make several conclusions and suggestions concerning the optimisation of the Annual Market Surveillance Program

scholarly journals Spectrophotometric determination of neomycin sulphate in tablets form via reaction with ninhydrin reagent

2019 ◽  
Vol 10 (2) ◽  
pp. 1392-1396 ◽  
Author(s):  
Khalaf F Alsamarrai ◽  
Menaa Abdulsalam Al-Abbasi ◽  
Eman Thiab Alsamarrai
Keyword(s):  
Spectrophotometric Determination ◽  
Spectrophotometric Method ◽  
Calibration Curve ◽  
Limit Of Detection ◽  
Basic Medium ◽  
Optimal Conditions ◽  
Limit Of Quantification ◽  
Maximum Absorbance ◽  
Ninhydrin Reagent

A new, sensitive, simple and cheap spectrophotometric method for the determination of Neomycin Sulphate (NEO) in pharmaceutical forms has been developed. The method is based on the reaction between NEO and NIN in basic medium. The maximum absorbance was at 574 nm. The conditions affecting the reaction were optimized. Under the optimal conditions, the calibration curve was linear over the range of 0.0002-0.0011 mol/L. The limit of detection and limit of quantification were 5.423×10-6 mol/L, and 1.643×10-5 mol/L, RSD% of seven replicate was 0.8217- 0.8321% and Rec% was between 99.2168-100.8857%. The proposed method was successfully applied to the determination of NEO tablets form.

scholarly journals Quantitative determination of trifuzol in the 2.5% injection solution by spectrophotometric method

2020 ◽  
pp. 64-71
Author(s):  
N. N. Borisenko ◽  
K. P. Medvedev ◽  
S. A. Vasyuk ◽  
I. V. Bushueva ◽  
V. V. Parchenko
Keyword(s):  
Quality Control ◽  
Quantitative Determination ◽  
Medicinal Products ◽  
Injection Solution ◽  
Working Standard ◽  
Total Uncertainty ◽  
Anti Inflammatory ◽  
Development And Validation ◽  
Veterinary Medicinal Products

The effectiveness of the treatment of common diseases of the respiratory system, hematopoietic system, digestive system of livestock and domestic animals with the help of existing drugs is not always sufficient, and there is an urgent need to expand the arsenal of domestic veterinary medicinal products that would exhibit antiviral, anti-inflammatory and low toxicity, prompted to search, create and improve existing veterinary medicines. A medicine in the form of a 2.5% injection solution containing, as an active substance, a 1,2,4-triazole derivative – piperidine 2-[5-(furan-2-yl)-4-phenyl-1,2,4-triazole-3-ylthio] acetate exhibits a fairly high level of anti-inflammatory, antiviral, and immunomodulating effects. The arsenal of domestic veterinary drugs with the above activity is currently limited. The analysis of veterinary medicinal products is the most important stage in the system for ensuring the quality control of medicinal products. During the entire storage period of the drug, various methods of identification and quantification of the active substances are needed. And despite the fact that spectrophotometry in the UV region is not very specific and selective, the expressness of these methods allows them to be widely used for routine quality control of drugs. Development and validation of a method for the quantitative determination of trifuzole in a 2.5% injection solution according to its own absorption. The study used a working standard sample of trifuzol 2.5% injection solution of trifuzol, as a solvent – purified water. Analytical equipment: Specord 200 spectrophotometer, electronic balance AVT-120-5DM. The aim of our work was the development and validation of a new, express method for the quantitative determination of trifuzol in the composition of a 2.5% injection solution in the UV region. The proposed method is based on measuring the optical density of an aqueous solution of a compound at 278 nm. The technique was successfully validated for such characteristics as linearity, precision, correctness, specificity and robustness, according to the requirements of HFCs. The analysis of the predicted total uncertainty of the analysis showed the reproduction of the method and the possibility of its application in other laboratories. The validation of the method for the quantitative determination of trifuzol in the composition of a 2.5% injection solution according to the requirements of HFCs was carried out. It is proved that according to such validation characteristics as linearity, specificity, precision, correctness and robustness, the technique is correct.

The titanometric determination of azobenzene derivatives in mixed acetonitrile-methanol-water medium

1982 ◽  
Vol 47 (2) ◽  
pp. 495-502 ◽  
Author(s):  
Jiří Barek ◽  
Antonín Berka ◽  
Vladimír Borek
Keyword(s):  
Potentiometric Titration ◽  
Sodium Citrate ◽  
Azo Compounds ◽  
Water Medium ◽  
Optimal Conditions ◽  
Azobenzene Derivatives ◽  
Trivalent Titanium

The possibility of titanometric determination of a number of azobenzene derivatives in a mixed acetonitrile-methanol-water medium, which ensures sufficient solubility of the substances determined, was studied. Trivalent titanium in the presence of sodium citrate was found to be optimal. Conditions were found for the automatic potentiometric titration of a number of azo-compounds using this reagent.

Liquid–liquid extraction and cloud point extraction for spectrophotometric determination of vanadium using 4-(2-pyridylazo)resorcinol

2015 ◽  
Vol 69 (4) ◽  
Author(s):  
Teodora S. Stefanova ◽  
Kiril K. Simitchiev ◽  
Kiril B. Gavazov
Keyword(s):  
Cloud Point ◽  
Spectrophotometric Determination ◽  
Cloud Point Extraction ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Liquid Extraction ◽  
Optimal Conditions ◽  
Liquid Liquid Extraction ◽  
Relative Standard

AbstractLiquid-liquid extraction (LLE) and cloud point extraction (CPE) of vanadium(V) ternary complexes with 4-(2-pyridylazo)resorcinol (PAR) and 2,3,5-triphenyl-2H-tetrazolum chloride (TTC) were investigated. The optimal conditions for vanadium extraction and spectrophotometric determination were identified. The composition (V : PAR : TTC) of the extracted species was 1 : 2 : 3 (optimal conditions; LLE), 2 : 2 : 2 (low reagents concentrations; LLE), 1 : 1 : 1 (short heating time; CPE), and 1 : 1 : 1 + 1 : 1 : 0 (optimal extraction conditions; CPE). LLE, performed in the presence of 1,2-diaminocyclohexane-N,N,N’,N’-tetraacetic acid and NH4F as masking agents, afforded the sensitive, selective, precise, and inexpensive spectrophotometric determination of vanadium. The absorption maximum, molar absorptivity, limit of detection, and linear working range were 559 nm, 1.95 × 105 dm3 mol−1 cm−1, 0.7 ng cm−3, and 2.2-510 ng cm−3, respectively. The procedure thus developed was applied to the analysis of drinking waters and steels. The relative standard deviations for V(V) determination were below 9.4 % (4-6 × 10−7 mass %; water samples) and 2.12 % (1-3 mass %; steel samples).

scholarly journals СПЕКТРОФОТОМЕТРИЧНЕ ВИЗНАЧЕННЯ КАРВЕДІЛОЛУ В ТАБЛЕТКАХ

2015 ◽  
Author(s):  
Ю. М. Жук ◽  
С. О. Васюк ◽  
І. С. Верьовкіна
Keyword(s):  
Spectrophotometric Determination ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Spectrophotometric Analysis ◽  
Pharmaceutical Drugs ◽  
Optimal Conditions ◽  
Colored Product ◽  
Medical University ◽  
Adrenergic Blocking

<p><strong>SPECTROPHOTOMETRIC DETERMINATION OF CARVEDILOL IN TABLETS</strong></p><p><strong>Y. Zhuk, S. Vasjuk, I. Ver</strong><strong>оvkina</strong></p><p>Zaporozhye State Medical University, Zaporozhye</p><p><strong>Summary:</strong> in this investigation a visible spectrophotometric method for the determination of carvedilol based on the absorbance of colored product of the reaction between carvedilol and bromcresol purple in acetone medium at 399 nm measurement was developed. The optimal conditions for the quantitative determination of carvedilol in the content of pharmaceutical drugs were established. The validation of the worked out procedure on such validated characteristics as linearity, precision, accuracy and robustness was carried out.</p><p><strong>Keywords:</strong> spectrophotometric analysis, carvedilol, bromcresol purple.</p><p><strong>Introduction. </strong>Carvedilol (1-(9H-carbazol-4-yloxy)-3-[2-(2-methoxyphenoxy)ethylamino]propan-2-2) belongs to a group of medicines called beta-adrenergic blocking agents, that are indicated for the treatment of hypertension angina pectoris and heart failure.</p><p>Our aim is to develop a simple, accurate and valid method for the spectrophotometric determination of carvedilol.</p><p>Purposes:</p><ul><li>establish optimal conditions of the photometric reaction between carvedilol and bromcresol purple;</li><li>develop the method for the determination of carvedilol in pharmaceutical formulations;</li><li>carry out validation of the worked out procedure.</li></ul><p><strong>Methods of analysis.</strong></p><p>Object of research: tablets «Corvazan» 25 mg (Arterium), tablets «Coriol» 12,5 mg (KRKA), tablets «Coriol» 25 mg (KRKA).</p><p>Reagents and Chemicals: standard solution of carvedilol, bromcresol purple, acetone. All reagents and chemicals used were of analytical grade.</p><p>Instrument: spectrophotometer Specord 200, electronic balance ABT-120-5PM, ultrasonic bath ELMASONIC 60Н.</p><p><strong>Results and discussion</strong>.</p><p>Linearity. The analytical parameters such as molar absorptivity, Beer’s law limits and Sandell’s sensitivity values were calculated.</p><p>Precision. The developed methods give the result with repeatability sufficient for dependable determination the investigated substance in pharmaceutical formulations.</p><p>Accuracy. Accuracy established by analyte addition technique.</p><p>Robustness. Determined factors that influence on the absorbance value: reagent quantity and timing stability.</p><p>Sample solutions stable during 30 min.</p><p>Addition to sample solution ±10 % bromcresol purple solution is not change the absorbance value.</p><p><strong>Conclusions. </strong>Established that reaction between carvedilol and bromcresol purple proceeds in acetone medium at room temperature.</p><p>Molar absorption coefficient is 2,13·10<sup>4</sup>.<strong></strong></p><p>Developed the method of spectrophotometric determination of carvedilol in pharmaceutical formulations.</p><p>Proved that the method is valid on such validated characteristics as linearity, precision, accuracy and robustness. </p>

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