Development and Validation of an analytical method for the determination of Ofloxacin and Benzyl alcohol in a Pharmaceutical mixture

2021 ◽  
pp. 2133-2138
Author(s):  
Ghadeer Balloul ◽  
Nikolay N. Boyko ◽  
Elena T. Zhilyakova ◽  
Solaiman Doba
Keyword(s):  
Benzyl Alcohol ◽  
Linear Dependence ◽  
Low Cost ◽  
Correlation Coefficients ◽  
Analytical Signal ◽  
Pure Substance ◽  
Apparent Concentration ◽  
Proportional Relationship ◽  
Development And Validation

The aim of the study is to develop a validated, rapid, simple and low-cost method for estimating ofloxacin and benzyl alcohol in a combined dosage. Materials and methods: Materials which were used ofloxacin pure substance and benzyl alcohol pure substance which were determined by UV spectrophotometer using ethanol 95% as a solvent and a blank. Results and discussion: Ofloxacin shows the absorption maxima at 300.0 ± 2.0 nm in ethanol 95% with an apparent concentration absorptivity of (30 to 90) µg/ml and benzyl alcohol shows the absorption maxima at 312.0 ± 2.0 nm in ethanol 95% with an apparent concentration absorptivity of (60 to 200) µg/ml, it was found that in the selected range of application of the method there is a directly proportional relationship between the concentration of ofloxacin and benzyl alcohol respectively, in the measured samples and the analytical signal, linear dependence is characterized by high correlation coefficients (R> 0.999)for both of drugs, which is considered acceptable for establishing strict linearity. Conclusion: The method has been verified as it has been proven simple, fast, accurate and low-cost method and does not require any expensive equipment for the analysis of Ofloxacin and benzyl alcohol separately and in a pharmaceutical mixture.

Development and Validation of an Eco-Friendly and Low-Cost Method for the Quantification of Cefepime Hydrochloride in Powder for Injectable Solution Using Infrared (IR) Spectroscopy

2020 ◽  
Vol 16 (4) ◽  
pp. 456-464
Author(s):  
Danilo F. Rodrigues ◽  
Hérida R.N. Salgado
Keyword(s):  
Ir Spectroscopy ◽  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Potassium Bromide ◽  
Pharmaceutical Products ◽  
Injectable Formulation ◽  
Ich Guidelines ◽  
Lactam Ring ◽  
Development And Validation

Background: A simple, eco-friendly and low-cost Infrared (IR) method was developed and validated for the analysis of Cefepime Hydrochloride (CEF) in injectable formulation. Different from some other methods, which employ organic solvents in the analyses, this technique does not use these types of solvents, removing large impacts on the environment and risks to operators. Objective: This study aimed at developing and validating a green analytical method using IR spectroscopy for the determination of CEF in pharmaceutical preparations. Methods: The method was validated according to ICH guidelines and the quantification of CEF was performed in the spectral region absorbed at 1815-1745 cm-1 (stretching of the carbonyl group of β- lactam ring). Results: The validated method showed to be linear (r = 0.9999) in the range of 0.2 to 0.6 mg/pellet of potassium bromide, as well as for the parameters of selectivity, precision, accuracy, robustness and Limits of Detection (LOD) and Quantification (LOQ), being able to quantify the CEF in pharmaceutical preparations. The CEF content obtained by the IR method was 103.86%. Conclusion: Thus, the method developed may be an alternative in the quality control of CEF sample in lyophilized powder for injectable solution, as it presented important characteristics in the determination of the pharmaceutical products, with low analysis time and a decrease in the generation of toxic wastes to the environment.

scholarly journals Development and Validation of an UHPLC Method for Ostarine Determination in Dietary Supplements

2019 ◽  
Vol 65 (2) ◽  
pp. 49-54
Author(s):  
Amalia Miklos ◽  
Amelia Tero-Vescan ◽  
Lénárd Farczádi ◽  
Daniela-Lucia Muntean
Keyword(s):  
Quantitative Determination ◽  
Dietary Supplements ◽  
Low Cost ◽  
Reversed Phase ◽  
European Pharmacopoeia ◽  
Average Mass ◽  
7Th Edition ◽  
Development And Validation ◽  
Mg Content

AbstractObjective: The purpose of this study was to develop a low-cost, yet sensitive and precise UHPLC method for the quantitative determination of ostarine from dietary supplements (DS) for athletes. The analytical performance of the method was verified on a DS legally acquired from a specialized website for athletes. The uniformity of mass and content of the ostarine DS was also verified.Methods: For the quantitative determination of ostarine a UHPLC method was developed and validated. The separation was performed using a reversed-phase C18 column, using a mixture of 75% methanol: 25% formic acid 0.1% in isocratic elution, at a flow rate of 0.5 ml/min. The uniformity of mass and content of DS was performed following the methodology described in the European Pharmacopoeia 7th Edition.Results: The validated method was specific and linear on the concentration range of 1-25 µg/ml and was precise and accurate at all concentration levels, according to the official guidelines for validating analytical methods. An average mass of 510 mg content was obtained for the ostarine capsules, with an RSD of 2.41%. Regarding the uniformity of the content, an average of 4.65 mg ostarine/capsule was obtained with an RSD of 1.05%.Conclusions: The developed UHPLC method was suitable, rapid, sensitive and allowed quantitative determination of active substance content in a DS with ostarine (92.91% ostarine/capsule from 5 mg ostarine/capsule declared by the manufacturer).

scholarly journals Spectrophotometric and Smartphone-Assisted Determination of Phenolic Compounds Using Crude Eggplant Extract

Molecules ◽  
2019 ◽  
Vol 24 (23) ◽  
pp. 4407 ◽  
Author(s):  
M.A. Morosanova ◽  
A.S. Bashkatova ◽  
E.I. Morosanova
Keyword(s):  
Phenolic Compounds ◽  
Chlorogenic Acid ◽  
Caffeic Acid ◽  
Polyphenol Oxidase ◽  
Oxidase Activity ◽  
Biological Fluids ◽  
Low Cost ◽  
Analytical Signal ◽  
Polyphenol Oxidase Activity

In order to develop a simple, reliable and low cost enzymatic method for the determination of phenolic compounds we studied polyphenol oxidase activity of crude eggplant (S. melongena) extract using 13 phenolic compounds. Catechol, caffeic and chlorogenic acids, and L-DOPA have been rapidly oxidized with the formation of colored products. Monophenolic compounds have been oxidized at a much slower speed. Ferulic acid, quercetin, rutin, and dihydroquercetin have been found to inhibit polyphenol oxidase activity of crude eggplant extract. The influence of pH, temperature, crude eggplant extract amount, and 3-methyl-2-benzothiazolinone hydrazone (MBTH) concentration on the oxidation of catechol, caffeic acid, chlorogenic acid, and L-DOPA has been investigated spectrophotometrically. Michaelis constants values decrease by a factor of 2 to 3 in the presence of MBTH. Spectrophotometric (cuvette and microplate variants) and smartphone-assisted procedures for phenolic compounds determination have been proposed. Average saturation values (HSV color model) of the images of the microplate wells have been chosen as the analytical signal for smartphone-assisted procedure. LOD values for catechol, caffeic acid, chlorogenic acid, and L-DOPA equaled 5.1, 6.3, 5.8 and 30.0 µM (cuvette procedure), 12.2, 13.2, 13.2 and 80.4 µM (microplate procedure), and 23.5, 26.4, 20.8 and 120.6 µM (smartphone procedure). All the variants have been successfully applied for fast (4-5 min) and simple TPC determination in plant derived products and L-DOPA determination in model biological fluids. The values found with smartphone procedure are in good agreement with both spectrophotometric procedures values and reference values. Using crude eggplant extract- mediated reactions combined with smartphone camera detection has allowed creating low-cost, reliable and environmentally friendly analytical method for the determination of phenolic compounds.

scholarly journals Validation of analytical method for determination of furosemide in extemporaneous syrup

2017 ◽  
Author(s):  
D. Alfred-Ugbenbo ◽  
O. A. Zdoryk ◽  
V. A. Georgiyants
Keyword(s):  
Sodium Hydroxide Solution ◽  
Correlation Coefficients ◽  
Active Pharmaceutical Ingredient ◽  
Stability Study ◽  
Assay Method ◽  
Pure Substance ◽  
Ultraviolet Region ◽  
Validation Parameters ◽  
Development And Validation ◽  
Medicinal Drugs

Introduction. Extreme syrups can be manufactured using substances or ready medicinal drugs as the active pharmaceutical ingredient. There is a necessity in the development and validation of analytical methods that can be used for quality control of pharmaceutical manufacturing of syrups containing furosemide.The aim of the study – to develop and validate assay method for furosemide in extemporaneous syrups prepared from both pure substance and finished products. Methods of the research. For proposed UV spectrophotometric assay method the conditions of analysis, sample preparation and validation characteristics were defined. Suspensions of substance and crushed commercial tablets were dissolved in 0.1 M sodium hydroxide solution and evaluated spectrophotometrically in ultraviolet region of light at a wavelength 271 nm using method of specific absorbance.Results and Discussion. Samples comply with the Beer-Lambert Bouguer law within the concentration range of 8×10-3 – 1.2×10-2 mg/ml with correlation coefficients ≥ 0.9981. The uncertainty of the methods was well within the critical value of the error (0.72 %≤ maxΔAs) for both samples of syrup containing pure substance and commercial tablets. Recovery studies for furosemide in syrup samples of substance and crushed commercial tablets yielded 99.92 ±0.54 % and 99.14±0.16 % respectively. Assay limit of ±10 % by the validation parameters: specificity, linearity, precision, accuracy within the range of 80–120 % of the nominal contents was met by all compounded preparations.Conclusions. The results of validation proved that this method can be reproduced correctly and is suitable for use in pharmaceutical analysis. Adoption of this method is planned in evaluating uniformity of content and, in combination of other methods, ascertain chemical stability study of compounded furosemide syrups.

scholarly journals Quantitative Analysis of Eugenol in Clove Extract by a Validated HPLC Method

2010 ◽  
Vol 93 (6) ◽  
pp. 1806-1810 ◽  
Author(s):  
So-Mi Yun ◽  
Myoung-Heon Lee ◽  
Kwang-Jick Lee ◽  
Hyun-Ok Ku ◽  
Seong-Wan Son ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Marker Compound ◽  
Safety Assurance ◽  
Chemical Evaluation ◽  
Array Detection ◽  
Digestive Disorders ◽  
Development And Validation

Abstract Clove (Eugenia caryophyllata) is a well-known medicinal plant used for diarrhea, digestive disorders, or in antiseptics in Korea. Eugenol is the main active ingredient of clove and has been chosen as a marker compound for the chemical evaluation or QC of clove. This paper reports the development and validation of an HPLC-diode array detection (DAD) method for the determination of eugenol in clove. HPLC separation was accomplished on an XTerra RP18 column (250 4.6 mm id, 5m) with an isocratic mobile phase of 60 methanol and DAD at 280 nm. Calibration graphs were linear with very good correlation coefficients (r2 > 0.9999) from 12.5 to 1000 ng/mL. The LOD was 0.81 and the LOQ was 2.47 ng/mL. The method showed good intraday precision (RSD 0.080.27) and interday precision (RSD 0.321.19). The method was applied to the analysis of eugenol from clove cultivated in various countries (Indonesia, Singapore, and China). Quantitative analysis of the 15 clove samples showed that the content of eugenol varied significantly, ranging from 163 to 1049 ppb. The method of determination of eugenol by HPLC is accurate to evaluate the quality and safety assurance of clove, based on the results of this study.

A New Green Method for the Quantitative Analysis of Enrofloxacin by Fourier-Transform Infrared Spectroscopy

2018 ◽  
Vol 101 (6) ◽  
pp. 2001-2005 ◽  
Author(s):  
Camila Tavares Rebouças ◽  
Ana Carolina Kogawa ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Quantitative Analysis ◽  
Fourier Transform Infrared Spectroscopy ◽  
Low Cost ◽  
Bacterial Species ◽  
Correlation Coefficients ◽  
Fourier Transform Infrared ◽  
Green Method

Abstract Background: A green analytical chemistry method was developed for quantification of enrofloxacin in tablets. The drug, a second-generation fluoroquinolone, was first introduced in veterinary medicine for the treatment of various bacterial species. Objective: This study proposed to develop, validate, and apply a reliable, low-cost, fast, and simple IR spectroscopy method for quantitative routine determination of enrofloxacin in tablets. Methods: The method was completely validated according to the International Conference on Harmonisation guidelines, showing accuracy, precision, selectivity, robustness, and linearity. Results: It was linear over the concentration range of 1.0–3.0 mg with correlation coefficients >0.9999 and LOD and LOQ of 0.12 and 0.36 mg, respectively. Conclusions: Now that this IR method has met performance qualifications, it can be adopted and applied for the analysis of enrofloxacin tablets for production process control. The validated method can also be utilized to quantify enrofloxacin in tablets and thus is an environmentally friendly alternative for the routine analysis of enrofloxacin in quality control. Highlights: A new green method for the quantitative analysis of enrofloxacin by Fourier-Transform Infrared spectroscopy was validated. It is a fast, clean and low-cost alternative for the evaluation of enrofloxacin tablets.

scholarly journals Development and Validation of an Autonomous System for Measurement of Sunshine Duration

Sensors ◽  
2020 ◽  
Vol 20 (16) ◽  
pp. 4606
Author(s):  
Álvaro B. da Rocha ◽  
Eisenhawer de M. Fernandes ◽  
Carlos A. C. dos Santos ◽  
Júlio M. T. Diniz ◽  
Wanderley F. A. Junior
Keyword(s):  
Sunshine Duration ◽  
Low Cost ◽  
Electronic System ◽  
Operational Amplifiers ◽  
Solar Panels ◽  
Calculation Methods ◽  
Contrast Method ◽  
Microcontroller Unit ◽  
Development And Validation

This paper presented an autonomous electronic system for sunshine duration (SD) monitoring based on the contrast method and developed to operate on a horizontal surface. The prototype uses four photoresistors arranged at 90° in a 20 mm diameter circumference separated by a shading structure used to create a shadow pattern on the detection element. Photoresistors are inserted in individual signal conditioning circuits based on the association between Wheatstone bridges and operational amplifiers to provide an analog signal to the microcontroller unit. The determination of SD occurs through the implementation of fuzzy logic with numerical calculation methods to estimate the probability (f) of solar disk obstruction and estimate SD values. The system does not require additional adjustments after installation or use of energy sources for operation due to the use of an internal battery with charge recovery by solar panels. Experimental results of the proposed system were validated with the ones provided by a government meteorology station. Statistical analysis of the results showed a confidence index (c) greater than 90%, with a precision of 94.26%. The proposed system is a feasible low-cost solution to the available commercial systems for the measurement of sunshine duration.

DEVELOPMENT AND VALIDATION OF UV SIMULTANEOUS EQUATION METHOD FOR DETERMINATION OF AZITHROMYCIN AND LEVOFLOXACIN IN BULK DRUGS AND MARKETED FORMULATION

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 51-56
Author(s):  
S Kamepalli ◽  
◽  
J Pachipanta ◽  
A. K. Pathan ◽  
B. S. S. Naik
Keyword(s):  
Calibration Curve ◽  
Bacterial Infections ◽  
Uv Spectroscopy ◽  
Correlation Coefficients ◽  
Simultaneous Equation ◽  
Simultaneous Equations ◽  
Absorbance Maximum ◽  
Ich Guidelines ◽  
Development And Validation

Azithromycin and levofloxacin used for the treatment of bacterial infections. Simple, specific, accurate and precise UV spectroscopy method has been developed and validated for simultaneous determination of azithromycin and levofloxacin in bulk drugs and marketed formulation. The developed method involves solving of simultaneous equations using methanol as solvent where an absorbance maximum for azithromycin and levofloxacin was found to be at 291.92nm and 294.08nm, respectively. The drugs obeyed Beer’s law in the concentration range of 50- 250 μg/ mL & 2 – 10 μg/ mL. The method was validated as per ICH guidelines .The method showed good correlation coefficients (r2) 0.999, indicated good linearity of calibration curve for both the drugs. The recovery of azithromycin and levofloxacin was 98.82% and 97 .74% respectively. The robustness and ruggedness of azithromycin (0.368, 0.285), and levofloxacin (0.556, 0.442). The developed method was found to be accurate, reliable, robust showing LOD 0.012μg/mL and 0.016μg/mL LOQ 0.053μg/mL and 0.058μg/mL for azithromycin and levofloxacin.

scholarly journals TLC-Densitometric Determination of Five Coxibs in Pharmaceutical Preparations

Processes ◽  
2020 ◽  
Vol 8 (5) ◽  
pp. 620
Author(s):  
Paweł Gumułka ◽  
Monika Dąbrowska ◽  
Małgorzata Starek
Keyword(s):  
Low Cost ◽  
Pharmaceutical Preparations ◽  
Correlation Coefficients ◽  
Relieve Pain ◽  
Ich Guidelines ◽  
Wide Range ◽  
Densitometric Detection ◽  
Cox 2 ◽  
Cox 2 Inhibitors

A class of drugs called coxibs (COX-2 inhibitors) were created to help relieve pain and inflammation of osteoarthritis and rheumatoid arthritis with the lowest amount of side effects possible. The presented paper describes a new developed, optimized and validated thin layer chromatographic (TLC)-densitometric procedure for the simultaneous assay of five coxibs: celecoxib, etoricoxib, firecoxib, rofecoxib and cimicoxib. Chromatographic separation was conducted on HPTLC F254 silica gel chromatographic plates as a stationary phase using chloroform–acetone–toluene (12:5:2, v/v/v) as a mobile phase. Densitometric detection was carried out at two wavelengths of 254 and 290 nm. The method was tested according to ICH guidelines for linearity, recovery and specificity. The presented method was linear in a wide range of concentrations for all analyzed compounds, with correlation coefficients greater than 0.99. The method is specific, precise (%RSD < 1) and accurate (more than 95%, %RSD < 2). Low-cost, simple and rapid, it can be used in laboratories for drug monitoring and quality control.

Development and Validation of One-Step Ultrasound-Assisted Extraction for Simultaneous Determination of Multiclass Fungicides in Soils

2015 ◽  
Vol 98 (1) ◽  
pp. 192-200
Author(s):  
Yared Merdassa ◽  
Jing-fu Liu ◽  
Negussie Megersa
Keyword(s):  
Correlation Coefficients ◽  
Sonication Time ◽  
Ultrasound Assisted Extraction ◽  
Extraction Solvent ◽  
Assisted Extraction ◽  
One Step ◽  
Ultrasound Assisted ◽  
Wavelength Detection ◽  
Development And Validation

Abstract A rapid, efficient, and simple one-step ultrasound-assisted extraction (UAE) method was developed forthe analysis of seven fungicides (cymoxanil, metalaxyl, mandipropamid, folpet, chlorothalonil, kresoxim-methyl, and famoxadone) in horticultural soils. Analytes in the samples were determined by HPLC with variable wavelength detection. Key parameters that influence the UAE procedure were optimized, such as the nature and volume of extraction solvent, number of sonication steps, and sonication time. The highest extraction efficiencies in the range of 61.1–87.8% were obtained by using only 7.5 mL of ethyl acetate–hexane (1 + 1, v/v) and sonicating for 10 min. At 0.5 and 2.0 μg/g fortification levels, satisfactory recoveries (&gt;60%) with RSD &lt;13% were obtained for each analyte, except for folpet (&gt;52%). The method was linear over the range of 0.005 to 10 μg/g and the correlation coefficients (r2) obtained ranged from 0.9955 to 0.9992. The LODs (S/N = 3) varied from 0.0015 to 0.006 μg/g. The proposed UAE procedure was compared to classical extractions (shake-flask and Soxhletextraction) and showed satisfactory extraction efficiencies using shorter time and smaller amounts of organic solvents, thereby minimizing the costs of the analysis and the disposal of waste solvent.

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