scholarly journals GREEN ANALYTICAL METHOD FOR QUANTIFICATION OF SECNIDAZOLE IN TABLETS BY HPLC-UV

2018 ◽  
Vol 2 (2) ◽  
pp. 20-26
Author(s):  
Jéssica Lima ◽  
Ana Kogawa ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Analytical Chemistry ◽  
Particle Size ◽  
Analytical Method ◽  
Mobile Phase ◽  
Toxic Waste ◽  
Green Analytical Chemistry ◽  
Injection Volume ◽  
As Stress ◽  
Routine Quality Control

A simple, rapid, economic and green analytical method was validated for the determination of secnidazole in tablets. The aim was to contribute to the green analytical chemistry since it has low use of organic solvent and low production of toxic waste. For the HPLC-UV method, the mobile phase was a mixture of purified water + 0.7 % acetic acid and ethanol (78:22, v/v), flow rate was 1.3 mL min-1 on column CN Phenomenex Luna (250 x 4.60 mm, 5 μm particle size), injection volume was 20 μL with UV detection at 318 nm and retention time of 4.26 minutes. The method was linear over the concentration range of 5-100 μg mL-1 (r = 0.9998) with limits of detection and quantitation of 0.533 e 1.615 μg mL-1, respectively. The precision of the method showed RSD less than 2 %. The accuracy determined by the average recoveries was 99.58 %. The secnidazole tablets were subjected to oxidation, acid, alkaline, neutral and photolysis degradation as stress conditions and the method was considered as indicative of stability. The method is adequate and safe to be a great alternative method in routine quality control analyzes for determination and quantification of secnidazole tablets.

scholarly journals ECO-FRIENDLY GREEN LIQUID CHROMATOGRAPHIC FOR DETERMINATION OF DOXYCYCLINE IN TABLETS AND IN THE PRESENCE OF ITS DEGRADATION PRODUCTS

2018 ◽  
Vol 2 (2) ◽  
pp. 49-55
Author(s):  
Loren Ghidini ◽  
Ana Kogawa ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Analytical Chemistry ◽  
Quality Control ◽  
Degradation Products ◽  
Toxic Waste ◽  
Green Analytical Chemistry ◽  
Photolytic Degradation ◽  
Liquid Chromatographic ◽  
Detection And Quantification ◽  
Routine Quality Control

Doxycycline, an oral antimicrobial, does not present a sustainable analytical method described in the literature using liquid chromatography. A new and efficient method was developed and validated for the quantification of doxycycline tablets by HPLC-UV. Its aim is the contribution to the green analytical chemistry since it has low use of organic solvent and low production of toxic waste. The HPLC-UV method used a mixture of purified water + 0.5 % acetic acid and ethanol (40:60, v/v). The flow rate was 0.8 mL min-1, C18 Luna column, 20 μL of injected volumes at 275 nm. The samples were prepared in purified water and the method was linear over the concentration range of 20–200 μg mL-1 (r = 0.9997) with limits of detection and quantification of 1.08 and 3.27 μg mL-1, respectively. The precision of the method showed RSD 0.50 % (intra-assay), 2.35 % (inter-assay) and 1.13 % (between analysts). The accuracy of the method was determined by standard recovery and it was 99.85 %. The DOX tablets were subjected to oxidative, acid, basic, neutral and photolytic degradation and it showed be stability indicative. Statistical analysis provided reliable, safety and reproducible results. The method is considered linear, selective, precise, accurate, robust, indicative of stability and safe to be used in routine quality control analyzes for determination and quantification of doxycycline in tablets. The proposed method is an ecologically correct alternative for the evaluation of doxycycline tablets.

scholarly journals NEW, GREEN AND MINIATURIZED ANALYTICAL METHOD FOR DETERMINATION OF CEFADROXIL MONOHYDRATE IN CAPSULES

2019 ◽  
Vol 3 (1) ◽  
pp. 23-28 ◽  
Author(s):  
Bianca Marco ◽  
Ana Kogawa ◽  
Hérida Salgado
Keyword(s):  
Analytical Chemistry ◽  
Standard Sample ◽  
Low Cost ◽  
Visible Region ◽  
Hplc Method ◽  
Minimal Amount ◽  
Green Analytical Chemistry ◽  
Color Reagent ◽  
Routine Quality Control

Cefadroxil, an oral antimicrobial, presents few techniques optimized for the reduction of solvents and toxic residues and/or non-use of them. So, a quantitative, new and miniaturized method for determination of cefadroxil monohydrate in capsules has been developed and validated by spectrophotometric method in the visible region according to the international guidelines. The analyzes were performed using microplates containing 96 wells, 1 % of phenolphthalein and sodium hydroxide 0.1 M as reagent at 552 nm. The method was (i) linear in the range of 15-115 µg mL-1, (ii) selective when comparing standard, sample, adjuvants and color reagent, (iii) precise with deviations below 4 %, (iv) accurate when comparing the proposed method with the HPLC method, (v) robusts by making small and deliberate modifications to the method, (vi) besides being fast, low cost, eco-friendly and generates minimal amount of waste. The method can be applied to the routine quality control of cefadroxil monohydrate in capsules and an effective and accessible alternative that contemplates the concepts of current and sustainable green analytical chemistry.

scholarly journals Comprehensive Assessment of Flow and Other Analytical Methods Dedicated to the Determination of Zinc in Water

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3914
Author(s):  
Paweł Kościelniak ◽  
Paweł Mateusz Nowak ◽  
Joanna Kozak ◽  
Marcin Wieczorek
Keyword(s):  
Analytical Chemistry ◽  
Green Chemistry ◽  
Analytical Method ◽  
Analytical Methods ◽  
Green Analytical Chemistry ◽  
General Quality ◽  
Analytical Strategies ◽  
High Degree

An original strategy to evaluate analytical procedures is proposed and applied to verify if the flow-based methods, generally favorable in terms of green chemistry, are competitive when their evaluation also relies on other criteria. To this end, eight methods for the determination of zinc in waters, including four flow-based ones, were compared and the Red–Green–Blue (RGB) model was exploited. This model takes into account several features related to the general quality of an analytical method, namely, its analytical efficiency, compliance with the green analytical chemistry, as well as practical and economic usefulness. Amongst the investigated methods, the best was the flow-based spectrofluorimetric one, and a negative example was that one involving a flow module, ICP ionization and MS detection, which was very good in analytical terms, but worse in relation to other aspects, which significantly limits its overall potential. Good assessments were also noted for non-flow electrochemical methods, which attract attention with a high degree of balance of features and, therefore, high versatility. The original attempt to confront several worldwide accepted analytical strategies, although to some extent subjective and with limitations, provides interesting information and indications, establishing a novel direction towards the development and evaluation of analytical methods.

A New Ecological HPLC Method for Determination of Vancomycin Dosage form

2020 ◽  
Vol 7 (2) ◽  
pp. 82-90
Author(s):  
Patricia Aleixa do Nascimento ◽  
Ana Carolina Kogawa ◽  
Hérida R.N. Salgado
Keyword(s):  
Analytical Chemistry ◽  
Quality Control ◽  
Acetic Acid ◽  
Dosage Form ◽  
Uv Light ◽  
Hplc Method ◽  
Green Analytical Chemistry ◽  
Vancomycin Dosage ◽  
Routine Quality Control

Aims: To develop and validate a new ecological HPLC method for the determination of vancomycin dosage form. Background: Vancomycin is an important antimicrobial. According to the literature, there are many methods that use HPLC, but none of these methods follow the green analytical chemistry principles. Objective: Therefore, a green analytical method to quantify vancomycin in lyophilized powder for injectable solution by HPLC was developed. Materials and Methods: It uses less quantity of toxic solvents, minimizing the costs and optimizing the time of analysis. Water + 0.1% acetic acid and ethanol (85:15, v/v), 0.5 mL min-1, and C18 column (15 cm) at 280 nm were used. Results and Discussion: The method was linear in the range of 40 to 140 μg mL-1, with a correlation coefficient of 0.9998. It was selective when subjected to acid 0.1M, basic 0.01M, oxidative 0.3%, UV light and neutral degradation in a bath of 60 ºC for 8 hours. The precision of the method was proved at intraday (RSD 1.08%), interday (RSD 0.47%) and intermediate levels (RSD 2.35%). It was accurate with a mean recovery of 100.19% and robust when changes were performed in seven parameters of the method and analyzed by the Youden and Steiner test. Conclusion: The method can be applied to routine quality control of vancomycin lyophilized powder for injectable solution as an ecological and sustainable alternative that contemplates the green analytical chemistry and the current pharmaceutical analyses.

A Green Liquid Chromatographic Method For The Simultaneous Determination of Chlorpheniramine Maleate, Pseudoephedrine Hydrochloride and Propyphenazone

2019 ◽  
Vol 15 (6) ◽  
pp. 635-641
Author(s):  
Nadia M. Mostafa ◽  
Ghada M. Elsayed ◽  
Nagiba Y. Hassan ◽  
Dina A. El Mously
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Green Analytical Chemistry ◽  
Chlorpheniramine Maleate ◽  
Accuracy And Precision ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Background:The concept of green analytical chemistry prevails due to the growing environmental pollution.Objective:Our attempts are to develop simple and eco-friendly method which is non-harmful to the environment by producing minimal waste. In this context, a green liquid chromatographic method was applied for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride and propyphenazone in their combined dosage form.Methods:Separation was carried out using X select HSS RP C18 analytical column (250 × 4.6 mm, 5μm) using methanol - 0.02 M phosphate buffer pH 3 - triethylamine (60:40: 0.1, by volume) as a mobile phase. The separated peaks were detected at 215 nm at a flow rate 1.0 mL/min.Results:Quantification was done over the concentration ranges of 1-25 µg/mL for chlorpheniramine maleate, 5-35 µg/mL for pseudoephedrine hydrochloride and 10-120 µg/mL for propyphenazone. The suggested method was validated with regard to linearity, accuracy and precision according to the International Conference on Harmonization guidelines with good results.Conclusion:It could be used as a safer alternative for routine analysis of the mentioned drugs in quality control laboratories.

scholarly journals RAPID ANALYTICAL METHOD FOR ASSAY DETERMINATION FOR PROCHLORPERAZINE EDISYLATE DRUG SUBSTANCES BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY

2017 ◽  
Vol 9 (4) ◽  
pp. 118 ◽  
Author(s):  
Kishorkumar L. Mule
Keyword(s):  
Liquid Chromatography ◽  
Trifluoroacetic Acid ◽  
Analytical Method ◽  
Mobile Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Drug Substance ◽  
Assay Method ◽  
Column Temperature ◽  
Drug Substances

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry. 

scholarly journals HPLC determination of hydrochlorothiazide in urine after solid-phase extraction

2005 ◽  
Vol 51 ◽  
pp. 23-28 ◽  
Author(s):  
Violeta Ivanova ◽  
Dragica Zendelovska ◽  
Marina Stefova
Keyword(s):  
Particle Size ◽  
Solid Phase Extraction ◽  
Mobile Phase ◽  
Solid Phase ◽  
Hplc Method ◽  
Phase Extraction ◽  
Hplc Separation ◽  
Isocratic Elution ◽  
Extraction Recovery

A simple, rapid and precise HPLC method has been developed for the assay of hydrochlorothiazide in urine. The clean-up of the urine samples was carried out by solid-phase extraction using HLB cartridges. Extraction recovery was 94.00-100.28 %. HPLC separation was performed with isocratic elution on Hypersil BDS C18 column (100 x 4.0 mm I.D., 3 µm particle size) protected with appropriate guard column. The mobile phase was 18 % acetonitrile and 0.025 mol/L solution of KH2PO4, pH 4 at flow rate of 0.3 mL/min. Detection of the substances was performed at 220 nm. The calibration curves were linear in the range of 2-50 µg/mL. The developed method is validated by checking its accuracy, precision and stability. The detection limit is 2 µg/mL hydrochlorothiazide. The method is proved to be convenient for routine analysis of hydrochlorothiazide in urine.

scholarly journals DETERMINATION OF 2-CYANO-4’-BROMOMETHYL BIPHENYL GENOTOXIC IMPURITY IN IRBESARTAN DRUG SUBSTANCES USING HPLC TECHNIQUE

2016 ◽  
Vol 8 (12) ◽  
pp. 225
Author(s):  
S. Senthil Kumar ◽  
Ritesh Kumar Srivastava ◽  
V. Srinivas Rao
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Development Activity ◽  
Validation Data ◽  
Column Temperature ◽  
Injection Volume ◽  
Drug Substances ◽  
Hplc Technique ◽  
Ich Guideline

<p><strong>Objective: </strong>The objective of present study was to develop and validate a specific and sensitive HPLC method for the quantitative determination of genotoxic impurity 2-cyano-4’-bromomethyl biphenyl present in irbesartan drug substance.</p><p><strong>Methods: </strong>The development activity was conducted by HPLC with UV as a detector. The impurity was separated on Kromasil C18 250 x 4.6 mm, 5 µm analytical column with a mobile phase consisting of buffer pH 3.2 and acetonitrile in the ratio of 60:40 v/v at a flow rate 1.5 ml/min. The effluent was monitored by UV detection at 258 nm with column temperature maintained at 40 °C and the injection volume 30 μl. Acetonitrile was selected as diluent.</p><p><strong>Results: </strong>Validation activity was planned and completed based on the ICH guideline. The LOD and LOQ value were found to be 0.167 µg/g and 0.506 µg/g and accuracy results were well in the range 98.34 to 103.46 %. The linearity curve showed the correlation coefficient of 0.9999 and method very sensitive.</p><p><strong>Conclusion: </strong>From validation data, it was confirmed that the developed method is specific, sensitive, linear, precise and accurate for the determination of 2-cyano-4’-bromomethyl biphenyl genotoxic impurity in irbesartan drug substances.</p>

Determination of the antidepressants maprotiline and amoxapine, and their metabolites, in plasma by liquid chromatography.

1983 ◽  
Vol 29 (2) ◽  
pp. 314-318 ◽  
Author(s):  
S H Wong ◽  
S W Waugh
Keyword(s):  
Particle Size ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
Peak Height ◽  
Reversed Phase ◽  
High Carbon ◽  
Phase Separations ◽  
Carbon Load ◽  
Interference Studies

Abstract Maprotiline, amoxapine, and their metabolites were determined in plasma by three separate procedures, each of which involves a three-step extraction followed by reversed-phase separations. Amoxapine, maprotiline, and N-desmethylmaprotiline can be measured with use of a conventional C-18 column with 10% carbon load, but analyses for 7- and 8-hydroxyamoxapines require a small (5-microns) particle size, high carbon load, 20% C-18 column with 0.2 mol/L phosphate as mobile phase. Within-run and day-to-day CVs were 5% and 8%, respectively. Peak-height ratios were linearly correlated with concentrations between 0 and 400 micrograms/L. Detection limits ranged from 1 to 3 ng. Interference studies indicated that nortriptyline co-elutes with maprotiline. Assays of patients' plasma showed substantial amounts of these drugs and most of their metabolites, but only trace amounts of 7-hydroxyamoxapine.

scholarly journals Implementing Green Analytical Methodologies Using Solid-Phase Microextraction: A Review

Molecules ◽  
2020 ◽  
Vol 25 (22) ◽  
pp. 5297
Author(s):  
Kayla M. Billiard ◽  
Amanda R. Dershem ◽  
Emanuela Gionfriddo
Keyword(s):  
Analytical Chemistry ◽  
Sample Preparation ◽  
Analytical Method ◽  
Analytical Methods ◽  
Solid Phase Microextraction ◽  
Method Development ◽  
Assessment Tool ◽  
Solid Phase ◽  
Assessment Tools ◽  
Green Analytical Chemistry

Implementing green analytical methodologies has been one of the main objectives of the analytical chemistry community for the past two decades. Sample preparation and extraction procedures are two parts of analytical method development that can be best adapted to meet the principles of green analytical chemistry. The goal of transitioning to green analytical chemistry is to establish new methods that perform comparably—or superiorly—to traditional methods. The use of assessment tools to provide an objective and concise evaluation of the analytical methods’ adherence to the principles of green analytical chemistry is critical to achieving this goal. In this review, we describe various sample preparation and extraction methods that can be used to increase the greenness of a given analytical method. We gave special emphasis to modern microextraction technologies and their important contributions to the development of new green analytical methods. Several manuscripts in which the greenness of a solid-phase microextraction (SPME) technique was compared to other sample preparation strategies using the Green Analytical Procedure Index (GAPI), a green assessment tool, were reviewed.

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