Development and Validation of Analytical Methods for Pharmaceuticals

Toomula, Nishant

doi:10.4172/2155-9872.1000127

Cited by 14 publications

(7 citation statements)

References 58 publications

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“…Plant medicines used as raw material in the production of herbal medicinal products should be subjected to qualitative and quantitative analysis of the active ingredients and / or chemical markers, when known. The methodologies developed and used in official compendia (pharmacopoeias) must be validated and all validation steps (specificity/selectivity, linearity, limits of detection (LOD) and quantification (LOQ), precision, precision and robustness) must be proven (5)(6)(7)(8)(9). The official compendia describe the determination of total alkaloids in A. belladonna by titration method (10)(11)(12) and also by gas chromatography (13), but these methods employ large amounts of solvents, mainly in the extraction stage and are difficult to reproduce.…”

Section: Introductionmentioning

confidence: 99%

Quantification of Atropine in Leaves of Atropa Belladonna: Development and Validation of Method by High-Perfomance Liquid Chromatography (Hplc)

et al. 2017

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The leaves of Atropa belladonna (L) are characterized by the presence of the alkaloid atropine, known for the antimuscarinic activity. The leaves are used in therapy, mainly in homeopathic preparations. An HPLC method was developed and validated to quantify atropine in belladonna leaves. The samples were extracted with methanol, followed by acid-base extraction with 5% HCl and dichloromethane. Analysis by HPLC was performed on C18 column, in a linear gradient system using a system with two mobile phases (water and acetonitrile), both acidified with trifluoroacetic acid. The determinations were performed using a reference standard and a diode array detector at 210 nm. The method was validated and proved to be specific / selective, comparing the UV profiles and the purity of the atropine peaks in reference and sample solutions and analyzing sample solutions with and without addition of standard, which produced an increase only of the area of peak of the sample, without changing the area of the adjacent peaks. The linearity (50 - 200 μg/mL) was provided by analysis of the analytical curves of atropine, with r2 = 0.9996. LOD and LOQ were 3.75 and 11.4 µg/ml, respectively. The method was precise, reproducible and accurate, and presented recovery equal to 103.0%. The method was considered robust for the analyzed parameters. Four commercial samples were analyzed and the mean levels of atropine found ranged from 0.16 - 0.27 %. Thus, the developed method is effective for quantification of atropine in beladona leaves and meets the validation requirements of current legislation and ensuring the quality control of the plant material.

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Section: Introductionmentioning

confidence: 99%

Quantification of Atropine in Leaves of Atropa Belladonna: Development and Validation of Method by High-Perfomance Liquid Chromatography (Hplc)

et al. 2017

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“…Analytical method development is the process of creating a procedure to enable a compound of interest to be identified and quantified in a matrix. A compound can often be measured by several methods and the choice of analytical method involves many considerations, such as: chemical properties of the analyte, concentrations levels, sample matrix, cost of the analysis, speed of the analysis, quantitative or qualitative measurement, precision required and necessary equipment [11,12] . The analytical chain describes the process of method development and includes sampling, sample preparation, separation, detection and evaluation of the results.…”

Section: Methods Developmentmentioning

confidence: 99%

A General Review on Bioanalytical Method Development and Validation for LC-MSMS

Badola¹,

Joshi²,

Kothiyal³

2018

IJTSRD

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Rapid growth in the use of LC-MS/MS for the analysis of drugs in biological matrices has been compelled by the need for timely and high data at every stages in drug discovery and development process: from throughput screening of drug candidates and rapid data generation for pre clinical studies to almost 'real-time' analysis of clinical samples. A well developed bioanalytical development and its validation plays a pivotal role in achieving the goals. . The aim behind this review is to enlighten the need of validation which provide a practical approach for determining the different parameters like selectivity, specifity, limit of detection, lower limit of quantitation, linearity, range, accuracy, precision, recovery, stability, ruggedness, and robustness to help the perfect studies of pharmacokinetic, toxic kinetic, bioavailability and bioequivalence. Bio-analysis study is for the quantitative determination of drug and their metabolites in biological fluids. Accurate and robust methods for quantitative analysis of drug and their metabolites are important for the successful conduct of pre-clinical, bio-pharmaceutics and clinical pharmacology.

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“…Validation is required for any new or modified method to ensure that the method isable to give reproducible and reliable results, when used by different operators employing the same equipment in the same or different laboratories. The validation plan depends entirely on the particular method and its proposed applications [35][36][37] .…”

Section: Methods Validationmentioning

confidence: 99%