Influence of number of calibration standards within a defined range on pharmacokinetic disposition-case studies with omeprazole and clopidogrel carboxylic acid (original) (raw)
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An Empirical Study on the Impact of Bioanalytical Method Variability on Estimation of PK Parameters
Chromatographia, 2004
The effect of the experimental error of bioanalytical methods on the estimation of pharmacokinetic (PK) parameters was formerly studied with simulation experiments. The results showed that the precision of affects both accuracy and precision of pharmacokinetic parameters. In particular for drugs with small within-individual pharmacokinetic variability the contribution of bioanalytical imprecision of 15% may become unacceptable. The above-mentioned simulation results were confirmed by a recent experiment where plasma curves were analysed in multifold in the same and in different analytical batches, thereby being able to quantify correlations between bioanalytical within-day and between-day variability and PK variability. The results showed that for compounds or formulations with large betweensubject or within-subject/between-dosing variability more bioanalytical variability may be acceptable than for drugs with small between-subject variability. Acceptability of analytical precision and accuracy depends on the compound and the study design. Influence of bioanalysis on final outcome is generally insignificant. In general it can be stated that most bioanalytical assays used for regulatory support are very suitable if they are operated within current guideline criteria.
An Evaluation of Analytic Goals for Assays of Drugs
Archives of Pathology & Laboratory Medicine, 2001
Objective.—To determine if the levels of imprecision of the commonly used analytic methods for drug measurements are suitable for long-term therapeutic drug monitoring. Design.—In 1996, 4 identical lyophilized samples (2 in the first mailing and 2 in the second mailing 4 months later) were sent to laboratories participating in a nationwide proficiency testing program. Similarly, in 1999, replicates from a liquid pool of spiked sera were mailed 3 times, 4 months apart, to participating laboratories. For each of 11 drugs regulated under the Clinical Laboratory Improvement Amendments of 1988 and 1 metabolite, the total variance for each method was partitioned into within- and between-laboratory components. The total within-laboratory and the total survey coefficients of variation (CVs) for each method were then compared with the “acceptable” precision criteria of Glick, Burnett, and Fraser for each drug. Setting.—The first 2 mailings of the College of American Pathologists Therapeutic ...
Bioanalytical Method Validation and Its Pharmaceutical Application- AReview
Pharmaceutica Analytica Acta, 2014
Bioanalytical methods, based on a variety of physico-chemical and biological techniques such as chromatography, immunoassay and mass spectrometry, must be validated prior to and during use to give confidence in the results generated. It is the process used to establish that a quantitative analytical method is suitable for biomedical applications. Bioanalytical method validation includes all of the procedures that demonstrate that a particular method used for quantitative measurement of analytes in a given biological matrix, such as blood, plasma, serum, or urine is reliable and reproducible for the intended use. The present manuscript focuses on the consistent evaluation of the key bioanalytical validation parameters is discussed: accuracy, precision, sensitivity, selectivity, standard curve, limits of quantification, range, recovery and stability. These validation parameters are described, together with an example of validation methodology applied in the case of chromatographic met...
Journal of chromatography. B, Biomedical applications, 1996
Validations of analytical methods are important for the generation of data for bioavailability, bioequivalence and pharmacokinetic studies. It is essential to use well defined and fully validated analytical methods to obtain reliable results that can be satisfactorily interpreted. This manuscript is intended to provide guiding principles for the evaluation of a method's overall performance. For this purpose, all of the variables of the method are considered, including sampling procedure, sample preparation, chromatographic separation, detection and data evaluation. The criteria considered are as follows: stability, selectivity, limits of quantification and of detection, accuracy, precision, linearity, recovery and ruggedness. Models used for analytical calibration curves are explained in term of validity and limitations, along with a presentation of the most common statistical considerations used to validate the model. Appropriate means of testing precision and accuracy, the mos...
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Pharmaceutical Methods, 2010
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NOVEL ANALYTICAL TECHNIQUES USED IN METHOD DEVELOPMENT AND VALIDATION OF PHARMACEUTICALS
The major goal of this review is to explain the novel analytical techniques used in method development and validation of various medicines because they are vitally important for the drug's consistency, efficacy, and quality. LC-MS, RP-HPLC, and other innovative analytical techniques During this review, automated development in HPTLC and LC-MS-MS are discussed using appropriate drug samples in accordance with ICH Guidelines. ICH Guidelines also specify many validation characteristics such as accuracy, specificity, precision, linearity, LOD, LOQ, ruggedness, and robustness. Validation is tremendously beneficial to pharmaceutical standard control and quality assurance, as well as patient safety.
Asian Journal of Pharmaceutical and Clinical Research, 2021
The focus of bioanalysis employed for the quantitative determination of an active analyte(s) and their metabolite(s) in the biological matrix such as plasma, serum, blood, cerebrospinal fluid, and tissues. The extraction of analyte and metabolite in the biological fluids is carried out using different separation methods such as protein precipitation, liquid-liquid extraction, and solid phase extraction. Bioanalytical method development and validation in the pharmaceutical industry are to provide an assessment and interpretation of pharmacokinetics, pharmacodynamics, toxicokinetics, bioavailability/bioequivalence, and therapeutic drug monitoring relationships. This review paper aims to provide a simple and accurate scientific background to improve the quality for development and validation of a bioanalytical method for small molecules with industrial technique as per regulatory agency requirements (United States Food and Drug Administration, EMEA, International Council for Harmonisation and ANVISA).
Analytical methods validation: Bioavailability, bioequivalence and pharmacokinetic studies
European Journal of Drug Metabolism and Pharmacokinetics, 1991
This is a summary report of the conference on Analytical Methods Validation: Bioavailability, Bioequivalence and Pharmacokinetic Studies. The conference was held from December 3 to 5, 1990 in the Washington, DC area and was sponsored by the American Association of Pharmaceutical Scientists, US Food and Drug Administration, Federation International Pharmaceutique, Health Protection Branch (Canada) and Association of Official Analytical Chemists. The purpose of the report is to represent our assessment of the major agreements and issues discussed at the conference. The report is also intended to provide guiding principles for validation of analytical methods employed in bioavailability, bioequivalence and pharmacokinetic studies in man and animals. The objectives of the conference were: 1. To reach a consensus on what should be required in analytical methods validation and the procedures to establish validation; 2. To determine processes of application of the validation procedures in the bioavailability, bioequivalence and pharmacokinetic studies; 3. To develop a report on analytical methods validation (which may be referred to in developing future formal guidelines). Acceptable standards for documenting and validating analytical methods with regard to processes, parameters or data treatments were discussed because of their importance in assessment of pharmacokinetic, bioavailability and bioequivalence studies. Other topics which were considered essential in the conduct of pharmacokinetic studies or in establishing bioequivalency criteria, including measurement of drug metabolites and stereoselective determinations, were also deliberated.