Measurement uncertainty in pharmaceutical analysis and its application

Calibration curve is a regression model used to predict the unknown concentrations of analytes of interest based on the response of the instrument to the known standards. Some statistical analyses are required to choose the best model fitting to the experimental data and also evaluate the linearity and homoscedasticity of the calibration curve. Using an internal standard corrects for the loss of analyte during sample preparation and analysis provided that it is selected appropriately. After the best regression model is selected, the analytical method needs to be validated using quality control (QC) samples prepared and stored in the same temperature as intended for the study samples. Most of the international guidelines require that the parameters, including linearity, specificity, selectivity, accuracy, precision, lower limit of quantification (LLOQ), matrix effect and stability, be assessed during validation. Despite the highly regulated area, some challenges still exist regarding the validation of some analytical methods including methods when no analyte-free matrix is available.

show abstract

“…Sampling, calibration and repeatability were the most significant sources, which affect combined uncertainty [20].…”

Section: Calibration and Validation Of Analytical Methods -A Samplingmentioning

confidence: 99%

Linearity of Calibration Curves for Analytical Methods: A Review of Criteria for Assessment of Method Reliability

Moosavi¹,

Ghassabian²

2018

Calibration and Validation of Analytical Methods - A Sampling of Current Approaches

104

View full text Add to dashboard Cite

show abstract

“…Traple et al (2014) published a review of MU applied in pharmaceutical analysis (Traple et al, 2014) describing the main sources of uncertainty such as sampling; instrumental effects; calibration mass and volumetric apparatus; purity of reagents and certified chemical substances; matrix effects and sample stability; analyst skills and training effects; environmental effects; random effects inherent to experimental determinations (Ellison, Williams, 2012).…”

Section: Introductionmentioning

confidence: 99%

Measurement uncertainty of dissolution test of acetaminophen immediate release tablets using Monte Carlo simulations

Romero¹,

Lourenço²

2017

Braz. J. Pharm. Sci.

Self Cite

View full text Add to dashboard Cite

Analytical results are widely used to assess batch-by-batch conformity, pharmaceutical equivalence, as well as in the development of drug products. Despite this, few papers describing the measurement uncertainty estimation associated with these results were found in the literature. Here, we described a simple procedure used for estimating measurement uncertainty associated with the dissolution test of acetaminophen tablets. A fractionate factorial design was used to define a mathematical model that explains the amount of acetaminophen dissolved (%) as a function of time of dissolution (from 20 to 40 minutes), volume of dissolution media (from 800 to 1000 mL), pH of dissolution media (from 2.0 to 6.8), and rotation speed (from 40 to 60 rpm). Using Monte Carlo simulations, we estimated measurement uncertainty for dissolution test of acetaminophen tablets (95.2 ± 1.0%), with a 95% confidence level. Rotation speed was the most important source of uncertainty, contributing about 96.2% of overall uncertainty. Finally, it is important to note that the uncertainty calculated in this paper reflects the expected uncertainty to the dissolution test, and does not consider variations in the content of acetaminophen.

show abstract

“…An analytical result is not complete unless it has been reported with its measurement uncertainty (Desimoni and Brunetti, 2011). Measurement uncertainty is a parameter that, when associated with a measurement result, characterizes values dispersion that can be fundamentally attributed to a result (Eurachem, 2012;Traple et al, 2014).…”

Section: Introductionmentioning

confidence: 99%

An alternative capillary electrophoresis method for the quantification of caspofungin in lyophilisate powder and its measurement uncertainty

Daniela¹,

Pinto²

2014

Afr. J. Pharm. Pharmacol.

View full text Add to dashboard Cite

Recently, the use of capillary electrophoresis (CE) methods in pharmaceutical practice has gradually increased. Moreover, measurement uncertainty has been used to guarantee the traceability and the reliability of analytical results obtained. The aim of this work was to develop and validate a CE method for the quantification of caspofungin in lyophilised powder for injection, as well as to study the main sources of uncertainty associated with the method proposed and establish a procedure to estimate uncertainty in routine analysis. The results obtained during the validation procedure were statistically evaluated and demonstrate the specificity, robustness, linearity (r = 0.9999; y= 7.9014x-0.0107, concentration range: 20 to 300 g/ml), precision (repeatability, RSD: 0.40%; intermediate precision, RSD: 0.54%) and accuracy (recovery range: 95.80 to 100.45%). Without using internal standard correction, almost all uncertainty is associated to repeatability of sample and standard peak areas (more than 90%). On the other hand, using internal standard reduced variability significantly. The results allow us to affirm that EC method is suitable for analysis of caspofungin and it may be applied in routine quality control laboratories. In addition, this study confirmed that the equations proposed in the paper may be used for the measurement of uncertainty estimation in routine analysis.

show abstract

Measurement uncertainty in pharmaceutical analysis and its application

Cited by 46 publications

References 29 publications

Linearity of Calibration Curves for Analytical Methods: A Review of Criteria for Assessment of Method Reliability

Linearity of Calibration Curves for Analytical Methods: A Review of Criteria for Assessment of Method Reliability

Measurement uncertainty of dissolution test of acetaminophen immediate release tablets using Monte Carlo simulations

An alternative capillary electrophoresis method for the quantification of caspofungin in lyophilisate powder and its measurement uncertainty

Contact Info

Product

Resources

About