Key aspects of analytical method validation and linearity evaluation

Araujo, Pedro

doi:10.1016/j.jchromb.2008.09.030

Cited by 377 publications

(275 citation statements)

References 43 publications

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“…FED, a systematic approach for studying the effects of multiple factors, 28 has been successfully used in the optimization and robustness testing of pharmaceutical analytical procedures. 29,30 However, it has not been widely used, although recommended, in optimization and validation studies of biological assays yet, 31 particularly in assays involving animals.…”

Section: Introductionmentioning

confidence: 99%

Factors influencing preclinicalin vivoevaluation of mumps vaccine strain immunogenicity

Halassy

Kurtović

Brgles

et al. 2015

Human Vaccines & Immunotherapeutics

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Keywords: design of Experiments (DoE), in vivo bioassay optimization, mumps virus, non-clinical vaccine immunogenicity assessmentImmunogenicity testing in animals is a necessary preclinical assay for demonstration of vaccine efficacy the results of which are often the basis for the decision whether to proceed or withdraw the further development of the novel vaccine candidate. However, in vivo assays are rarely, if at all, optimized and validated. Here we clearly demonstrate the importance of in vivo assay (mumps virus immunogenicity testing in guinea pigs) optimization for gaining reliable results and the suitability of Fractional factorial design of experiments (DoE) for such a purpose. By the use of DoE with resolution IV (2 IV (4-1) ) we clearly revealed that the parameters significantly increasing assay sensitivity were interval between animal immunizations followed by the body weight of experimental animals. The quantity (0 versus 2%) of the stabilizer (fetal bovine serum, FBS) in the sample was shown as non-influencing parameter in DoE setup. However, the separate experiment investigating only the FBS influence, and performed under other parameters optimally set, showed that FBS also influences the results of immunogenicity assay. Such finding indicated that (a) factors with strong influence on the measured outcome can hide the effects of parameters with modest/low influence and (b) the matrix of mumps virus samples to be compared for immunogenicity must be identical for reliable virus immunogenicity comparison. Finally the 3 mumps vaccine strains widely used for decades in the licensed vaccines were for the first time compared in an animal model, and results obtained were in line with their reported immunogenicity in human population supporting the predictive power of the optimized in vivo assay.

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Section: Introductionmentioning

confidence: 99%

Factors influencing preclinicalin vivoevaluation of mumps vaccine strain immunogenicity

Halassy

Kurtović

Brgles

et al. 2015

Human Vaccines & Immunotherapeutics

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“…In many reports linearity was simply evaluated by the correlation coefficient, r, but this might be not sufficient and F-test is also needed. 30 The linear range for DA quantification was from 40 to 1000 pg/mL.…”

Section: Resultsmentioning

confidence: 99%

“…A correlation coefficient (r) above 0.990 and F > Fα were required for determining the linearity. 30 The lowest concentration of the calibration curve was gradually diluted and analyzed for determining the LOD and LOQ. The LOD was defined as the concentration level at which the signal-to-noise ratio (S/N) equals to or is greater than 3 for selected ion transitions.…”

Section: Methods Validationmentioning

confidence: 99%

Quantification of Dopamine in Brain Microdialysates with High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Zhang

Zhou

et al. 2016

ANAL. SCI.

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The dopamine level in the brain and the mesolimbick dopaminergic system are responsible for nicotine addiction. In the present study, extracellular dopamine in nucleus accumbens was collected by a brain microdialysis technique. Also a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method with a gradient elution procedure was developed for a precise determination of dopamine in brain dialysate. The retention time of dopamine was about 11.32 min. The linear range was 20 -1000 pg/mL. The limit of detection (LOD) and the limit of qualification (LOQ) were 5 and 20 pg/mL, respectively. The recovery ranged from 98.2 to 109.0%, and both the intra-RSD and inter-RSD were below <9%, respectively. The probe recovery for dopamine in this brain microdialysis experiment was about 25%. Finally, the dopamine concentrations in the rat brain microdialysates were determined, and the pharmacokinetics of extracellular dopamine in the brain nucleus accumbens after an intravenous injection of nicotine was successfully evaluated.

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“…The coefficient of determination is not a true indicator of linearity, therefore the Fischer variance ratio (Araujo, 2009) (test of linearity) was used. The test of linearity was performed using the Statistica v. 10.0 statistical software.…”

Section: Captopril/p-chloranil/h 2 O 2 Systemmentioning

confidence: 99%

Development and application of a portable instrument for drugs analysis in pharmaceutical preparations

Ribeiro

Pezza

et al. 2015

Braz. J. Pharm. Sci.

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This article describes the application and performance of an inexpensive, simple and portable device for colorimetric quantitative determination of drugs in pharmaceutical preparations. The sensor is a light detector resistor (LDR) incorporated into a black PTFE cell and coupled to a low-cost multimeter (Ohmmeter). Quantitative studies were performed with captopril/p-chloranil/H 2 O 2 and methyldopa/ ammonium molybdate systems. Calibration curves were obtained by plotting the electrical resistance of the LDR against the concentration of the colored species in the ranges 1.84 × 10 -4 to 1.29 × 10 -3 mol L -1 and 5.04 × 10 -4 to 2.52 × 10 -3 mol L -1 for captopril/p-chloranil/H 2 O 2 and methyldopa/ammonium molybdate systems, respectively, exhibiting good coefficients of determination. Statistical analysis of the results obtained showed no significant difference between the proposed methodologies and the official reported methods, as evidenced by the t-test and variance ratio at a 95% confidence level. The results of this study demonstrate the applicability of the instrument for simple, accurate, precise, fast, in situ and low-cost colorimetric analysis of drugs in pharmaceutical products. Uniterms:Optical sensor/application/colorimetric analysis. Instrumentation/drugs dosage. Drugs/ quantitative analysis. Drugs/dosage. Pharmaceutical formulations/quality control.Este artigo descreve o desenvolvimento e a aplicação de um dispositivo portátil, simples e barato para a determinação colorimétrica quantitativa de fármacos em formulações farmacêuticas. O sensor é um resistor detector de luz (RDL) colocado numa célula de PTFE e acoplado a um multímetro de baixo custo. Os estudos quantitativos foram realizados utilizando captopril/p-cloranil/H 2 O 2 e metildopa/molibdato de amônio como sistemas reacionais. As curvas de calibração foram obtidas através da representação gráfica da resistência elétrica do RDL contra a concentração dos complexos coloridos formados nas faixas de 1,84 × 10 -4 e 1,29 × 10 -3 mol L -1 e 5,04 × 10 -4 e 2,52 × 10 -3 mol L -1 para captopril/p-cloranil/H 2 O 2 e de metildopa/molibdato de amônio, respectivamente, com bons coeficientes de determinação. As análises estatísticas dos resultados obtidos mostraram que não houve diferença significativa entre os métodos propostos e os métodos oficiais como evidente a partir dos testes "t-Student" e F-Fisher, com nível de confiança de 95%. Os resultados deste estudo demonstram que o instrumento proposto neste trabalho é simples, de fácil operação, baixo custo e apresentou boa exatidão e boa precisão para o doseamento de fármacos em medicamentos.Unitermos: Sensor óptico/aplicação/análise colorimétrica. Instrumentação/doseamento de fármacos. Fármacos/análise quantitativa. Fármacos/doseamento. Formulações farmacêuticas/controle de qualidade.

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Key aspects of analytical method validation and linearity evaluation

Cited by 377 publications

References 43 publications

Factors influencing preclinicalin vivoevaluation of mumps vaccine strain immunogenicity

Factors influencing preclinicalin vivoevaluation of mumps vaccine strain immunogenicity

Quantification of Dopamine in Brain Microdialysates with High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Development and application of a portable instrument for drugs analysis in pharmaceutical preparations

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