A strategy for validation of bioanalytical methods

Braggio, Simone; Barnaby, Robert J.; Grossi, Paula; Cugola, M.

doi:10.1016/0731-7085(95)01644-9

Cited by 177 publications

(102 citation statements)

References 14 publications

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“…The deviation at the lower end of the range was relatively large using simple least-squares linear regression because of the concentration ranges over 3 orders of magnitude. This phenomenon is common in bioanalytical analysis using LC/ MS based methods [48]. As such, a weighted least-squares linear regression was used [58,59] in our method.…”

Section: Methods Validation Design-mentioning

confidence: 99%

“…The guiding principles [41][42][43][44][45][46][47][48][49][50][51][52][53][54][55][56][57] for validation of bioanalytical methods were used as references to design the experiments. Since PGs, DiHETrEs, HETEs, EETs, and AA are endogenous compounds, the analyte-free brain matrix is not available for matrix-based method validation and there is no other proxy matrix available to mimic the complicated solid brain tissue.…”

Section: Methods Validation Design-mentioning

confidence: 99%

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A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue

Yue

Jansen

Strauss

et al. 2007

Journal of Pharmaceutical and Biomedical Analysis

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A sensitive, specific, and robust liquid chromatography/mass spectrometric (LC/ MS) method was developed and validated that allows simultaneous analysis of arachidonic acid (AA) and its cyclooxygenase, cytochrome P450, and lipoxygenase pathway metabolites prostaglandins (PGs), dihydroxyeicosatrienoic acids (DiHETrEs), hydroxyeicosatetraenoic acids (HETEs) and epoxyeicosatrienoic acids (EETs), including PGF 2α , PGE 2 , PGD 2 , PGJ 2 ,14,11,8,5,14,11,8,9-EET, and 5,6-EET in rat brain tissues. Deuterium labeled PGF 2α -d 4 , PGD 2 -d 4 , 15(S)-HETE-d 8 , 14,15-EET-d 8 , 11,12-EET-d 8 , 8,9-EET-d 8 , and AA-d 8 were used as internal standards. Solid phase extraction was used for sample preparation. A gradient LC/MS method using a C18 column and electrospray ionization source under negative ion mode was optimized for the best sensitivity and separation within 35 min. The method validation, including LC/MS instrument qualification, specificity, calibration model, accuracy, precision (without brain matrix and with brain matrix), and extraction efficiency were performed. The linear ranges of the calibration curves were 2-1000 pg for PGs, DiHETrEs, HETEs, and EETs, 10-2400 pg for PGE 2 and PGD 2 , and 20-2000 ng for AA, respectively.

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Section: Methods Validation Design-mentioning

confidence: 99%

Section: Methods Validation Design-mentioning

confidence: 99%

A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue

Yue

Jansen

Strauss

et al. 2007

Journal of Pharmaceutical and Biomedical Analysis

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“…It is determined by calculating the percent difference (bias%) between the measured mean contents and the corresponding nominal contents (Braggio et al, 1996). Table II shows the results obtained for intra-and inter-day accuracy.…”

Section: Accuracy and Recovery Studiesmentioning

confidence: 99%

Optimization and validation of an RP-HPLC method for the estimation of 6-mercaptopurine in bulk and pharmaceutical formulations

Somasekhar¹

2014

Braz. J. Pharm. Sci.

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A reverse phase HPLC method is described for the determination of 6-mercaptopurine in bulk and tablets. Chromatography was carried on a C 18 column using a mixture of acetonitrile and 0.05 mol/L sodium acetate buffer (10:90 v/v) as the mobile phase at a flow rate of 1 mL/min -1 with detection at 324 nm. The retention time of the drug was 3.25 min. The detector response was linear in the concentration of 0.01-5 μg/mL. The limit of detection and limit of quantification were 17 and 52 ng/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of mercaptopurine in bulk and tablets.Uniterms: 6-Mercaptopurine/determination. High perfomance liquid chromatography/reverse phase/ quantitative analysis. Pharmaceutical formulations/quality control Descreve-se método de CLAE em fase reversa para a determinação de mercaptopurina a granel e em comprimidos. A cromatografia foi realizada em coluna C18, utilizando mistura de acetonitrila em tampão acetato de sódio 0,05 mol/L (10:90 v/v) como fase móvel, com fluxo de 1 mL/min e detecção a 324 nm. O tempo de retenção do fármaco foi de 3,25 min. A resposta do detector foi linear na concentração de 0,01-5 μg/mL. O limite de detecção e o limite de quantificação foram de 17e 52 ng/mL, respectivamente. O método foi validado pela determinação de sua sensibilidade, linearidade, acurácia e precisão. O método proposto é simples, econômico, rápido, acurado e preciso e, então, pode ser aplicado para controle de qualidade de rotina da mercaptopurina em batelada e em comprimidos.Unitermos: Mercaptopurina/determinação. Cromatografia líquida de alta eficiência/fase reversa/análise quantitativa. Formulações farmacêuticas/controle de qualidade.

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“…Stability data are obtained from two or three different concentration levels (low, medium and high concentrations of the linearity range) at different time intervals after storing, performing replicate analysis (between 5 and 10 experiments) [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20][77][78][79][80][81][82][83][84][85][86][87][88]. For the determination of compound amount, freshly prepared calibration samples must be diluted from stock solutions using the same substance batch, same blank in the matrix of pharmaceutical dosage forms and same blank biological matrix as used for the stored samples [77][78][79][80][81][82][83][84][85][86][87][88]. A few hours of standard and sample solution stability can be required even for fast voltammetric methods [1][2]...…”

Section: Stabilitymentioning

confidence: 99%

“…Hence, it is considered appropriate when the RSD values calculated on the assay results obtained at different time intervals. System stability is appropriate if results do not exceed 20% of system precision [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20][77][78][79][80][81][82][83][84][85][86]. Stability data are obtained from two or three different concentration levels (low, medium and high concentrations of the linearity range) at different time intervals after storing, performing replicate analysis (between 5 and 10 experiments) [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18]…”

Section: Stabilitymentioning

confidence: 99%

The Role of and the Place of Method Validation in Drug Analysis Using Electroanalytical Techniques

Gümüştaş¹,

Özkan²

2014

TOACJ

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Electroanalytical methods are chosen for the sensitive analysis of pharmaceutically active compounds in their dosage forms and biological samples. Electroanalytical method validation is the process used to confirm that the determination procedure employed for a specific test is suitable for its intended use like other analytical methods. Results from electroanalytical method validation can be used to judge the quality, applicability, accuracy, reliability and consistency of analytical results; it is an integral part of any analytical procedure. Also in electroanalytical drug analysis, important decisions are taken which are based on data obtained from real samples. Validation parameters help assure that the electroanalytical methods ensure the correct identity, strength, quality, accurate, precise, selective, robust and sensitive. A well-defined and well-documented validation process provides regulatory agencies with evidence that the system and method suitable for its intended use. Method validation is an essential component of the measures that a laboratory should implement to permit it to produce reliable electroanalytical data.

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A strategy for validation of bioanalytical methods

Cited by 177 publications

References 14 publications

A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue

A liquid chromatography/mass spectrometric method for simultaneous analysis of arachidonic acid and its endogenous eicosanoid metabolites prostaglandins, dihydroxyeicosatrienoic acids, hydroxyeicosatetraenoic acids, and epoxyeicosatrienoic acids in rat brain tissue

Optimization and validation of an RP-HPLC method for the estimation of 6-mercaptopurine in bulk and pharmaceutical formulations

The Role of and the Place of Method Validation in Drug Analysis Using Electroanalytical Techniques

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