Confirmatory reanalysis of incurred bioanalytical samples

Rocci, Mario L.; Devanarayan, Viswanath; Haughey, David B.; Jardieu, Paula

doi:10.1208/aapsj0903040

Cited by 136 publications

(76 citation statements)

References 10 publications

(19 reference statements)

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“…The original Bland-Altman (BA) analysis is a statistical method that is useful in assessing the agreement between two data sets with paired observations and in evaluating both systematic and random differences (4). It has been suggested that the agreement between original and reanalyzed results for ISR can be evaluated by using the assay acceptance criteria and an mBA statistical approach (5).…”

Section: Introductionmentioning

confidence: 99%

Assessment of Incurred Sample Reanalysis for Macromolecules to Evaluate Bioanalytical Method Robustness: Effects from Imprecision

Thway

Eschenberg

Calamba

et al. 2011

AAPS J

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Abstract. Incurred sample reanalysis (ISR) is recommended by regulatory agencies to demonstrate reproducibility of validated methods and provide confidence that methods used in pharmacokinetic and toxicokinetic assessments give reproducible results. For macromolecules to pass ISR, regulatory recommendations require that two thirds of ISR samples be within 30% of the average of original and reanalyzed values. A modified Bland-Altman (mBA) analysis was used to evaluate whether total error (TE), the sum of precision and accuracy, was predictive of a method's passing ISR and to identify potential contributing parameters for ISR success. Simulated studies determined minimum precision requirements for methods to have successful ISR and evaluated the relationship between precision and the probability of a method's passing ISR acceptance criteria. The present analysis evaluated ISRs conducted for 37 studies involving ligand-binding assays (LBAs), with TEs ranging from 15% to 30%. An mBA approach was used to assess accuracy and precision of ISR, each with a threshold of 30%. All ISR studies met current regulatory criteria; using mBA, all studies met the accuracy threshold of 30% or less, but two studies (5%) failed to meet the 30% precision threshold. Simulation results showed that when an LBA has ≤15% imprecision, the ISR criteria for both the regulatory recommendation and mBA would be met in 99.9% of studies. Approximately 71% of samples are expected to be within 1.5 times the method imprecision. Therefore, precision appears to be a critical parameter in LBA reproducibility and may also be useful in identifying methods that have difficulty passing ISR.

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Section: Introductionmentioning

confidence: 99%

Assessment of Incurred Sample Reanalysis for Macromolecules to Evaluate Bioanalytical Method Robustness: Effects from Imprecision

Thway

Eschenberg

Calamba

et al. 2011

AAPS J

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“…3). Правильность измерения определяли по формуле: (Hcy I -Hcy II) / GM, полученные значения находились в допустимом интервале (<20% по модулю) [20].…”

Section: рисунокunclassified

Determination of homocysteine by lc-ms-ms with atmospheric pressure chemical ionization

et al. 2014

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Homocysteine (Hcy) is an intermediate of methionine metabolism. High plasma Hcy concentrations are an independent risk factor for stroke, peripheral vascular disease, deep venous thrombosis, coronary disease, and cognitive deficiency. Apparently, it is a great importance to measure Hcy levels in human blood. A new method for the quantification of Hcy by means of reversed-phase LC/atmospheric pressure chemical ionization mass spectrometry has been developed. The MRM ion transition, m/z 136.0 ® 90.0 was used for Hcy quantification. The limit of detection was 0.4 mM, quantification was performed from 1 mM to 40 mM with coefficient of determination of R2=0,997. The method was applied successfully to Hcy determination in human blood.

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“…There have been reports that have assessed the above issues. Rocci et al (2007) and Hoffman (2009) This work was performed while Barbara Davit was with the FDA.…”

Section: Introductionmentioning

confidence: 99%

“…investigated appropriate design and sample size requirements for ISR testing (12,13). Recently, Thway et al (2011) investigated the effect of imprecision on ISR analysis for macromolecules (14).…”

Section: Introductionmentioning

confidence: 99%

Analysis of Imprecision in Incurred Sample Reanalysis for Small Molecules

Subramaniam¹,

Patel²,

Davit

et al. 2014

AAPS J

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Abstract. Over the years, incurred sample (IS) reanalysis (ISR) has become a tool to confirm the reliability of bioanalytical measurements. The recommendation for ISR acceptance criterion for small molecules is at least 67% of ISR samples that have reanalyzed concentrations within 20% of their original concentrations when normalized to their means. To understand the relevance of the ISR acceptance criterion and sample size requirements, simulated ISR studies evaluated the probability of ISR studies passing the acceptance criterion (ISR pass rate) as a function of IS imprecision and sample size. When IS imprecision (percent coefficient of variation: %CV) is low (≤10 or 1-10% CV), high ISR pass rate (≥99%) is attained with <50 samples. At intermediate IS imprecision (e.g., 12% CV or 7-12% CV range), 80-160 samples are required for a high ISR pass rate. When IS imprecision is at the higher end of the acceptance limit, ISR pass rate decreases significantly, and increasing sample size fails to achieve high ISR pass rate. The effect of systematic bias (e.g., instability, interconversion) on ISR pass rate is strongly dependent on sample size at intermediate IS imprecision. The results provide an understanding of the effect of IS imprecision on ISR pass rates and a framework for selection of ISR sample sizes.

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Confirmatory reanalysis of incurred bioanalytical samples

Cited by 136 publications

References 10 publications

Assessment of Incurred Sample Reanalysis for Macromolecules to Evaluate Bioanalytical Method Robustness: Effects from Imprecision

Assessment of Incurred Sample Reanalysis for Macromolecules to Evaluate Bioanalytical Method Robustness: Effects from Imprecision

Determination of homocysteine by lc-ms-ms with atmospheric pressure chemical ionization

Analysis of Imprecision in Incurred Sample Reanalysis for Small Molecules

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