Using tolerance intervals in pre-study validation of analytical methods to predict in-study results

Rozet, Eric; Hubert, Cédric; Ceccato, Attilio; Dewé, Walthère; Ziémons, Eric; Moonen, François; Michail, Karim; Wintersteiger, Reinhold; Streel, Bruno; Boulanger, Bruno; Hubert, Philippe

doi:10.1016/j.chroma.2007.03.102

Cited by 73 publications

(41 citation statements)

References 10 publications

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“…Thus, the selection of the calibration curve for the quantification of iohexol in the two matrices should be the fit for purpose response function [25]. To determine the most adequate one for our goal, different calibration models have been evaluated.…”

Section: Response Functionmentioning

confidence: 99%

Performance of iohexol determination in serum and urine by HPLC: Validation, risk and uncertainty assessment

Cavalier

Rozet

Dubois

et al. 2008

Clinica Chimica Acta

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Background: Determination of glomerular filtration rate plays an important role in nephrological practice. Iohexol is a reference marker for glomerular filtration rate determination. It is available and safe. The aim of this study was to develop a simple, efficient and easy to use analytical method for the quantification of iohexol in serum and urine by high performance liquid chromatography and to thoroughly validate this method. Methods: The HPLC method was inspired from the method published by Krutzen. The e.noval software V2.0 (Arlenda, Liège, Belgium) was used to compute all validation results. Results: The validation results indicate that the method will give accurate and reliable results for serum values ranging from 12.95 to 1295 μg/ml and for urine values ranging from 86.0 to 4144 μg/ml. In routine practice, iohexol concentrations found in plasma after injection range from 40 to 600 μg/ml. The expected urinary values are much wider. One should not hesitate to dilute urine samples to fit with the validated range over 5000 μg/ml. Conclusion: This is the first time that a reference method for the determination of GFR is validated with such a rigorous and thorough protocol. Contrary to other GFR markers, iohexol is now strongly validated from an analytical point of view.

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Section: Response Functionmentioning

confidence: 99%

Performance of iohexol determination in serum and urine by HPLC: Validation, risk and uncertainty assessment

Cavalier

Rozet

Dubois

et al. 2008

Clinica Chimica Acta

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“…In order to evaluate the reliability of the results, an accuracy profile based on tolerance intervals was used (Rozet et al, 2007). Tolerance intervals or b-expectation tolerance intervals defined an interval space where each future result will fall with a specific probability (b).…”

Section: Validation Methodsmentioning

confidence: 99%

Rapid quantification of 2-hydroxypropyl-β-cyclodextrin in liquid pharmaceutical formulations by 1H nuclear magnetic resonance spectroscopy

Dufour

Évrard

Tullio

2015

European Journal of Pharmaceutical Sciences

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a b s t r a c tQuantification of 2-hydroxypropyl-b-cyclodextrin (2-HP-b-CD) is not yet described in United States Pharmacopeia (USP) and European Pharmacopeia (EP). A useful quality control tool is therefore needed for the specific quantification in finished liquid pharmaceutical products, especially for formulations containing 2-HP-b-CD as an active ingredient. A new technique is also mandatory for the development of future formulations in which 2-HP-b-CD concentration could influence the properties of these formulations. Here, we described the use of 1 H NMR for the rapid quantification of 2-HP-b-CD directly into pharmaceutical solutions without any extraction or separation steps. This technique was successfully applied to different pharmaceutical solutions comprising an i.v. solution (budesonide/2-HP-b-CD complex), an eye drop solution (Indocollyre Ò ) and an oral solution (Sporanox Ò ). Specificity, linearity, precision (repeatability and intermediate precision), trueness, limits of quantification (LOQs) and accuracy were used as validation criteria.

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“…This validation procedure, well described in the literature [28,29,[41][42][43][44][45][46][47][48][49], can be summarized as follows:…”

Section: Statistical Processing: Accuracy Profilementioning

confidence: 99%

“…With the results calculated from this study, a decrease in risk led to an increase in the LLOQ and, consequently, to a decrease in the validated range of concentrations. Furthermore, papers dealing with the accuracy profile procedure have obtained a probability of 95% [41][42][43][44][45][46][47][48][49]. Fig.…”

Section: Accuracy Profilementioning

confidence: 99%

Development and validation by accuracy profile of a method for the analysis of monoterpenes in indoor air by active sampling and thermal desorption-gas chromatography-mass spectrometry

Marlet

Lognay

2010

Talanta

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The technique of thermal desorption (TD)-GC/MS was evaluated for the measurement of monoterpenes in indoor air. The validation strategy was intentionally oriented towards routine use and the reliability of the method rather than extreme performance. For this reason, validation by accuracy profile was chosen. The accuracy profile procedure, which is based on the concept of total error (bias + standard deviation), guarantees that a known proportion of future results obtained with the method will be within acceptance limits. For all the compounds tested in the present study, α-pinene, α-terpineol, β-pinene, d-limonene, ∆ 3 -carene, camphene, 1,8-cineole, p-cymene, linalool, but not in the case of carvone, the accuracy profile procedure established that at least 95% of the future results obtained would be within the ±15% acceptance limits of the validated method over the whole defined concentration range. Other parameters, such as selectivity, recovery, repeatability, stability of the molecules of interest and the effect of temperature, were also determined. The performance of the described method was finally evaluated by the analysis of indoor air from new timber frame constructions.

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Using tolerance intervals in pre-study validation of analytical methods to predict in-study results

Cited by 73 publications

References 10 publications

Performance of iohexol determination in serum and urine by HPLC: Validation, risk and uncertainty assessment

Performance of iohexol determination in serum and urine by HPLC: Validation, risk and uncertainty assessment

Rapid quantification of 2-hydroxypropyl-β-cyclodextrin in liquid pharmaceutical formulations by 1H nuclear magnetic resonance spectroscopy

Development and validation by accuracy profile of a method for the analysis of monoterpenes in indoor air by active sampling and thermal desorption-gas chromatography-mass spectrometry

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