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See detailAN INNOVATIVE APPROACH TO SELECT THE PREDICTION MODEL IN THE DEVELOPMENT OF NIR SPECTROSCOPIC METHODS
Ziemons, Eric ULg; Mantanus, Jérôme ULg; Rozet, Eric ULg et al

Poster (2012, March)

Taking into account its non-invasive, non-destructive character and fast data acquisition, near infrared spectroscopy is more and more integrated in production processes to acquire analytical results ... [more ▼]

Taking into account its non-invasive, non-destructive character and fast data acquisition, near infrared spectroscopy is more and more integrated in production processes to acquire analytical results. Implementation of a NIR quantitative method is performed using an iterative heuristic approach that will ultimately build a model allowing the prediction of the concentration of the analyte of interest. In this context, the aim of the present study was to develop an innovative approach based on statistical tolerance intervals and the desirability index FMI (Fitting Model Index) to select the most appropriate prediction model from a list of candidate models instead of using conventional criteria such as R², RMSEC, RMSECV and RMSEP [1-2] without objective decision rules. This new approach is illustrated on different steps of a real pharmaceutical manufacturing process: water and Active Pharmaceutical Ingredient (API) determinations in pharmaceutical pellets. Variability sources such as production campaigns, batches, days and operators were introduced in the calibration and validation sets. Partial Least Square (PLS) regression on the calibration sets was performed to build prediction models of which the ability to quantify accurately was tested with the validation sets. Regarding the product specifications, the acceptance limits were set at 20% and 5%, for the moisture and API determination, respectively.As can be seen from Figure 1 and 2, this innovative approach based on the desirability index FMI of the accuracy profile enabled to build and select the most appropriate prediction model in full accordance with its very final goal, to quantify as accurately as possible the analytes of interest. [1] Hubert Ph. et al., J. Pharm. Biomed. Anal., 36, 2007, 579-586. [2] Rozet E. et al., Ana. Chim. Acta, 591, 2007, 239-247. [less ▲]

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See detailCritical analysis of several analytical method validation strategies in the framework of the fit for purpose concept.
Rozet, Eric ULg; Bouabidi, A.; Fillet, Marianne ULg et al

in Journal of Chromatography. A (2010), 1217

Analytical method validation is a mandatory step at the end of the development in all analytical laboratories. It is a highly regulated step of the life cycle of a quantitative analytical method. However ... [more ▼]

Analytical method validation is a mandatory step at the end of the development in all analytical laboratories. It is a highly regulated step of the life cycle of a quantitative analytical method. However, even if some documents have been published there is a lack of clear guidance for the methodology to follow to adequately decide when a method can be considered as valid. This situation has led to the availability of several methodological approaches and it is therefore the responsibility of the analyst to choose the best one. The classical decision processes encountered during method validation evaluation are compared, namely the descriptive, difference and equivalence approaches. Furthermore a validation approach using accuracy profile computed by means of beta-expectation tolerance interval and total measurement error is also available. In the present paper all of these different validation approaches were applied to the validation of two analytical methods. The evaluation of the producer and consumer risks by Monte Carlo simulations were also made in order to compare the appropriateness of these various approaches. The classical methodologies give rise to inadequate and contradictory conclusions which do not allow them to answer adequately the objective of method validation, i.e. to give enough guarantees that each of the future results that will be generated by the method during routine use will be close enough to the true value. It is found that the validation methodology which gives the most guarantees with regards to the reliability or adequacy of the decision to consider a method as valid is the one based on the use of the accuracy profile. [less ▲]

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See detailMoisture content determination of pharmaceutical pellets by near infrared spectroscopy: method development and validation.
Mantanus, Jérôme ULg; Ziemons, Eric ULg; Lebrun, Pierre ULg et al

in Analytica Chimica Acta (2009), 642(1-2), 186-92

The aim of the present study was to develop and validate a near infrared method able to accurately determine a moisture content of pharmaceutical pellets ranging from 1% to 8% in order to check their ... [more ▼]

The aim of the present study was to develop and validate a near infrared method able to accurately determine a moisture content of pharmaceutical pellets ranging from 1% to 8% in order to check their moisture content conformity. A calibration and validation set were designed for the conception and evaluation of the method adequacy. An experimental protocol was then followed, involving two operators, independent production campaign batches and different temperatures for data acquisition. On the basis of this protocol, prediction models based on partial least squares (PLS) regression were then carried out. Conventional criteria such as the R(2), the root mean square errors of calibration and prediction (RMSEC and RMSEP) as well as the number of PLS factors enabled the selection of three preliminary models. However, such criteria did not clearly demonstrate the model's ability to give accurate predictions over the whole analyzed water content range. Consequently, a novel approach based on accuracy profiles which allow the selection of the most fitted model for purpose was used. According to this novel approach, the model using multiplicative scatter correction (MSC) pre-treatment was obviously the most suitable. Indeed, the resulting accuracy profile clearly showed that this model was able to determine moisture content over the range of 1-8% with a very acceptable accuracy. The present study confirmed that NIR spectroscopy could be used in the PAT concept as a non-invasive, non-destructive and fast technique for moisture content determination in pharmaceutical pellets. In addition, facing the limit of the classical and commonly used criteria, the use of accuracy profiles proved to be useful as a powerful decision tool to demonstrate the suitability of the proposed analytical method. [less ▲]

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See detailNew validation strategy for the LC determination of ascorbic acid in sublingual tablets
Cahay, B.; Rousseau, Anne ULg; Klinkenberg, R. et al

Poster (2006)

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See detailValidation of a liquid chromatographic-tandem mass spectrometric method for the determination of loperamide in human plasma
Streel, B.; Ceccato, Attilio ULg; Klinkenberg, R. et al

in Journal of Chromatography. B : Analytical Technologies in the Biomedical & Life Sciences (2005), 814(2), 263-273

A sensitive and selective method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the quantitative determination of loperamide in human plasma. Automated solid ... [more ▼]

A sensitive and selective method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the quantitative determination of loperamide in human plasma. Automated solid-phase extraction (SPE) on disposable extraction cartridges (DEC) is used to isolate the compounds from the biological matrix and to prepare a cleaner sample before injection and analysis in the LC-MS/MS system. After conditioning, the plasma sample is loaded on the DEC filled with endcapped ethyl silica (C2(EC)) and washed twice with water. The analytes are therefore eluted by dispensing methanol. The eluate is then collected and added with ammonium acetate solution in order to inject an aliquot of this final extract in the LC-MS/MS system. On-line LC-MS/MS system using atmospheric pressure chemical ionization (APCI) has been developed for the determination of loperamide. The separation is obtained on a octadecylsilica based stationary phase using a mobile phase consisting in a mixture of methanol and 5 mM ammonium acetate solution (25:75, v/v). Clonazepam is used as internal standard (IS). The MS/MS ion transitions monitored are m/z 477 --> 266 and 316 --> 270 for loperamide and clonazepam, respectively. The most appropriate regression model of the response function as well as the limit of quantitation were first selected during the pre-validation step. These latter criteria were then assessed during the formal validation step. The limit of quantitation (LOQ) was around 50 pg/ml for loperamide. The method was also validated with respect to recovery, precision, trueness, accuracy and linearity. (C) 2004 Elsevier B.V. All rights reserved. [less ▲]

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See detailUSING TOTAL ERROR AS DECISION CRITERION IN METHOD TRANSFER
Rozet, Eric ULg; Mertens, B.; Dewe, W. et al

Poster (2005)

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See detailFully automated method for the liquid chromatographic-tandem mass spectrometric determination of cyproterone acetate in human plasma using restricted access material for on-line sample clean-up
Christiaens, B.; Fillet, Marianne ULg; Chiap, Patrice ULg et al

in Journal of Chromatography. A (2004), 1056(1-2), 105-110

A new automated method for the quantitative analysis of cyproterone acetate (CPA) in human plasma has been developed using on-line solid phase extraction (SPE) prior to the LC-MS/MS determination. The ... [more ▼]

A new automated method for the quantitative analysis of cyproterone acetate (CPA) in human plasma has been developed using on-line solid phase extraction (SPE) prior to the LC-MS/MS determination. The method was based on the use of a pre-column packed with internal-surface reversed-phase material (LiChrospher RP-4 ADS, 25 mm x 2 mm) for sample clean-up coupled to LC separation on an octadecyl silica stationary phase by means of a column switching system. A 30 microl plasma sample volume was injected directly onto the pre-column using a mixture of water, acetonitrile and formic acid (90:10:0.1 (v/v/v)) adjusted to pH 4.0 with diluted ammonia as washing liquid. The analyte was then eluted in the back-flush mode with the LC mobile phase consisting of water, methanol and formic acid (10:90:0.1 (v/v/v)). The dispensing flow rates of the washing liquid and the LC mobile phase were 300 microl min(-1). Medroxyprogesterone acetate (MPA) was used as internal standard. The MS ionization of the analytes was achieved using electrospray (ESI) in the positive ion mode. The pseudomolecular ionic species of CPA and MPA (417.4 and 387.5) were selected to generate daughter ions at 357.4 and 327.5, respectively. Finally, the developed method was validated according to a new approach using accuracy profiles as a decision tool. Very good results with respect to accuracy, detectability, repeatability, intermediate precision and selectivity were obtained. The LOQ of cyproterone acetate was 300 pg ml(-1). [less ▲]

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See detailSensitive determination of buprenorphine and its N-dealkylated metabolite norbuprenorphine in human plasma by liquid chromatography coupled to tandem mass spectrometry
Ceccato, Attilio ULg; Klinkenberg, R.; Hubert, Philippe ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2003), 32(4-5), 619-631

A highly sensitive method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the quantitative determination of buprenorphine and its active metabolite ... [more ▼]

A highly sensitive method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the quantitative determination of buprenorphine and its active metabolite norbuprenorphine in human plasma. Automated solid. phase extraction (SPE) on disposable extraction cartridges (DEC) is used to isolate the compounds from the biological matrix and to prepare a cleaner sample before injection and analysis in the LC-MS/MS system. After conditioning, the plasma sample (1.0 ml) is loaded on the DEC filled with octyl silica (C8) and washed with water. The analytes are, therefore, eluted by dispensing methanol containing 0.1% of acetic acid. The eluate is collected and evaporated to dryness. The residue is dissolved in mobile phase and an aliquot is injected in the LC-MS/ MS system. On-line LC-MS/MS system using atmospheric pressure chemical ionization (APCI) has been developed for the determination of buprenorphine and norbuprenorphine. The separation is obtained on a RP-18 stationary phase using a mobile phase consisting in a mixture of methanol and 50 mM ammonium acetate solution (50:50, v/v). Clonazepam is used as internal standard (IS). The MS/MS ion transitions monitored are m/z 468-->468, 414-->414 and 316-->270 for buprenorphine, norbuprenorphine and clonazepam, respectively. The method was validated regarding recovery, linearity, precision and accuracy. The limits of quantification (LOQs) were around 10 pg/ml for buprenorphine and 50 pg/ml for norbuprenorphine. (C) 2003 Elsevier Science B.V. All rights reserved. [less ▲]

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See detailQuantitative Analysis of N-Acetylcysteine and Its Pharmacopeial Impurities in a Pharmaceutical Formulation by Liquid Chromatography-Uv Detection-Mass Spectrometry
Toussaint, B.; Pitti, C.; Streel, B. et al

in Journal of Chromatography. A (2000), 896(1-2), 191-9

A new method for the simultaneous determination of N-acetylcysteine and its pharmacopeial impurities, cysteine, cystine, N,N'-diacetylcystine and N,S-diacetylcysteine in an effervescent tablet has been ... [more ▼]

A new method for the simultaneous determination of N-acetylcysteine and its pharmacopeial impurities, cysteine, cystine, N,N'-diacetylcystine and N,S-diacetylcysteine in an effervescent tablet has been developed. The method is based on on-line LC-UV-MS using a pneumatically-assisted electrospray interface (ionspray). The stability of the thiol moieties of the analytes was ensured by the acidic pH of the LC mobile phase. Quantitation of N-acetylcysteine was performed with UV detection to avoid ion-source overloading effect due to its higher concentration, whereas the impurities could be easily separated and quantified in MS. The method was validated in terms of stability, linearity, precision and accuracy. [less ▲]

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See detailDetermination of the Enantiomers of 3-Tert.-Butylamino-1,2-Propanediol by High-Performance Liquid Chromatography Using Mass Spectrometric Detection
Toussaint, B.; Streel, B.; Ceccato, Attilio ULg et al

in Journal of Chromatography. A (2000), 896(1-2), 201-7

The chiral synthesis of beta-blockers such as (S)-timolol requires a sensitive analytical method for the enantioseparation of its intermediate, 3-tert.-butylamino-1,2-propanediol, in the ng/ml range. The ... [more ▼]

The chiral synthesis of beta-blockers such as (S)-timolol requires a sensitive analytical method for the enantioseparation of its intermediate, 3-tert.-butylamino-1,2-propanediol, in the ng/ml range. The method developed is based on on-line normal-phase LC-MS-MS using a chiral stationary phase and an atmospheric pressure chemical ionization (APCI) interface. The MS detection of 3-tert.-butylamino-1,2-propanediol was first optimized with a pneumatically-assisted electrospray interface (ionspray). The APCI interface was then selected for LC-MS-MS because of the incompatibility of electrospray with n-hexane. The method was validated for both enantiomers in the 25-500 ng/ml concentration range. [less ▲]

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See detailDetermination of N-acetylcysteine and its metabolites in plasma by LC-MS-MS
Toussaint, B.; Streel, B.; Ceccato, Attilio ULg et al

Poster (2000)

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See detailQuantitative analysis of N-acetylcysteine and its pharmacopeial impurities in a pharmaceutical formulation by LC-UV-MS
Toussaint, B.; Pitti, Ch.; Streel, B. et al

Poster (2000)

Detailed reference viewed: 35 (0 ULg)
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See detailDetermination of 3-tert.butylamino-1,2-propanediol enantiomers by LC-MS-MS
Toussaint, B.; Streel, B.; Ceccato, Attilio ULg et al

Poster (2000)

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See detailSimultaneous determination of nifedipine and its metabolite in human plasma by LC/MS/MS using APCI interface
Streel, B.; Ceccato, Attilio ULg; Sibenaler, R. et al

Poster (1998)

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See detailHPLC determination of fenofibric acid in human plasma using automated solid phase extraction as sample preparation
Streel, B.; Zimmer, C.; Sibenaler-Dechamps, R. et al

in Journal de Pharmacie de Belgique (1995), 50

Detailed reference viewed: 29 (2 ULg)