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See detailDevelopment of a LC-MS/MS analytical method for the simultaneous measurement of aldehydes coming from polyunsaturated fatty acids degradation in animal feed
Douny, Caroline ULg; Bayram, Pinar; Brose, François ULg et al

in Drug Testing and Analysis (2016), 8(5-6), 458-464

Knowing that polyunsaturated fatty acids can lead to the formation of potentially toxic aldehydes as secondary oxidation products, an analytical method using liquid chromatography coupled to tandem mass ... [more ▼]

Knowing that polyunsaturated fatty acids can lead to the formation of potentially toxic aldehydes as secondary oxidation products, an analytical method using liquid chromatography coupled to tandem mass spectrometry detection (LC-MS/MS) has been developed to evaluate the concentration of eight aldehydes in animal feed: malondialdehyde (MDA), 4-hydroxy-2-nonenal (4-HNE), 4-hydroxy-2-hexenal (4-HHE), crotonaldehyde (CRT), benzaldehyde (BNZ), hexanal (HXL), 2,4-nonadienal and 2,4-decadienal. The developed method has been validated according to the criteria and procedure described in international standards. The evaluated parameters were: specificity/selectivity, recovery, precision, accuracy, uncertainty, limits of detection and quantification, using the concept of accuracy profiles. These parameters have been determined during experiments realized on 3 different days with grounded Kellogg’s® Corn Flakes® cereals as model matrix for animal feed and spiked at different levels of concentration. Malondialdehyde, 4-HHE, 4-HNE, crotonaldehyde, benzaldehyde and hexanal can be analysed in the same run in animal feed with a very good accuracy, with recovery rates ranging from 86 to 109% for a working range going from 0.16 to 12.50 mg/kg. Concerning 2,4-nonadienal and 2,4-decadienal, their analysis can be realized as well but in a limited range of concentration and with a limited accuracy. Indeed, recovery rates ranged between 54 and 114% and coefficient of variation for the intermediate precision between 11 and 25% for these two compounds. [less ▲]

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See detailFlexibility and Applicability of β-expectation tolerance interval approach to assess the fitness of purpose of pharmaceutical analytical methods
Bouabidi, Abderrahim; Talbi, M.; Bourichi, H. et al

in Drug Testing and Analysis (2012), 4(12), 1014-1027

An innovative versatile strategy using Total Error has been proposed to decide about the method’s validity that controls the risk of accepting an unsuitable assay together with the ability to predict the ... [more ▼]

An innovative versatile strategy using Total Error has been proposed to decide about the method’s validity that controls the risk of accepting an unsuitable assay together with the ability to predict the reliability of future results. This strategy is based on the simultaneous combination of systematic (bias) and random (imprecision) error of analytical methods. Using validation standards both types of error are combined through the use of a prediction interval or β-expectation tolerance interval. Finally, an accuracy profile is built by connecting, on one hand all the upper tolerance limits, and on the other hand all the lower tolerance limits. This profile combined with pre-specified acceptance limits allows to evaluate the validity of any quantitative analytical method and thus their fitness for their intended purpose. In this work, the approach of accuracy profile was evaluated on several types of analytical methods encountered in pharmaceutical industrial field and also covering different pharmaceutical matrices. The four studied examples depicted the flexibility and applicability of this approach for different matrices ranging from tablets to syrups, different techniques such as liquid chromatography, or UV spectrophotometry and for different categories of assays commonly encountered in the pharmaceutical industry that are content assays, dissolution assays and quantitative impurity assays. The accuracy profile approach assesses the fitness of purpose of these methods for their future routine application,. It also allows to select the most suitable calibration curve, to evaluate adequately a potential matrix effect and propose efficient solution and to define correctly the limits of quantification of the studied analytical procedures. [less ▲]

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