Optimized DLLME Method Coupled to HPLC for Simultaneous Analyses of Benzoates, Sorbates and Methyl p-hydroxyl Benzoates in Fruits Products

We used an accurate and green technique "Dispersive Liquid Liquid Micro Extraction" (DLLME) followed by HPLC-UV analysis for the analysis of benzoates (BA), sorbates (SA), and p-hydroxyl methyl benzoates (MB) in fruits products. We optimized the   extraction parameters by the box Behnken design. We validated the method by using the β accuracy profile including the systematic (trueness) and random (intermediate precision) errors. The extraction efficiency varied from 82.98 to 100.8 %. This method was linear with R2s values higher than 0.9752 for all the compounds. The repeatability and intermediate precision were less than 3.18 and 12.02 respectively; whereas, the detection limits were respectively 0.304, 0.306 and 0.153 mg/ ml for BA, SA and MB. This method is therefore reliable to the simultaneous quantification of these preservatives in fruit juices, nectars and jams. The levels of these additives in the samples exceeded 833.97 and 290.67 ppm for BA and SA, respectively; while, MB was not detected. &nbsp

Strategies validation de nettoyage en industrie pharmaceitique : nouvelles recommandations et applications aux equipements de fabrication dans un site multiproduits

305f. : ill. ; 3cm. (+ CD -Rom)Dans ce travail de thèse de doctorat en sciences médicales, spécialité Chimie analytique – filière pharmacie, nous avons validé le nettoyage des équipements de fabrication de plusieurs formes pharmaceutiques selon la stratégie des pires cas. Cette stratégie est devenue une exigence réglementaire du fait qu’elle a été intégrée dans les récentes révisions des Bonnes Pratiques de Fabrication (BPF). La nouveauté apportée dans notre travail par rapport aux travaux existant est la proposition d’une démarche quantitative pour le choix des traceurs physicochimiques et microbiologique d’une part, et l’introduction de l’approche PDE (Permitted Daily Exposure) qui a pour finalité d’établir des limites d’exposition basée sur le risque santé du patient, d’autre part. Cette nouvelle approche d’introduction très récente en industrie pharmaceutique est exigé par la ligne directrice de l’Agence Européenne des Médicaments (EMA) et reprise par la récente version des BPF, en appliquant cette approche nous nous sommes conformés aux nouvelles exigences réglementaires

Optimized DLLME Method Coupled to HPLC for Simultaneous Analyses of Benzoates, Sorbates and Methyl p-hydroxyl Benzoates in Fruits Products

We used an accurate and green technique “Dispersive Liquid Liquid Micro Extraction” (DLLME) followed by HPLC-UV analysis for the analysis of benzoates (BA), sorbates (SA), and p-hydroxyl methyl benzoates (MB) in fruits products. We optimized the   extraction parameters by the box Behnken design. We validated the method by using the β accuracy profile including the systematic (trueness) and random (intermediate precision) errors. The extraction efficiency varied from 82.98 to 100.8 %. This method was linear with R2s values higher than 0.9752 for all the compounds. The repeatability and intermediate precision were less than 3.18 and 12.02 respectively; whereas, the detection limits were respectively 0.304, 0.306 and 0.153 mg/ ml for BA, SA and MB. This method is therefore reliable to the simultaneous quantification of these preservatives in fruit juices, nectars and jams. The levels of these additives in the samples exceeded 833.97 and 290.67 ppm for BA and SA, respectively; while, MB was not detected.  </jats:p

Application of an Accuracy Profile Strategy Based on the β-Expectation Tolerance Interval for the Validation of a Liquid Chromatography Analytical Method for the Quantification of Benzoic Acid and Its Salts in Different Foodstuffs

Abstract This paper presents the validation of a method for the quantification of benzoic acid and its salt preservatives, which are extensively used in the preservation of foodstuffs. The Joint Expert Committee on Food Additives at the Food Agricultural Organization and World Health Organization has established maximum permitted limits for these compounds in different foodstuffs because of the harmful effects of benzoic acid and its salt preservatives when they exceed certain limits. Therefore, a reliable and simple method to quantify these preservatives was validated. The developed method used a combination of extracted external calibration standards, a simple extraction procedure, and reversed-phase HPLC. This method was validated by applying a new approach in which the total error was based on the β-expectation tolerance interval developed by the Society of Pharmaceutical Science and Techniques Commission with an acceptability limit fixed ata λ of ±15%. The results demonstrated that themethod is accurate, with repeatability between 1.096 and 1.986% and intermediate precision between 1.133 and 2.005% in the considered concentration range. The LOD was 0.1597 μg/mL.</jats:p

Simultaneous Extraction and Determination of Preservatives and Antioxidants in Juice Samples by an Optimized Microextraction Method Using Central Composite Design and Validated with Accuracy Profile

Background: Food additives are widely used in industries. Overall, these additives have a beneficial role, but if their concentration exceeds certain limits, they may have an adverse effect on human health. Objective: This study outlines the determination of benzoic acid (BA), sorbic acid (SA), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) in juices using dispersive liquid-liquid microextraction and HPLC-diode-array detection. Methods: Different parameters that significantly affect the extraction efficiency were optimized. The disperser and extraction solvents were acetone and chloroform, respectively. The other parameters were selected and optimized using two-level (2k) factorial and central composite designs, respectively. A full method validation using an accuracy profile for the total measurement error was carried out. Results: The optimized conditions were 625 μL acetone, 350 μL chloroform, 0.85 g NaCl, and pH 2. The validated method demonstrated good linearity with R² ≥ 0.99 and good precision with the RSD of repeatability and intermediate precision at 1.97-10.7% and 2.31-11.9%, respectively. The relative recoveries were 96.2-105.4%, and the LODs were around 0.03 μg/mL for all compounds. The analysis of 41 samples revealed that BA and SA were quantified in 25 and 20 samples, respectively. BHA and BHT were not detected. Conclusions: The proposed methodology is an appropriate tool to determine important food additives in juices to ensure their compliance with the food additives legislation. Highlights: The work has demonstrated that the method can be successfully used in the simultaneous determination of four food additives in fruit juices.This work received financial support from the European Union (FEDER funds POCI/01/0145/FEDER/007265) and National Funds (FCT/MEC, Fundação para a Ciência e Tecnologia and Ministério da Educação e Ciência) under the Partnership Agreement PT2020 UID/QUI/50006/2013.info:eu-repo/semantics/publishedVersio