Simultaneous extraction and analysis of preservatives and artificial sweeteners in juices by salting out liquid-liquid extraction method prior to ultra-high performance liquid chromatography.

A novel and fast salting out liquid-liquid extraction method was developed for simultaneous determination of food additives with different polarities in juices. Chromatographic separation was achieved in less than 6 min using Acquity UPLC BEH C 18 (100 mm × 2.1 mm d.i. × 1.7 µm) column with ammonium acetate with 0.01% of trifluoroacetic acid as eluent A and acetonitrile as eluent B at a flow rate of 0.2 mL min-1. The main factors affecting the extraction efficiency were optimized. The method was validated applying accuracy profile based on total error. The extraction recoveries ranged from 84.97 to 122%. Relative standard deviation ranged from 1.24 to 7.99% for intraday assay and from 1.69 to 9.16% for intermediate precision. The limits of detection for five food additives were from 0.3 to 1.42 µg mL-1. The method was successfully applied to 47 samples of juices from nine brands.

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.

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

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 ß-expectation tolerance interval developed by the Society of Pharmaceutical Science and Techniques Commission with an acceptability limit fixed at a λ of ±15%. The results demonstrated that the method 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.

ICD-11 (JLMMS) and SCT Inter-Operation.

The goal of this work is to contribute to a smooth and semantically sound inter-operability between the ICD-11 (International Classification of Diseases-11th revision Joint Linearization for Mortality, Morbidity and Statistics) and SNOMED CT (SCT). To guarantee such inter-operation between a classification, characterized by a single hierarchy of mutually exclusive and exhaustive classes, as is the JLMMS successor of ICD-10 on the one hand, and the multi-hierarchical, ontology-based clinical terminology SCT on the other hand, we use ontology axioms that logically express generalizable truths. This is expressed by the compositional grammar of SCT, together with queries on axiomsof SCT. We test the feasibility of the method on the circulatory chapter of ICD-11 JLMMS and present limitations and results.

Representing ICD-11 JLMMS Using IHTSDO Representation Formalisms.

It is investigated whether the content of the Joint Linearization for Mortality and Morbidity Statistics of the 11th ICD revision can be semantically represented by formalisms acting on the clinical terminology SNOMED CT, viz. the IHTSDO Compositional Grammar (CG) and the Expression Constraint Language (ECL). Whereas CG provides a composition syntax for building coordinated SNOMED CT expressions, ECL provides a powerful query mechanism. Both formalisms can be leveraged to guarantee inter-operation between an ontology-based terminology like SNOMED CT and a statistical classification like ICD, characterized by single hierarchies and exhaustive, mutually exclusive classes. We test the feasibility of the method on the circulatory chapter of ICD-11 JLMMS.