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IVES 9 IVES Conference Series 9 OIV 9 OIV 2024 9 Short communications - Oenology, methods of analysis 9 Determination of steviol glycosides in wine by HPLC

Determination of steviol glycosides in wine by HPLC

Abstract

The SCL laboratory in Bordeaux is one of the two official control laboratories for wine and wine products in france, under the authority of the ministry of finance and two of its general directorates: the DGCCRF (directorate general for competition, consumer affairs and fraud control) and the DGDDI (directorate general of customs and excise duties). In this capacity, it verifies the regulatory compliance of wines and investigates any possible falsifications or fraud. Steviol glycosides are natural sweeteners that are not authorized as additives in wine. The delegated regulation (eu) 2019/934 establishes the oenological practices authorized in the european union, and steviol glycosides are not included in part d setting the limits and conditions for the sweetening of wines. Their use in wines therefore constitutes fraud. Since there is no specific analytical method for the determination of steviol glycosides in the oiv international methods of analysis of wines and musts, the laboratory has developed a simple and rapid method to identify and quantify them by liquid chromatography. The method allows the separation and quantification of the following sweeteners, in the order of elution: rebaudioside d, rebaudioside m, rebaudioside a, stevioside, rebaudioside c, dulcoside, rebaudioside b, steviolbioside. Validation tests for the accreditation of the determination of rebaudioside a and stevioside were carried out on 8 different matrices. The matrices of interest for the oiv are grape juice, white wine, rosé wine, red wine and fortified wine. Accreditation according to ISO/IEC 17025 standard was obtained in 2022. This communication aims to present the implemented method, examples of chromatograms, validation data (detection and quantification limits, uncertainties), as well as the strategy implemented in the absence of interlaboratory comparison circuits for alcoholic matrices such as wines.

Determinación de glicósidos de esteviol en vino por HPLC

El laboratorio scl de Burdeos es uno de los dos laboratorios oficiales de control de productos vitivinícolas en francia, dependiente del ministerio de finanzas y de dos de sus direcciones generales: la DGCCRF (dirección general de competencia, consumo y represión del fraude) y la DGDDI (dirección general de aduanas e impuestos especiales). En este sentido, verifica el cumplimiento normativo de los vinos y busca posibles falsificaciones o fraudes. Los glicósidos de esteviol son edulcorantes naturales que no están autorizados como aditivos en el vino. El reglamento delegado (UE) 2019/934 establece las prácticas enológicas autorizadas en la unión europea, y los glicósidos de esteviol no figuran en la parte d que fija los límites y condiciones para la edulcoración de los vinos. Su uso en los vinos constituye, por lo tanto, un fraude. Dado que no existe un método de análisis específico para los glicósidos de esteviol en la recopilación de métodos internacionales de análisis de vinos y mostos de la oiv, el laboratorio ha desarrollado un método sencillo y rápido para identificarlos y cuantificarlos mediante cromatografía líquida. El método permite separar y cuantificar los siguientes edulcorantes, en orden de elución: rebaudiósido d, rebaudiósido m, rebaudiósido a, estevióside, rebaudiósido c, dulcósido, rebaudiósido b, esteviol-biósido. Los ensayos de validación para la acreditación de la determinación de rebaudiósido a y estevióside se realizaron en 8 matrices diferentes. Las matrices de interés para la oiv son el jugo de uva, el vino blanco, el vino rosado, el vino tinto y el vino de licor. La acreditación según la norma iso/iec 17025 se obtuvo en 2022. Esta comunicación tiene como objetivo presentar el método implementado, ejemplos de cromatogramas, datos de validación (límites de detección y cuantificación, incertidumbres), así como la estrategia implementada en ausencia de circuitos de intercomparación para matrices alcohólicas como los vinos.

Dosage des glycosides de steviol dans le vin par CLHP 

Le laboratoire SCL de bordeaux est l’un des deux laboratoires officiels de contrôle des produits vitivinicoles en France, rattaché au ministère des finances et à deux de ses directions générales : la DGCCRF (direction générale de la concurrence, de la consommation et de la répression des fraudes) et la DGDDI (direction générale des douanes et droits indirects).   A ce titre il vérifie la conformité réglementaire des vins et recherche d’éventuelles falsifications ou fraudes. Les glycosides de stéviol sont des édulcorants naturels qui ne sont pas autorisés comme additifs dans le vin. Le règlement délégué (UE) 2019/934 établit les pratiques œnologiques autorisées dans l’union européenne, et les glycosides de stéviol ne figurent pas dans la partie d fixant les limites et conditions pour l’édulcoration des vins. Leur utilisation dans les vins constitue donc une fraude. Comme il n’existe pas de méthode de dosage spécifique pour les glycosides de stéviol dans le recueil des méthodes internationales d’analyse des vins de l’oiv, le laboratoire a développé une méthode simple et rapide à mettre en œuvre pour les identifier et les quantifier par chromatographie liquide en phase liquide.  La méthode permet de séparer et doser les édulcorants suivants, dans l’ordre d’élution : rébaudioside d, rébaudioside m, rébaudioside a, stévioside, rébaudioside c, dulcoside, rébaudioside b, stéviolbioside.  Les essais de validation en vue de l’accréditation du dosage des rébaudioside a et stévioside ont été réalisés sur 8 matrices différentes. Les matrices d’intérêt pour l’oiv sont un jus de raisin, un vin blanc, un vin rosé, un vin rouge et un vin de liqueur. L’accréditation selon la norme iso/cei 17025 a été obtenue en 2022. Cette communication vise à présenter la méthode mise en œuvre, des exemples de chromatogrammes, les données de validation (limite de détection, de quantification, incertitudes), ainsi que la stratégie mise en œuvre en l’absence de circuits d’intercomparaison pour les matrices alcoolisées telles que les vins.

Publication date: November 18, 2024

Issue: OIV 2024

Type: Article

Authors

Sophie Rosset¹, Nathalie Corradi¹

¹ Service Commun des Laboratoires – Laboratoire de Bordeaux, 3 avenue du Dr Albert Schweitzer, Pessac, France

Contact the author*

Tags

IVES Conference Series | OIV | OIV 2024

Citation

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