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IVES 9 IVES Conference Series 9 OIV 9 OIV 2024 9 Short communications - Oenology, methods of analysis 9 Validation of a method for the determination of volatile compounds in in spirituous beverages using contained ethanol as a reference substance

Validation of a method for the determination of volatile compounds in in spirituous beverages using contained ethanol as a reference substance

Abstract

The results of experimental studies of the method based on the usage of ethyl alcohol as an internal standard for the direct determination of volatile compounds in wines and others alcohol contained products are presented. The method was validated in terms of precision, accuracy, limits of detection and quantification (lod and loq), linearity, and robustness. Experimental studies were carried out using standard solutions of volatile components acetaldehyde, methyl acetate, ethyl acetate, isopropanol, propanol, isobutanol , butanol, isoamylol in the concentration range from 2 to 5000 mg/l of anhydrous ethanol in water-ethanol matrices with a volume content of ethyl alcohol from 96% to 10%.the within- and between-day precision (rsd) values of concentrations were in the ranges of 0.1–1.6 %. The linearity parameters r2 were more than 0.996 for all compounds. In 2021, the validation of new method for determining the quantitative content of volatile components such as of isopropyl alcohol and methyl ethyl ketone in alcoholic products was carried out during interlaboratory study with the participation of 49 customs laboratories of the european union. Based on the positive results, the standard iliade 453:2024 | clen method “determination of isopropyl alcohol and methyl ethyl ketone in alcoholic products by gc-fid” was adopted on february 13, 2024. A system has been developed to unify the transfer of measured chromatogram data from participants in interlaboratory tests into ms excel tables. Opportunities have been prepared for the interaction of the new method with the labwork platform, which will contribute to the effective implementation of the cii-scma 2023-09 06 project. In conclusion, it is important to note that the validation of the proposed method can be carried out on the basis of experimental data obtained in a testing laboratory during the validation of a traditional internal standard method, for example, in accordance with EC regulation 2870/2000 or analytical methods OIV-MA-BS-14, OIV-MA-AS312-03a, OIV-MA-AS315-27. No additional material, financial or labor costs are required. 

References 1. Charapitsa s., et al. The method for direct gas chromatographic determination of acetaldehyde, methanol, and other volatiles using ethanol as a reference substance: application for a wide range of alcoholic beverages. Food analytical methods (2021), vol. 14: p. 2088–2100. Https://doi.org/10.1007/s12161-021-02047-8. 2. Iliade 453:2024 | clen method “determination of isopropyl alcohol and methyl ethyl ketone in alcoholic products by gc-fid”, https://taxation-customs.ec.europa.eu/system/files/2023-09/iliade453_ipa%26mek_v25july2023_clenmethod.pdf . 3. Working with spreadsheets (mso excel, lo calc) in unichrom way. Https://www.unichrom.com/calc/calce.shtml .

валидация метода определения количественного содержания летучих соединений в спиртныхнапитках с использованием содержащегося в нем этанола в качестве эталонного вещества

Представлены результаты экспериментальных исследований метода, основанного наиспользовании этилового спирта в качестве эталонного вещества для прямого определениялетучих соединений в винах и другой спиртосодержащей продукции. Метод был валидирован втерминах прецизионности, точности, пределов обнаружения и количественного определения (lod иloq), линейности и устойчивости. Экспериментальные исследования проводились с использованиемстандартных растворов летучих компонентов ацетальдегида, метилацетата, этилацетата, изопропанола, пропанола, изобутанола, бутанола, изоамилола в диапазоне концентраций от 2 до5000 мг/л абсолютного алкоголя (aa) в водно-этанольных матрицах с объемны содержаниемэтилового спирта от 96 до 10%. Внутри- и междневные значения прецизионности находились впределах 0,1 – 1,6%. Параметры линейности r2 для всех соединений составили более 0,996. В 2021 году валидация нового метода определения количественного содержания летучих компонентов, таких как изопропиловый спирт и метилэтилкетон, в алкогольной продукции была проведена входе межлабораторный исследований с участием 49 таможенных лабораторий европейского союза. На основании положительных результатов этих межлабораторных исследований стандарт iliade 453:2024|clen method «определение изопропилового спирта и метилэтилкетона в алкогольнойпродукции методом гх-пид» был принят 13 февраля 2024 года. Разработана система унификациипереноса данных измеренных хроматограмм от участников межлабораторных испытаний в таблицыms excel. Подготовлены возможности для взаимодействия нового метода с платформой labwork, что будет способствовать эффективной реализации проекта cii-scma 2023-09 06. В заключениеважно отметить, что валидация предложенного метода может быть выполнена на основеэкспериментальных данных, получаемых в испытательной лаборатории при валидации методатрадиционного внутреннего стандарта, например, в соответствии регламентом ес 2870/2000 илиметодами анализа oiv-ma-bs-14, oiv-ma-as312-03a, oiv-ma-as315-27. Каких-либо дополнительныхматериальных, финансовых или трудовых затрат при этом не требуется.  

Литература 1. Charapitsa s., et al. The method for direct gas chromatographic determination of acetaldehyde, methanol, and other volatiles using ethanol as a reference substance: application for a wide range of alcoholic beverages. Food analytical methods (2021), vol. 14: p. 2088–2100. Https://doi.org/10.1007/s12161-021-02047-8.  2. Iliade 453:2024 | clen method “determination of isopropyl alcohol and methyl ethyl ketone in alcoholic products by gc-fid”, https://taxation-customs.ec.europa.eu/system/files/2023-09/iliade453_ipa%26mek_v25july2023_clenmethod.pdf . 3. Working with spreadsheets (mso excel, lo calc) in unichrom way. Https://www.unichrom.com/calc/calce.shtml .

Die validierung der methode zur bestimmung des quantitativen gehalts an flüchtigen verbindungen in alkoholischen getränken unter verwendung von ethanol als referenzsubstanz

Es werden die ergebnisse experimenteller untersuchungen neuer methode zur direkten bestimmung flüchtiger verbindungen in weinen und anderen alkoholischen getränken vorgestellt, die sich auf der verwendung von ethylalkohol als referenzsubstanz beruht. Die methode wurde hinsichtlich präzision, richtigkeit, nachweis- und quantifizierungsgrenzen (lod und loq), linearität und robustheit validiert. Die experimentellen untersuchungen wurden mit standardlösungen der flüchtigen komponenten acetaldehyd, methylacetat, ethylacetat, isopropanol, propanol, isobutanol, butanol, isoamylol im konzentrationsbereich von 2 bis 5000 mg/l absolutem alkohol (aa) in wasser durchgeführt.  Der volumetrische gehalt an ethylalkohol in hergestellten ethanol-matrizen betrug von 96 bis 10 %. Die intra- und interday-präzisionswerte lagen zwischen 0,1 und 1,6 %. Die linearitätsparameter r2 waren für alle verbindungen größer als 0,996. Die validierung der neuen methode zur bestimmung des quantitativen gehalts an flüchtigen bestandteilen wie isopropylalkohol und methylethylketon in alkoholischen produkten wurde im jahr 2021 im rahmen eines ringversuches unter beteiligung von 49 zolllabors der europäischen union durchgeführt. Die standardmethode iliade 453:2024 | clen «bestimmung von isopropylalkohol und methylethylketon in alkoholischen getränken durch gc-fid» basierend auf den positiven ergebnissen dieses ringversuches wurde am 13. Februar 2024 verabschiedet. Es wurde ein system entwickelt, um die übertragung gemessener chromatogrammdaten von teilnehmern an ringversuchen in ms-excel-tabellen zu vereinheitlichen. Es wurden möglichkeiten für die interaktion der neuen methode mit der labwork-plattform vorbereitet, die zur effektiven umsetzung des projektes cii-scma 2023-09 06 beitragen wird. Abschließend ist es wichtig anzumerken, dass die validierung der vorgeschlagenen methode auf der grundlage experimenteller daten durchgeführt werden kann, die in einem testellen labor während der validierung einer traditionellen methode mit internem standard gewonnen wurden, beispielsweise gemäß der eu-verordnung 2870/ 2000 oder analysemethoden oiv-ma-bs-14, oiv-ma-as312-03a, oiv-ma-as315-27. Es sind keine zusätzlichen material-, finanz- oder arbeitskosten erforderlich.

Literatur: 1. Charapitsa s., et al. The method for direct gas chromatographic determination of acetaldehyde, methanol, and other volatiles using ethanol as a reference substance: application for a wide range of alcoholic beverages. Food analytical methods (2021), vol. 14: p. 2088–2100. Https://doi.org/10.1007/s12161-021-02047-8.  2. Iliade 453:2024 | clen method “determination of isopropyl alcohol and methyl ethyl ketone in alcoholic products by gc-fid”, https://taxation-customs.ec.europa.eu/system/files/2023-09/iliade453_ipa%26mek_v25july2023_clenmethod.pdf . 3. Working with spreadsheets (mso excel, lo calc) in unichrom way. Https://www.unichrom.com/calc/calce.shtml .

Publication date: November 18, 2024

Issue: OIV 2024

Type: Article

Authors

Siarhei Charapitsa¹, Svetlana Sytova¹, Alena Kavalenka², Anton Kavalenka¹, Aleksander Kolesnov³

¹ Institute for Nuclear Problems of Belarusian State University, Bobruyskaya Str. 11, Minsk, Belarus
² Belarus State University, Nezavisimosti Ave. 4, Minsk, Belarus
³ RUDN University, Miklukho-Maklaya Str. 6, Moscow, Russia

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Tags

IVES Conference Series | OIV | OIV 2024

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