Food Processing: Techniques and Technology Food Processing: Techniques and Technology Техника и технология пищевых производств 2074-9414 2313-1748 96585 10.21603/2074-9414-2025-1-2554 ОРИГИНАЛЬНАЯ СТАТЬЯ ORIGINAL ARTICLE ОРИГИНАЛЬНАЯ СТАТЬЯ Effect of Oak Wood Aging on Chemical Composition of Wheat Distillate Химический состав дистиллята из пшеницы в процессе выдержки в контакте с древесиной дуба https://orcid.org/0000-0001-7735-2942 Шелехова Наталия Викторовна Shelekhova Natalya V. 4953610101@mail.ru https://orcid.org/0000-0001-9297-0554 Абрамова Ирина Михайловна Abramova Irina M. https://orcid.org/0000-0003-3851-4034 Шелехова Тамара Михайловна Shelekhova Tamara M. https://orcid.org/0000-0002-0737-0624 Скворцова Любовь Ивановна Skvortsova Liubov I. https://orcid.org/0000-0003-1266-523X Полтавская Наталья Валериевна Poltavskaya Natalya V. Всероссийский научно-исследовательский институт пищевой биотехнологии Москва Россия Russian Scientific Research Institute of Food Biotechnology Moscow Russian Federation Всероссийский научно-исследовательский институт пищевой биотехнологии Москва Россия Russian Scientific Research Institute of Food Biotechnology Moscow Russian Federation Всероссийский научно-исследовательский институт пищевой биотехнологии Москва Россия Russian Scientific Research Institute of Food Biotechnology Moscow Russian Federation Всероссийский научно-исследовательский институт пищевой биотехнологии Москва Россия Russian Scientific Research Institute of Food Biotechnology Moscow Russian Federation Всероссийский научно-исследовательский институт пищевой биотехнологии Москва Россия Russian Scientific Research Institute of Food Biotechnology Moscow Russian Federation 28 03 2025 28 03 2025 55 1 17 28 20 03 2024 07 05 2024 https://fptt.ru/en/issues/23416/23361/

Приготовление выдержанных зерновых дистиллятов по классической технологии предполагает длительную выдержку в дубовых бочках. Особую актуальность приобретают исследования, направленные на интенсификацию данного процесса. Несмотря на значительный объем научных публикаций, проблема остается недостаточно изученной. Цель данного исследования – расширить и уточнить данные о химическом составе зерновых дистиллятов, находившихся в контакте с древесиной дуба. Объектами исследования послужили образцы невыдержанного зернового дистиллята крепостью 60 % из пшеницы урожая 2023 г. и модельные растворы, приготовленные из невыдержанного зернового дистиллята и промышленной дубовой щепы размером 1,0×0,5 см (Экочипс, Франция) слабой, средней и сильной степени термической обработки, выдержанные в течение 7, 14, 21, 28 суток в защищенном от света месте. В работе реализован подход, обеспечивающий повышение информативности исследования химического состава зерновых дистиллятов, основанный на сочетании методов газовой хроматографии, хромато-масс-спектрометрии, капиллярного электрофореза. В качестве варьируемых факторов были выбраны степень термической обработки дубовой щепы и продолжительность экстракции. С применением комплекса разработанных авторами экспрессных методик был установлен состав летучих органических примесей и ионный состав зерновых дистиллятов. В наибольших концентрациях обнаружены высшие спирты изоамилол, изобутанол и 1-пропанол – до 80 % к сумме зарегистрированных летучих органических примесей. Определены диапазоны варьирования: для изоамилола – 1354,3–1489,3 мг/дм3, для изобутанола – 235,0–261,9 мг/дм3, для 1-пропанола – 119,6–134,9 мг/дм3. Подтвердилось, что тематическая спектральная библиотека Whiskey22 обеспечивает точность идентификации не менее 90 %. В процессе выдержки дистиллята в контакте с древесиной дуба различной степени обжига изменялись не только массовые концентрации, но и перечень идентифицированных ионов. В максимальных концентрациях ацетаты (67,3 мг/дм3), калий (4,2 мг/дм3), фосфаты (2,9 мг/дм3), лактаты (2,4 мг/дм3), хлориды (2,3 мг/дм3) обнаружены в модельном растворе, приготовленном с использованием дубовой щепы сильной степени обжига. Найдены соотношения и обозначены их характерные диапазоны – изоамилол:изобутанол (5,7–5,9), изобутанол:1-пропанол (1,9–2,0), этилкапринат:этиллаурат (2,1–2,3), этилкапринат:этилкаприлат (2,9–3,2). Проведенное исследование выявило перспективность разработанных инструментальных методик определения химического состава зерновых дистиллятов, которые могут быть использованы при разработке новых технологических приемов производства спиртных напитков.

Traditionally, grain distillates are left to age in oak barrels. This process needs intensification, and this problem remains understudied despite numerous scientific publications. The study expands and clarifies the data on the chemical composition of grain distillates after a long-term contact with oak wood. The research featured samples of 60% immature grain distillate from wheat harvested in 2023 and model solutions prepared from immature grain distillate in industrial oak chips (1.0×0.5 cm, Ecochips, France) subjected to a weak, medium, and strong heat treatment modes and stored in the dark for 7, 14, 21, and 28 days. The study relied on a combination of gas chromatography, chromatography / mass spectrometry, and capillary electrophoresis. The thermal treatment mode and extraction time were variables. The authors developed a set of express methods to define the composition of volatile organic impurities and the ionic composition of grain distillates. Isoamylol, isobutanol, and 1-propanol were the most abundant higher alcohols (≤ 80% total volatile organic impurities). The variation ranges were 1 354.3–1 489.3 mg/dm3 for isoamylol, 235.0–261.9 mg/dm3 for isobutanol, and 119.6–134.9 mg/dm3 for 1-propanol. The Whiskey22 thematic spectral library provided a 90% identification accuracy. The aging affected not only the mass concentrations but also the list of ions. In the model solution with the highest degree of thermal treatment, the maximal concentrations belonged to acetates (67.3 mg/dm3), potassium (4.2 mg/dm3), phosphates (2.9 mg/dm3), lactates (2.4 mg/dm3), and chlorides (2.3 mg/dm3). The optimal ratios and ranges were as follows – isoamylol:isobutanol (5.7–5.9), isobutanol:1-propanol (1.9–2.0), ethyl caprate:ethyl laurate (2.1–2.3), and ethyl caprate:ethyl caprylate (2.9–3.2). The new methods proved effective in determining the chemical composition of grain distillates and can be recommended for commercial production of alcoholic beverages

 Зерновой дистиллят химический состав древесина дуба газовая хроматография хромато-масс- спектрометрия капиллярный электрофорез Grain distillate chemical composition oak wood gas chromatography chromatography / mass spectrometry capillary electrophoresis Исследование проведено за счет средств субсидии на выполнение государственного задания (тема № FGMF-2025-0009). The research was part of State Assignment, research topic No. F GMF-2025-0009.

Skurikhin IM. On the chemical processes that occur during aging of cognac spirits in oak barrels. Winemaking and Viticulture of the USSR. 1960;(1):8–15. (In Russ.) Skurikhin IM. On the chemical processes that occur during aging of cognac spirits in oak barrels. Winemaking and Viticulture of the USSR. 1960;(1):8–15. (In Russ.) Okolo CA, Kilcawley KN, O’Connor C. Recent advances in whiskey analysis for authentication, discrimination, and quality control. Comprehensive Reviews in Food Science and Food Safety. 2023;22(6):4957–4992. https://doi.org/10.1111/1541- 4337.13249 Okolo CA, Kilcawley KN, O’Connor C. Recent advances in whiskey analysis for authentication, discrimination, and quality control. Comprehensive Reviews in Food Science and Food Safety. 2023;22(6):4957–4992. https://doi.org/10.1111/1541- 4337.13249 Oganesyants LA, Krikunova LN, Dubinina EV, Shvets SD. Evaluation of the fermentation activators use prospects in the technology of cornelian cherries distillates. Polzunovskiy Vestnik. 2020;(3):24–30. (In Russ.) https://doi.org/10.25712/ASTU.2072-8921.2020.03.004 Oganesyants LA, Krikunova LN, Dubinina EV, Shvets SD. Evaluation of the fermentation activators use prospects in the technology of cornelian cherries distillates. Polzunovskiy Vestnik. 2020;(3):24–30. (In Russ.) https://doi.org/10.25712/ASTU.2072-8921.2020.03.004 Krikunova LN, Dubinina EV, Peschanskaya VA, Obodeeva ON. Acidification in distillation technology. Food Processing: Techniques and Technology. 2022;52(4):694–705. (In Russ.) https://doi.org/10.21603/2074-9414-2022-4-2399 Krikunova LN, Dubinina EV, Peschanskaya VA, Obodeeva ON. Acidification in distillation technology. Food Processing: Techniques and Technology. 2022;52(4):694–705. (In Russ.) https://doi.org/10.21603/2074-9414-2022-4-2399 Lutkov IP, Yermolin DV. Typical properties of beverages with different ethanol content: A comparative analysis. Food Processing: Techniques and Technology. 2023;53(2):404–414. (In Russ.) https://doi.org/10.21603/2074-9414-2023-2-2444 Lutkov IP, Yermolin DV. Typical properties of beverages with different ethanol content: A comparative analysis. Food Processing: Techniques and Technology. 2023;53(2):404–414. (In Russ.) https://doi.org/10.21603/2074-9414-2023-2-2444 Carpena M, Pereira AG, Prieto MA, Simal-Gandara J. Wine aging technology: Fundamental role of wood barrels. Foods. 2020;9(9):1160. https://doi.org/10.3390/foods9091160 Carpena M, Pereira AG, Prieto MA, Simal-Gandara J. Wine aging technology: Fundamental role of wood barrels. Foods. 2020;9(9):1160. https://doi.org/10.3390/foods9091160 Tarko T, Krankowski F, Duda-Chodak A. The impact of compounds extracted from wood on the quality of alcoholic beverages. Molecules. 2023;28(2):620. https://doi.org/10.3390/molecules28020620 Tarko T, Krankowski F, Duda-Chodak A. The impact of compounds extracted from wood on the quality of alcoholic beverages. Molecules. 2023;28(2):620. https://doi.org/10.3390/molecules28020620 Flamini R, Panighel A, De Marchi F. Mass spectrometry in the study of wood compounds released in the barrel-aged wine and spirits. Mass Spectrometry Reviews. 2023;42(4):1174–1220. https://doi.org/10.1002/mas.21754 Flamini R, Panighel A, De Marchi F. Mass spectrometry in the study of wood compounds released in the barrel-aged wine and spirits. Mass Spectrometry Reviews. 2023;42(4):1174–1220. https://doi.org/10.1002/mas.21754 Krikunova LN, Dubinina EV, Sviridov DA, Tomgorova SM. Assessment-based optimization of distillation parameters. Food Processing: Techniques and Technology. 2023;53(2):326–334. (In Russ.) https://doi.org/10.21603/2074- 9414-2023-2-2437 Krikunova LN, Dubinina EV, Sviridov DA, Tomgorova SM. Assessment-based optimization of distillation parameters. Food Processing: Techniques and Technology. 2023;53(2):326–334. (In Russ.) https://doi.org/10.21603/2074- 9414-2023-2-2437 Rimareva LV, Serba EM, Overchenko MB, Shelekhova NV, Ignatova NI, et al. Enzyme complexes for activating yeast generation and ethanol fermentation. Foods and Raw Materials. 2022;10(1):127–136. https://doi.org/10.21603/2308-4057-20 Rimareva LV, Serba EM, Overchenko MB, Shelekhova NV, Ignatova NI, et al. Enzyme complexes for activating yeast generation and ethanol fermentation. Foods and Raw Materials. 2022;10(1):127–136. https://doi.org/10.21603/2308-4057-20 Verges VL, Gollihue JW, Joyce GE, DeBolt S. Lab-scale methodology for new-make bourbon whiskey production. Foods. 2023;12(3):457. https://doi.org/10.3390/ foods12030457 Verges VL, Gollihue JW, Joyce GE, DeBolt S. Lab-scale methodology for new-make bourbon whiskey production. Foods. 2023;12(3):457. https://doi.org/10.3390/ foods12030457 Aylott R, MacKenzie WM. Analytical strategies to confirm the generic authenticity of scotch whisky. Journal of Institute of Brewery. 2010;116:215–229. https://doi.org/10.1002/j.2050-0416.2010.tb00424.x Aylott R, MacKenzie WM. Analytical strategies to confirm the generic authenticity of scotch whisky. Journal of Institute of Brewery. 2010;116:215–229. https://doi.org/10.1002/j.2050-0416.2010.tb00424.x Cody RB, Fukudome T, Ubukata M. Integrated data analysis making use of the total information from gas chromatography and high-resolution time-of-flight mass spectrometry to identify qualitative differences between two whisky samples. Rapid Communications in Mass Spectrometry. 2022;36(3):9225. https://doi.org/10.1002/rcm.9225 Cody RB, Fukudome T, Ubukata M. Integrated data analysis making use of the total information from gas chromatography and high-resolution time-of-flight mass spectrometry to identify qualitative differences between two whisky samples. Rapid Communications in Mass Spectrometry. 2022;36(3):9225. https://doi.org/10.1002/rcm.9225 Gnilomedova NV, Anikina NS, Kolesnov AYu. A review of methodological approaches to authenticating the geographical origin of wines. Food Processing: Techniques and Technology. 2023;53(2):231–246. (In Russ.) https://doi.org/10.21603/2074-9414-2023-2-2429 Gnilomedova NV, Anikina NS, Kolesnov AYu. A review of methodological approaches to authenticating the geographical origin of wines. Food Processing: Techniques and Technology. 2023;53(2):231–246. (In Russ.) https://doi.org/10.21603/2074-9414-2023-2-2429 Cook GT, Dunbar E, Tripney BG, FabeI D. Using carbon isotopes to fight the rise in fraudulent whisky. Radiocarbon. 2020;62(1):51–62. https://doi.org/10.1017/RDC.2019.153 Cook GT, Dunbar E, Tripney BG, FabeI D. Using carbon isotopes to fight the rise in fraudulent whisky. Radiocarbon. 2020;62(1):51–62. https://doi.org/10.1017/RDC.2019.153 Lutkov IP, Makarov AS, Shmigelskaya NA. Quality assessment of young sparkling wines of Crimean indigenous grape varieties. Food Processing: Techniques and Technology. 2024;54(1):1–17. (In Russ.) https://doi.org/10.21603/2074-9414-2024-1-2483 Lutkov IP, Makarov AS, Shmigelskaya NA. Quality assessment of young sparkling wines of Crimean indigenous grape varieties. Food Processing: Techniques and Technology. 2024;54(1):1–17. (In Russ.) https://doi.org/10.21603/2074-9414-2024-1-2483 Sheludko ON, Prakh AV, Chemisova LE, Bakhmetov RN. Effect of wine and grape spirits from table grape varieties on sensory profile of grape beverages. Food Processing: Techniques and Technology. 2024;54(1):18–26. (In Russ.) https:// doi.org/10.21603/2074-9414-2024-1-2484 Sheludko ON, Prakh AV, Chemisova LE, Bakhmetov RN. Effect of wine and grape spirits from table grape varieties on sensory profile of grape beverages. Food Processing: Techniques and Technology. 2024;54(1):18–26. (In Russ.) https:// doi.org/10.21603/2074-9414-2024-1-2484 Li J, Zhang Q, Sun B. Chinese baijiu and whisky: Research reservoirs for flavor and functional food. Foods. 2023; 12(15):2841. https://doi.org/10.3390/foods12152841 Li J, Zhang Q, Sun B. Chinese baijiu and whisky: Research reservoirs for flavor and functional food. Foods. 2023; 12(15):2841. https://doi.org/10.3390/foods12152841 Ashmore PL, DuBois A, Tomasino E, Harbertson JF, Collins TS. Impact of dilution on whisky aroma: A sensory and volatile composition analysis. Foods. 2023;12(6):1276. https://doi.org/10.3390/foods12061276 Ashmore PL, DuBois A, Tomasino E, Harbertson JF, Collins TS. Impact of dilution on whisky aroma: A sensory and volatile composition analysis. Foods. 2023;12(6):1276. https://doi.org/10.3390/foods12061276 Guerrero-Chanivet M, Valcárcel-Muñoz MJ, García-Moreno MV, Guillén-Sánchez DA. Characterization of the aromatic and phenolic profile of five different wood chips used for ageing spirits and wines. Foods. 2020;9(11):1613. https:// doi.org/10.3390/foods9111613 Guerrero-Chanivet M, Valcárcel-Muñoz MJ, García-Moreno MV, Guillén-Sánchez DA. Characterization of the aromatic and phenolic profile of five different wood chips used for ageing spirits and wines. Foods. 2020;9(11):1613. https:// doi.org/10.3390/foods9111613 Shelekhova NV. Express method for the determination of anions in alcoholic beverages based on the CE-CD combination. Sorption and Chromatography Processes. 2023;23(2):199–215. (In Russ.) https://doi.org/10.17308/sorpchrom.2023.23/11144 Shelekhova NV. Express method for the determination of anions in alcoholic beverages based on the CE-CD combination. Sorption and Chromatography Processes. 2023;23(2):199–215. (In Russ.) https://doi.org/10.17308/sorpchrom.2023.23/11144 Shelekhova NV. Express method to determine volatile organic impuritiesin alcoholic distilled beverages basedon a combination of GC/FID and GC/MSD. Sorption and Chromatography Processes. 2022;22(1):58–68. (In Russ.) https://doi.org/ 10.17308/sorpchrom.2022.22/9021 Shelekhova NV. Express method to determine volatile organic impuritiesin alcoholic distilled beverages basedon a combination of GC/FID and GC/MSD. Sorption and Chromatography Processes. 2022;22(1):58–68. (In Russ.) https://doi.org/ 10.17308/sorpchrom.2022.22/9021 Pisarnitsky AF. Flavoring agents in wines and cognacs. Dr. Sci. Biol. Diss. Moscow, 1980. 364 p. (In Russ.) Pisarnitsky AF. Flavoring agents in wines and cognacs. Dr. Sci. Biol. Diss. Moscow, 1980. 364 p. (In Russ.) Karyakin AV, Petrosyan TsL, Dzhanpoladyan LM. Mineral composition of wood in cognac barrels. Winemaking and Viticulture of the USSR. 1972;(4):23–24. (In Russ.) Karyakin AV, Petrosyan TsL, Dzhanpoladyan LM. Mineral composition of wood in cognac barrels. Winemaking and Viticulture of the USSR. 1972;(4):23–24. (In Russ.)