Isolation of Anthocyanins by high-speed countercurrent chromatography and application of the color activity concept to different varieties of red grape pomace from Macedonia

Anthocyanins of Macedonian grape pomace from three varieties “Pinot noir”, “Merlot” and “Vranec” were isolated by high speed countercurrent chromatography. After purification of the fractions by means of preparative high performance liquid chromatography the structures of isolated pigments were elucidated by electrospray ionization multiple mass spectrometry (ESI-MSn) and nuclear magnetic resonance (NMR) spectroscopy. The major anthocyanin malvidin-3-glucoside and the minor pigments delphinidin-3-glucoside, cyaniding-3-glucoside, petunidin-3-glucoside, and malvidin-3-p-coumarоyl-glucoside were isolated. The “Color activity concept” was applied and visual detection thresholds of isolated anthocyanins were determined. The results of the “color activity value” of the isolated pigments and their detection thresholds were in good agreement with the color shade of the different varieties of red grape pomace

Characteristics of Petit verdot grape variety (Vitis vinifera L.) grown in Tikveš vineyards

Research is being performed to the variety of Petit verdot. The vineyards are sited on the Lepovo-Tikveš vineyards, in the property of Bovin winery. Plantation is started in 2008 with certified plantation material, 2.4 m planting distance between rows, and 1.0 m distance between vines in a row. The training system is Guyot two arms, with 20 eyelets leaving the vine. Some optimal agro-technical and ampelo-technical measures are applied. The plantation is under drip irrigation system. During the research period (2011– 2012) the following items were included: yield (kg/vine), chemical composition of grape must (sugar, total acid, pH), and chemical analysis of wine. The results show considerable variation in yield interest (14.48), which is due to the age of the crop, whether it is in the second (2011) or in the third (2012) year of birth. The must contains 230 g/L sugar and 5.5 g/L total acids, average for the test period. The wine has a high content of extract (40 g/L) and 13.11% vol alcohol, which is due to selective grape harvesting and the way of vinification (winemaking)

Incorporating standardised drift-tube ion mobility to enhance non-targeted assessment of the wine metabolome (LC×IM-MS)

Liquid chromatography with drift-tube ion mobility spectrometry-mass spectrometry (LCxIM-MS) is emerging as a powerful addition to existing LC-MS workflows for addressing a diverse range of metabolomics-related questions [1,2]. Importantly, excellent precision under repeatability and reproducibility conditions of drift-tube IM separations [3] supports the development of non-targeted approaches for complex metabolome assessment such as wine characterisation [4]. In this work, fundamentals of this new analytical metabolomics approach are introduced and application to the analysis of 90 authentic red and white wine samples originating from Macedonia is presented. Following measurements, intersample alignment of metabolites using non-targeted extraction and three-dimensional alignment of molecular features (retention time, collision cross section, and high-resolution mass spectra) provides confidence for metabolite identity confirmation. Applying a fingerprinting metabolomics workflow allows statistical assessment of the influence of geographic region, variety, and age. This approach is a state-of-the-art tool to assess wine chemodiversity and is particularly beneficial for the discovery of wine biomarkers and establishing product authenticity based on development of fingerprint libraries

Rapid Determination of Trace Elements in Macedonian Grape Brandies for Their Characterization and Safety Evaluation

A graphite furnace atomic absorption spectrometry (GFAAS) was used for determination of trace elements (Cd, Cr, Cu, Fe, Mn, Ni, Pb, and Zn) in Brakija^ samples, a grape brandy traditionally produced in Republic of Macedonia by distillation of grape pomace or wine, for characterization and safety evaluation. Cd, Pb, Cr, and Ni were determined directly, while Cu, Fe, Mn, and Zn were quantified after appropriate dilution. The calibration curves of all elements were linear with correlation coefficients (R 2 ) ranging from 0.9995 to 0.9998. The accuracy of the method was checked with a standard addition method showing good repeatability and reproducibility (relative standard deviation (RSD) <10 %). Relationship between several metal concentrations (Cu, Fe, Mn, Zn) in brandies and distillation system (homemade/industrial) on one side and aging mode (oak barrels/oak chips) on the other side were demonstrated. Two homemade brandies showed Cu, Fe, and Zn concentrations higher than industrial distillates and thus were found to be not safe for consumption because of Cu and Zn over the maximum allowed values. For the industrially produced brandies, Mn was identified to be a suitable marker related to aging with oak chips regardless variety, while Cu a marker for the influence of oak chip type

Нови стилови на вина од сортите Темјаника, Станушина и Смедеревка

На просторите на денешна Македонија има многу вековна традиција за производство на вино. Меденото вино претставува придизвик за нови модерни вински правци. Овa истражување се фокусира на примена на модерното производство на вино и развој на традиционални и нови стилови на вино, со користење на локални сорти грозје (Темјаника и Смедеревка) и автохтона сорта (Станушина) од Тиквешкото виногорје Македонија. За прв пат се произведува и проучува нов стил на вино, добиено со додавање на мед пред ферментација, со цел да се произведат нови карактеристични медени вина со поинтензивна арома, вкус и тело. Примарната проценка на хемискиот состав на произведените вина вклучува определување на општи параметри за квалитет на виното, анализа на полифеноли и антиоксиданти. Овој сеопфатен пристап овозможува да се проучи влијанието на новите процеси на производство на вино во споредба со традиционалните. Развојот на современата винификација со примена на нов стил на локаните сорти ќе придонесе за развој на винската економија и туризмот во земјата, а со тоа ќе се зголеми значењето и препознавањето на локалните македонски сорти

Honey wine, new wine style from Temjanika, Smederevka аnd Stanušina varieties

The aim of this study was to apply a modern vinification technique and develop a new wine style of local grape varieties, Temjanika and Smederevka, as well as autochthonous Stanušina variety, all grown in the Tikveš wine region. Wines were produced with addition of two doses (20 and 40 g/L) of honey before fermentation in order to study its influence on the overall quality. The following chemical parameters were determined: alcohol, density, pH, total acidity, total sugars, glycerol, glucose, fructose, sucrose, acetic acid, tartaric acid, lactic acid and malic acid, applying FTIR analyses. Spectrophotometric determination included analysis of polyphenols and antioxidant activity. It was noticed that addition of honey influenced the content of alcohol, total sugars, as well as individual glucose and fructose, observing increasing of their content. Moreover, slightly increased total phenolics content was noticed in wines fermented with honey and almost no influence of honey was observed on the antioxidant activity, glycerol, organic acids and acetic acid content. In general, addition of honey in grape mash before fermentation could be considered as a possible technique for increasing the wine quality and stability, especially of varieties with lower quality potential. Keywords: honey wine, Temjanika, Smederevska, Stanušina, FTIR, spectrophotometry

Влијание на времето на мацерација врз ароматичниот профил на вина од сортата Вранец

Вранец е една од најважните сорти на црвено винско грозје во Република Македонија што се одгледува во сите виногорја, но главно е најзастапено во Тиквешкото Виногорје. Во оваа магистерска работа беа испитувани вина од сортата вранец, произведени со различни периоди на мацерација (4, 7, 14 и 30 дена), во присуство на ензим и дабов чипс за време на ферментацијата, со цел да се утврди влијанието на условите за винификација врз профилот на аромата на овие вина. Екстракцијата на ароми беше извршена со примена на цврсто-фазна микроекстракција поврзана со автоматски headspace (HS-SPME), во комбинација со гасна хроматографија и масен детектор (GC-MS). Применетата техника е многу ефикасна техника за одделување, екстракција и за сепарација на ароматични соединенија во виното. Беа идентификувани вкупно 63 ароматични соединенија во вината вранец, кои главно припаѓаат на следниве групи соединенија: естри, алкохоли, масни киселини, алдехиди, кетони и сулфурни соединенија. Беше заклучено дека содржината на ароматичните соединенија главно зависи од времето на мацерација, при што беше забележана зголемена содржина на алкохоли, естри и масни киселини со зголемување на времето на мацерација, од четвртиот до седмиот ден. Присуството на дабов чипс за време на ферментацијата го подобрува формирањето на ароми во вината. Тестот StudentNewman-Keuls беше применет за да се утврдат можните значителни разлики помеѓу вината. Дополнително, беше применета карактеристична векторска анализа за да се утврди разделување и групирање на вината според времето на мацерација и третманот со дабов чипс. Клучни зборови: арома, вино, мацерација, ензим, дабов чипс, HS-SPMEGC-MS, вране

Isolation of Anthocyanins by high-speed countercurrent chromatography and application of the color activity concept to different varieties of red grape pomace from Macedonia

Anthocyanins of Macedonian grape pomace from three varieties “Pinot noir”, “Merlot” and “Vranec” were isolated by high speed countercurrent chromatography. After purification of the fractions by means of preparative high performance liquid chromatography the structures of isolated pigments were elucidated by electrospray ionization multiple mass spectrometry (ESI-MSn) and nuclear magnetic resonance (NMR) spectroscopy. The major anthocyanin malvidin-3-glucoside and the minor pigments delphinidin-3-glucoside, cyaniding-3-glucoside, petunidin-3-glucoside, and malvidin-3-p-coumarоyl-glucoside were isolated. The “Color activity concept” was applied and visual detection thresholds of isolated anthocyanins were determined. The results of the “color activity value” of the isolated pigments and their detection thresholds were in good agreement with the color shade of the different varieties of red grape pomace

Characteristics of Petit verdot grape variety (Vitis vinifera L.) grown in Tikveš vineyards

Research is being performed to the variety of Petit verdot. The vineyards are sited on the Lepovo-Tikveš vineyards, in the property of Bovin winery. Plantation is started in 2008 with certified plantation material, 2.4 m planting distance between rows, and 1.0 m distance between vines in a row. The training system is Guyot two arms, with 20 eyelets leaving the vine. Some optimal agro-technical and ampelo-technical measures are applied. The plantation is under drip irrigation system. During the research period (2011– 2012) the following items were included: yield (kg/vine), chemical composition of grape must (sugar, total acid, pH), and chemical analysis of wine. The results show considerable variation in yield interest (14.48), which is due to the age of the crop, whether it is in the second (2011) or in the third (2012) year of birth. The must contains 230 g/L sugar and 5.5 g/L total acids, average for the test period. The wine has a high content of extract (40 g/L) and 13.11% vol alcohol, which is due to selective grape harvesting and the way of vinification (winemaking)