Effect of Protease Combined with Heat Treatment on the Volatile Composition and Aroma Quality in Liqueur Wine.

The aim of this paper was to compare the effects of two clarification methods, protease combined with heat treatment and bentonite, on the aroma quality of liqueur wines, and to identify and analyze the overall differences between the basic components and volatile aroma compounds of liqueur wines after the two treatments by chemical analysis, headspace-solid-phase microextraction-gas chromatography/mass spectrometry (HS-SPME-GC/MS), and orthogonal partial least squares discriminant analysis (OPLS-DA). The results showed that total acidity, volatile acidity and pH in liqueur wines after protease combined with heat treatment were not significantly different from those of the blank control, and the ability to remove proteins was equal to that of the bentonite treatment. A total of 58 volatile aroma compounds were detected by HS-SPME-GC/MS. Compared with the blank control group (44 species, total 108.705 mg/L), 52 (83.233 mg/L) and 50 (120.655 mg/L) aroma compounds were detected in the bentonite and protease combined with heat treatments, respectively. Compared with the control and bentonite treatment, the protease combined with heat treatment significantly increased the total content of aromatic compounds in liqueur wines, and the types and contents of olefins, furans and phenols were higher. Among them, the compounds with major contributions in the protease combined with heat treatment were ionone, ß-damascenone, 3-methyl-1-butanol, alpha-terpineol and limonene, which helped increase the content of terpenoids and enhance the floral and fruit aroma of the wine. Meanwhile, linalool, diethyl succinate, 2-methyl-3-heptanone, butanal diethyl acetal, hexanal and n-octanol were six compounds with high content of aromatic compounds unique to liqueur wines after protease combined with heat treatment. The sensory evaluation results were consistent with the results of aromatic compound detection, and the overall quality was better. The results may provide a reference for further exploration of protease-based clarifiers suitable for liqueur wines.

Traditional Knowledge Evolution over Half of a Century: Local Herbal Resources and Their Changes in the Upper Susa Valley of Northwest Italy.

Susa Valley, located in the Italian Western Alps, has served as a meeting point for cultural, spiritual, and commercial exchange for a long period of history. The valley's role as one of the main connecting routes between south and southwestern Europe resulted in its acquisition of a rich traditional ecological knowledge. However, like other Italian mountainous valleys, this valley has suffered from abandonment and depopulation in the past 50 years. Our study aims to investigate the current ethnobotanical medicinal knowledge in the valley and to compare our findings with a study conducted over 50 years ago in the same area. In 2018, we conducted 30 in-depth semi-structured interviews on medicinal plants and food-medicines used in the Susa Valley. We documented 36 species, of which 21 species were used for medical purposes and 15 species were used as food-medicine. The comparison with the previous study on medicinal herbs conducted in 1970 in the valley demonstrated a significant decrease in both the knowledge and use of medicinal plants, which could be attributed to socioeconomic, cultural, and possibly environmental changes that occurred in the past half-century. Our study highlights several promising species for future use as nutraceuticals, food, and medicinal products, such as Taraxacum officinale, Urtica dioica, and Artemisia genipi.

The Effect of Crataegus Fruit Pre-Treatment and Preservation Methods on the Extractability of Aroma Compounds during Liqueur Production.

The leaves, inflorescences, and fruits of hawthorn have long been known for their therapeutic properties. A wide range of hawthorn products, including liqueurs, are manufactured, due to the technological potential of the raw material as well as the richness of its volatile compounds. This study aimed to determine the effect of the liqueur production method and various methods of fruit preservation on the quantitative and qualitative composition of volatile compounds in the liqueurs produced. Hawthorn fruits saturated with sucrose and non-saturated with sucrose, fresh or preserved through one of three methods: freezing, air-drying, and freeze-drying, were used for liqueur preparation. The samples were analyzed using a gas chromatograph-mass spectrometer. They were found to contain 54 volatile compounds classified into 12 groups of chemicals. All 54 identified volatile compounds were detected in the liqueur made from hawthorn fruits non-saturated with sucrose and preserved by freeze-drying. In this liqueur type, 12 of the identified volatile compounds occurred in the highest concentration when compared to the other treatments. Among all volatiles, the following compounds were present in the analyzed liqueurs in the highest concentrations: dodecanoic acid ethyl ester (11.782 g/100 g), lactones (6.954 g/100 g), five monoterpenes (3.18 g/100 g), two aromatic hydrocarbons (1.293 g/100 g), isobensofuran (0.67 g/100 g), alcohol-2-methyl-2-propanol (0.059 g/100 g), and malonic ester (0.055 g/100 g). Among all analyzed liqueurs, the one made from the fruits non-saturated with sucrose and frozen was characterized by the smallest diversity of volatiles, which were present in the lowest concentrations in that liqueur.

A strategy for rapid discovery of traceable chemical markers in herbal products using MZmine 2 data processing toolbox: A case of Jing Liqueur.

Objective: The quality evaluation of herbal products remains a big challenge. Traceable markers are the core concept of the authentication of herbal products. However, the discovery of traceable markers is labor-intensive and time-consuming. The aim of this study is to develop a convenient approach to rapidly screen the traceable markers for herbal product authentication. Methods: Commercial Jing Liqueur and its 22 species of herbal ingredients were analyzed using HPLC-QTOF-MS and GC-MS to characterize nonvolatile and volatile chemicals. The acquired data were imported into MZmine 2 software for mass detection, chromatogram building, deconvolution and alignment. The aligned data were exported into a csv file and then traceable markers were selected using the built-in filter function in Excel. Finally, the traceable markers were identified by searching against online databases or publications, some of which were confirmed by reference standards. Results: A total of 288 chemical features transferred from herbal materials to Jing Liqueur product were rapidly screened out. Among them, 52 markers detected by HPLC-QTOF-MS were annotated, while nine volatile markers detected by GC-MS were annotated. Moreover, 30 of these markers were confirmed by comparing with reference standards. A chemical fingerprint consisting of traceable markers was finally generated to ensure the authentication and quality consistency of Jing Liqueur. Conclusion: A strategy for rapid discovery of traceable markers in herbal products using MZmine 2 software was developed.

A strategy for rapid discovery of traceable chemical markers in herbal products using MZmine 2 data processing toolbox: A case of Jing Liqueur / 中草药·英文版

Objective: The quality evaluation of herbal products remains a big challenge. Traceable markers are the core concept of the authentication of herbal products. However, the discovery of traceable markers is labor-intensive and time-consuming. The aim of this study is to develop a convenient approach to rapidly screen the traceable markers for herbal product authentication. Methods: Commercial Jing Liqueur and its 22 species of herbal ingredients were analyzed using HPLC-QTOF-MS and GC–MS to characterize nonvolatile and volatile chemicals. The acquired data were imported into MZmine 2 software for mass detection, chromatogram building, deconvolution and alignment. The aligned data were exported into a csv file and then traceable markers were selected using the built-in filter function in Excel. Finally, the traceable markers were identified by searching against online databases or publications, some of which were confirmed by reference standards. Results: A total of 288 chemical features transferred from herbal materials to Jing Liqueur product were rapidly screened out. Among them, 52 markers detected by HPLC-QTOF-MS were annotated, while nine volatile markers detected by GC–MS were annotated. Moreover, 30 of these markers were confirmed by comparing with reference standards. A chemical fingerprint consisting of traceable markers was finally generated to ensure the authentication and quality consistency of Jing Liqueur. Conclusion: A strategy for rapid discovery of traceable markers in herbal products using MZmine 2 software was developed.

Influence of elaboration process on chemical, biological, and sensory characteristics of European pennyroyal liqueurs.

BACKGROUND: Mentha pulegium is an aromatic and medicinal plant used in different Mediterranean herb-based liqueurs, whose phytochemical composition depends on the elaboration technique used. The aim of this work was to investigate differences in the sensory, chemical, and biological characteristics of pennyroyal liqueurs elaborated by hydro-alcoholic (HI) and aqueous (AI) infusions, percolation (P), maceration (M), and distillation (D) techniques, and by the mixture of spirit with pennyroyal essential oil (EO). The volatile composition determined by gas chromatography-mass spectrometry (GC-MS) and gas chromatography coupled to flame ionization detection (GC-FID), the total phenolic (TPC) and flavonoid (TFC) contents, the antioxidant (AC), and enzyme (α-glucosidase, tyrosinase, and acetylcholinesterase) inhibitory capacities, and the sensory analysis by napping, were evaluated in the liqueurs obtained. RESULTS: Monoterpenes and sesquiterpenes were the main volatiles present in liqueurs. The M, P, HI, and AI liqueurs showed the highest TPC, TFC, and AC values; and pulegone, the main hepatotoxic chemotype, was found in concentrations that gave rise to concern. The D and EO liqueurs stand out for their acceptable pulegone content and greater tyrosinase inhibition. Similar liqueur classifications were achieved by sensory analyses, and physico-chemical and biological analyses using multiple factor and principal component analyses, respectively. CONCLUSION: These results are an important contribution to the identification of the most appropriate elaboration conditions for herbal liqueurs with the healthiest chemical composition and functional properties. © 2020 Society of Chemical Industry.

Chemical characterization of eight herbal liqueurs by means of liquid chromatography coupled with ion mobility quadrupole time-of-flight mass spectrometry.

Herbal liqueurs are a large group of diverse alcoholic beverages with an ancient tradition produced by maceration of various herbs and spices and are commonly drunken before or after a meal to aid in the digestion because of their potential functional properties. In the presented work, eight different commercial herbal liqueurs were investigated with regard to their composition of phenolic compounds by liquid chromatography ion mobility quadrupole time-of-flight mass spectrometry (LC-IM-QTOF-MS). This multidimensional analytical platform uses all-ion fragmentation for a deep coverage of the foodome. After an extensive data clean-up, 3225 features were found. 213 features were manually annotated due to the absence of databases and software tools able to consider the drift time or Collison Cross Section (CCS) together with high resolution MS/MS spectra for identification. The identified compounds reflected the large variance between the investigated samples and a wealth of potential bioactive compounds that these liqueurs harbor.

New herbal bitter liqueur with high antioxidant activity and lower sugar content: innovative approach to liqueurs formulations.

Herbal liqueurs are spirits with numerous functional properties, due to the presence of bioactive extractable compounds deriving from herbs. The aim of this study was to obtain new herbal bitter liqueur (HBL) on the basis of twelve selected bitter and aromatic plants extracts, with an optimal sensory profile for consumer acceptance. Also, the determination of optimal sugar content in HBL was done. Furthermore, antioxidant (AO) capacity and total phenolic content (TPC) of HBL was evaluated and compared to similar commercial herbal spirits. Among five tested formulations, assessed by 9-point hedonic scale, HBL with the ratio of bitter and aromatic plants 1:4 was the most acceptable. Ideal concentration of sugar in HBL, determined using a just-about-right scale, was found to be 80.32 g/l of sucrose, which is approximately 20% less than the minimum stipulated by European Union Regulation and several times lower than in the majority of commercial liqueurs. Obtained result indicates the possibility of sugar reduction in liqueurs, and suggests the need to carry out sensory analysis before production of these high-calorie beverages. Radical scavenging ability against DPPH and ABTS radicals, as well as ferric reducing antioxidant power and TPC of HBL were convincingly superior in comparison to similar commercial herbal alcoholic beverages. High correlation coefficients between TPC and other assays applied strongly support the significant role of the polyphenols in the total AO capacity of the HBL and other tested commercial herbal spirits. Headspace GC/MS revealed that the most abundant terpenes were menthone (3.75%), eucalyptol (3.42%) and menthol (3.10%), whereas methanol was present in a small amount (4.97 mg/l).

Quantitative and qualitative analysis of pyrrolizidine alkaloids in liqueurs, elixirs and herbal juices.

Pyrrolizidine alkaloids (PAs and corresponding N-oxides (PANOs)) are known to have adverse health effects. Their toxic effects on liver cells are especially well-documented. In addition, potential carcinogenic and mutagenic effects in chronic exposure via food and/or herbal medicines have been a subject of vivid discussion in the last decade. Liqueurs and elixirs are traditionally used alcoholic extracts made from parts of plants and herbs. PA cross-contamination of the final products seems likely. Hence, this study aims to detect and quantify the PAs in such products in the light of a possible PA-contamination. The PA content was determined in the form of a single sum parameter using HPLC-ESI-MS/MS and a stable isotope-labeled internal standard. Overall, 56 products available at German pharmacies, drugstores, or internet shops were analyzed, comprising in total 38 samples of liqueurs (mainly bitters), 12 samples of plant elixirs and six different herbal juices. The results showed that 9 out of 38 liqueurs were PA-positive (24%). The total amount of PAs ranged from non-detectable to 9.5 µg/kg. Seven out of ten elixirs were PA-positive (70%) with a maximum PA-content of 3121 µg/kg. Four out of six plant juices were PA-positive (67%) with an average of 4.4 µg/kg (PA-positive samples only).The results and potential risks are discussed in the light of recommended portions for daily consumption or daily doses, in association with the detected PA amounts for individual products and product classes.

Artemisia umbelliformis Lam. and Génépi Liqueur: Volatile Profile as Diagnostic Marker for Geographic Origin and To Predict Liqueur Safety.

Artemisia umbelliformis, commonly known as "white génépi", is characterized by a volatile fraction rich in α- and ß-thujones, two monoterpenoids; under European Union (EU) regulations these are limited to 35 mg/L in Artemisia-based beverages because of their recognized activity on the human central nervous system. This study reports the results of an investigation to define the geographical origin and thujone content of individual plants of A. umbelliformis from different geographical sites, cultivated experimentally at a single site, and to predict the thujone content in the resulting liqueurs through their volatile fraction. Headspace solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) and non-separative HS-SPME-MS were used as analytical platforms to create a database suitable for chemometric description and prediction through linear discriminant analysis (LDA). HS-SPME-MS was applied to shorten analysis time. With both approaches, a diagnostic prediction of (i) plant geographical origin and (ii) thujone content of plant-related liqueurs could be made.

New grape stems-based liqueur: Physicochemical and phytochemical evaluation.

A number of traditional liqueurs are obtained by maceration of red fruits in aqueous ethanol liquor, namely sloe berries or sour cherry. On the other hand, the exploration of residual plant material derived from the winery industry (grape (Vitis vinifera L.) stems), which has been regarded as an interesting source of colored and uncolored (poly)phenols, could lead to an industrial alternative to the traditional distilled spirits produced, with valuable physicochemical and phytochemical properties. In the present work, vinification residues (grape stems) were used to produce a new beverage. The evaluation of the physic-chemical characteristics and phytochemical composition as well as the evolution of the determined parameters during maceration (90 and 180 days) allowed a number of interesting bioactive compounds to be identified. This new beverage is a liqueur with a high retention of phenolic compounds (ortho-diphenols, flavanols, flavonols, and anthocyanins), with interesting physic-chemical characteristics, that revealed significant antioxidant activity.