Evaluation of Volatile Metabolites Emitted In-Vivo from Cold-Hardy Grapes during Ripening Using SPME and GC-MS: A Proof-of-Concept

In this research, we propose a novel concept for a non-destructive evaluation of volatiles emitted from ripening grapes using solid-phase microextraction (SPME). This concept is novel to both the traditional vinifera grapes and the cold-hardy cultivars. Our sample models are cold-hardy varieties in the upper Midwest for which many of the basic multiyear grape flavor and wine style data is needed. Non-destructive sampling included a use of polyvinyl fluoride (PVF) chambers temporarily enclosing and concentrating volatiles emitted by a whole cluster of grapes on a vine and a modified 2 mL glass vial for a vacuum-assisted sampling of volatiles from a single grape berry. We used SPME for either sampling in the field or headspace of crushed grapes in the lab and followed with analyses on gas chromatography-mass spectrometry (GC-MS). We have shown that it is feasible to detect volatile organic compounds (VOCs) emitted in-vivo from single grape berries (39 compounds) and whole clusters (44 compounds). Over 110 VOCs were released to headspace from crushed berries. Spatial (vineyard location) and temporal variations in VOC profiles were observed for all four cultivars. However, these changes were not consistent by growing season, by location, within cultivars, or by ripening stage when analyzed by multivariate analyses such as principal component analysis (PCA) and hierarchical cluster analyses (HCA). Research into aroma compounds present in cold-hardy cultivars is essential to the continued growth of the wine industry in cold climates and diversification of agriculture in the upper Midwestern area of the U.S.

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Identification of Floral Scent Profiles in Bearded Irises

Molecules ◽

10.3390/molecules24091773 ◽

2019 ◽

Vol 24 (9) ◽

pp. 1773 ◽

Cited By ~ 4

Author(s):

Yuan Yuan ◽

Ye Sun ◽

Yanchun Zhao ◽

Chungui Liu ◽

Xiulan Chen ◽

...

Keyword(s):

Solid Phase ◽

Floral Scent ◽

Ornamental Plants ◽

Principal Component ◽

Hierarchical Cluster ◽

Gas Chromatography Mass Spectrometry ◽

Methyl Cinnamate ◽

Citronellyl Acetate ◽

Iris Germanica ◽

Scent Profile

Bearded irises are ornamental plants with distinctive floral fragrance grown worldwide. To identify the floral scent profiles, twenty-seven accessions derived from three bearded iris, including Iris. germanica, I. pumila and I. pallida were used to investigate the composition and relative contents of floral scent components by headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC-MS). A total of 219 floral scent components were detected in blooming flowers. The scent profile varied significantly among and within the three investigated species. Principal component analysis (PCA) indicated that terpenes, alcohols and esters contributed the most to the floral scent components and 1-caryophyllene, linalool, citronellol, methyl cinnamate, β-cedrene, thujopsene, methyl myristate, linalyl acetate, isosafrole, nerol, geraniol were identified as the major components. In a hierarchical cluster analysis, twenty-seven accessions could be clustered into six different groups, most of which had representative scent components such as linalool, citronellyl acetate, thujopsene, citronellol, methyl cinnamate and 1-caryophyllene. Our findings provide a theoretical reference for floral scent evaluation and breeding of bearded irises.

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In vivo and in vitro Volatile Constituents of the Flowers of Xylopia aromatica by HS‑SPME/GC-MS

Journal of the Brazilian Chemical Society ◽

10.21577/0103-5053.20210013 ◽

2021 ◽

Author(s):

João Junqueira ◽

Michelle do Nascimento ◽

Lucas da Costa ◽

Lincoln Romualdo ◽

Francisco de Aquino ◽

...

Keyword(s):

Solid Phase ◽

Floral Scent ◽

Principal Component ◽

Gas Chromatography Mass Spectrometry ◽

Large White ◽

Volatile Constituents ◽

Wide Range ◽

First Time

Xylopia aromatica (Lam.) Mart. (Annonaceae) is a typical species from the Brazilian cerrado that presents medicinal properties. The plant is distinguished by its large white flowers which produce a pleasant fragrance. X. aromatica is characterized by a wide range of medicinal application. These characteristics have motivated us to investigate the flowers volatile organic compounds (VOCs) via in vivo and in vitro protocols by a headspace solid-phase microextraction (HS‑SPME) technique combined with gas chromatography-mass spectrometry (HS-SPME/GC‑MS). Four different fibers, extraction times and temperatures were the parameters changed to lead to the maximum profiling of the volatile constituents. Data were analyzed using principal component analysis (PCA). A total of 77 VOCs were extracted from the floral scent, with 52 and 68 extracted from in vivo and in vitro sampling, respectively, of which 48 were reported for the first time in the literature as volatile constituents from X. aromatica flowers. The extraction and identification of VOCs were successfully performed through HS-SPME/GC-MS. The PCA data allowed the identification of parameters that led to the maximum number of VOCs, which were polyacrylate (PA) and carboxen/polydimethylsiloxane (CAR/PDMS) fibers, 60 min extraction time and temperature of 29.0 °C. Among the volatile constituents identified, sesquiterpenes predominated, comprising about 61.04%.

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Biogenic Volatiles Emitted from Four Cold-Hardy Grape Cultivars During Ripening

Data ◽

10.3390/data4010022 ◽

2019 ◽

Vol 4 (1) ◽

pp. 22 ◽

Cited By ~ 3

Author(s):

Somchai Rice ◽

Devin Maurer ◽

Anne Fennell ◽

Murlidhar Dharmadhikari ◽

Jacek Koziel

Keyword(s):

Solid Phase ◽

Grape Berry ◽

Biogenic Emissions ◽

Headspace Collection ◽

Mass Spectral ◽

Grape Berries ◽

Temporal And Spatial Variability ◽

Cold Hardy ◽

Spectral Libraries

In this research dataset, we summarize for the first time volatile organic compounds (VOCs) emitted in vivo from ripening wine grapes. We studied four cold-hardy cultivars grown in the Midwestern U.S.: St. Croix, Frontenac, Marquette, and La Crescent. These cultivars have gained popularity among local growers and winemakers, but still very little is known about their performance compared with long-established V. vinifera grapes. Volatiles were collected using two novel approaches: biogenic emissions from grape clusters on a vine and single grape berries. A third approach was headspace collection of volatiles from crushed grapes. Solid-phase microextraction (SPME) was used to collect volatiles. Vacuum-assisted SPME was used in the case of single grape berry. Collected VOCs were analyzed using separation and identification on a gas chromatograph mass spectrometer (GC-MS). More than 120 VOCs were identified using mass spectral libraries. The dataset provides evidence that detecting biogenic emissions from growing grapes is feasible. The dataset provides a record of temporal and spatial variability of VOCs, many of which could potentially impart aroma and flavor in the wine. The number of VOCs detected followed the order from single berry (the least) to crushed berry (the most). Thus, more information for potential use in harvesting in order to obtain the desired flavor is found in data from crushed grapes.

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Comparison of the Chemical and Sensorial Evaluation of Dark Chocolate Bars

Applied Sciences ◽

10.3390/app11219964 ◽

2021 ◽

Vol 11 (21) ◽

pp. 9964

Author(s):

Ylenia Pieracci ◽

Roberta Ascrizzi ◽

Luisa Pistelli ◽

Guido Flamini

Keyword(s):

Solid Phase ◽

Headspace Analysis ◽

Principal Component ◽

Hierarchical Cluster ◽

Dark Chocolate ◽

Gas Chromatography Mass Spectrometry ◽

Panel Test ◽

Sensorial Evaluation ◽

Consumer's Perception ◽

Chemical Class

As it mimics olfactory perception, headspace analysis is frequently used for examination of products like chocolate, in which aroma is a key feature. Chemical analysis by itself, however, only provides half the picture, as final consumer’s perception cannot be compared to that of a Gas Chromatography-Mass Spectrometry (GC-MS) port, but rather to a panel test assessment. The aim of the present study was the evaluation of combined chemical (by means of headspace solid-phase microextraction and GC-MS) and panel test data (by means of a sensory evaluation operated by 6 untrained panelists) obtained for 24 dark chocolate bars to assess whether these can discriminate between bars from different brands belonging to different commercial segments (hard discount, HD; supermarket, SM; organic bars, BIO). In all samples, with the only exception of one supermarket bar (in which esters exhibited the highest relative abundance), pyrazines were detected as the most abundant chemical class (HD: 56.3–74.2%; BIO: 52.0–76.4%; SM: 31.2–88.9%). Non-terpene alcohols, aldehydes, and esters followed as quantitatively relevant groups of compounds. The obtained data was then subjected to hierarchical cluster (HCA) and principal component (PCA) analysis. The statistical distribution of samples obtained for the chemical data did not match that obtained with panelists’ sensorial data. Moreover, although an overall ability of grouping samples of the same commercial origin was evidenced for hard discount and supermarket bars, no sharp grouping was possible.

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Non-destructive Analysis of Volatile Compounds for Geographical Identification of Rice

10.21203/rs.3.rs-20291/v1 ◽

2020 ◽

Author(s):

Shengying Hu ◽

Hongbo Ren ◽

Song Yong ◽

Siyuan Gao ◽

Li Meng

Keyword(s):

Volatile Compounds ◽

Goodness Of Fit ◽

Solid Phase ◽

Principal Component ◽

Current Method ◽

Rapid Identification ◽

Gas Chromatography Mass Spectrometry ◽

And Cluster Analysis ◽

Non Destructive

Abstract Background In recent years, high-quality rice adulteration has become a serious problem. It is essential to prevent false origin labels and dishonest transactions. However, there is still a lack of rapid identification methods for discriminating rice from different sources. In this study, we developed a method to profile volatile organic compounds (VOCs) using headspace solid phase microextraction (HS-SPME) combined with gas chromatography mass spectrometry (GC-MS). In addition, the identification efficiency of the biomarkers was determined using several multivariate analysis methods. Results Based on the t-test, fold changes and volcano plots, eight typical biomarkers were used based their differential levels. Among them, 2-acetyl-1-pyrroline (2-AP) is the most important source of aroma in rice flavor. Unsupervised analyses, including principal component analysis (PCA) and Cluster analysis, demonstrated the potential for geographic classification of rice between Wuchang and other regions. In addition, partial least squares discriminant analysis (PLS-DA) yielded a goodness of fit of 0.900, a goodness of prediction of 0.853, and a probability of substitution test of 0.012. Random forest (RF) algorithm further strengthened the discriminating ability of volatile compounds. Conclusion In short, the current method can quickly distinguish rice from Wu Chang and other regions, and the research method can facilitate controlling the authenticity and quality of rice.

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Use of solid phase microextraction to identify volatile organic compounds in brazilian wines from different grape varieties

BRAZILIAN JOURNAL OF FOOD TECHNOLOGY ◽

10.1590/1981-6723.05817 ◽

2018 ◽

Vol 21 (0) ◽

Author(s):

Natália Cristina Morais Fernandes ◽

Fátima de Cássia Oliveira Gomes ◽

Cleverson Fernando Garcia ◽

Mariana de Lourdes Almeida Vieira ◽

Ana Maria de Resende Machado

Keyword(s):

Volatile Organic Compounds ◽

Organic Compounds ◽

Solid Phase Microextraction ◽

Solid Phase ◽

Principal Component ◽

Wine Industry ◽

Gas Chromatography Mass Spectrometry ◽

Wine Production ◽

Volatile Organic ◽

Grape Varieties

Abstract The Brazilian wine industry has shown significant growth in recent years and the insertion of new concepts, such as geographical indications as signs of quality, has placed Brazil in tune with the tendencies of world wine production. The aim of this work was to apply the Solid Phase Microextraction technique in combination with Gas Chromatography-Mass Spectrometry to study Brazilian wines made from different grape varieties, in order to separate and identify their volatile organic compounds. These substances were identified by comparisons between the spectra obtained with those presented in the NIST library database, and by comparisons with linear retention indices and literature data. The amounts of the compounds were calculated based on the total peak areas of the chromatograms. Forty-seven volatile compounds were identified and grouped into alcohols, aldehydes, fatty acids, esters, hydrocarbons, ketones and terpenes. Most of them belonged to the ester function, conferring a fruity aroma on the wines. The alcohols may have originated from the yeast metabolism, contributing to the alcoholic and floral aromas. Ethyl lactate, 1-hexanol and diethyl maleate were identified in all the varieties, except Merlot. Decanal, methyl citronellate, (E)-2-hexenyl-3-methylbutyrate were only found in Merlot, while 2,3-butanediol was only present in the Tannat wines. 2-Phenylethanol was present in all varieties and is recognized as giving pleasant rose and honey attributes to wines. This study showed that the volatile profile of red wines is mainly characterized by esters and higher alcohols. The statistical analysis of the comparison of averages showed a greater amount of averages significantly different in the relative areas of Merlot wine. The Principal Component Analysis showed one grouping composed only of the Merlot wine samples, and this was probably related to the existence of the volatile organic compounds that were specifically identified in these wines.

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Spectroscopy as a useful tool for the identification of changes with time in post-mortem vitreous humor for forensic toxicology purposes

Monatshefte für Chemie - Chemical Monthly ◽

10.1007/s00706-021-02786-8 ◽

2021 ◽

Author(s):

Anna Wójtowicz ◽

Agata Mitura ◽

Renata Wietecha-Posłuszny ◽

Rafał Kurczab ◽

Marcin Zawadzki

Keyword(s):

Ir Spectra ◽

Forensic Toxicology ◽

Principal Component ◽

Hierarchical Cluster ◽

Vitreous Humor ◽

Attenuated Total Reflection ◽

Glass Slides ◽

Added Benefit ◽

Ft Ir ◽

Non Destructive

AbstractVitreous humor (VH) is an alternative biological matrix with a great advantage of longer availability for analysis due to the lack of many enzymes. The use of VH in forensic toxicology may have an added benefit, however, this application requires rapid, simple, non-destructive, and relatively portable analytical analysis methods. These requirements may be met by Fourier transform infrared spectroscopy technique (FT-IR) equipped with attenuated total reflection accessory (ATR). FT-IR spectra of vitreous humor samples, deposited on glass slides, were collected and subsequent chemometric data analysis by means of Hierarchical Cluster Analysis and Principal Component Analysis was conducted. Differences between animal and human VH samples and human VH samples stored for diverse periods of time were detected. A kinetic study of changes in the VH composition up to 2 weeks showed the distinction of FT-IR spectra collected on the 1st and 14th day of storage. In addition, data obtained for the most recent human vitreous humor samples—collected 3 and 2 years before the study, presented successful discrimination of all time points studied. The method introduced was unable to detect mephedrone addition to VH in the concentration of 10 µg/cm3. Graphic abstract

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Characterization of the Volatile Profile of Cultivated and Wild-Type Italian Celery (Apium graveolens L.) Varieties by HS-SPME/GC-MS

Applied Sciences ◽

10.3390/app11135855 ◽

2021 ◽

Vol 11 (13) ◽

pp. 5855

Author(s):

Samantha Reale ◽

Valter Di Cecco ◽

Francesca Di Donato ◽

Luciano Di Martino ◽

Aurelio Manzi ◽

...

Keyword(s):

Solid Phase ◽

Principal Component ◽

Apium Graveolens ◽

Gas Chromatography Mass Spectrometry ◽

Bioactive Metabolites ◽

Chemical Components ◽

Volatile Profile ◽

Wild Type ◽

Multivariate Statistical ◽

Clear Differentiation

Celery (Apium graveolens L.) is a vegetable belonging to the Apiaceae family that is widely used for its distinct flavor and contains a variety of bioactive metabolites with healthy properties. Some celery ecotypes cultivated in specific territories of Italy have recently attracted the attention of consumers and scientists because of their peculiar sensorial and nutritional properties. In this work, the volatile profiles of white celery “Sedano Bianco di Sperlonga” Protected Geographical Indication (PGI) ecotype, black celery “Sedano Nero di Torricella Peligna” and wild-type celery were investigated using head-space solid-phase microextraction combined with gas-chromatography/mass spectrometry (HS-SPME/GC-MS) and compared to that of the common ribbed celery. Exploratory multivariate statistical analyses were conducted using principal component analysis (PCA) on HS-SPME/GC-MS patterns, separately collected from celery leaves and petioles, to assess similarity/dissimilarity in the flavor composition of the investigated varieties. PCA revealed a clear differentiation of wild-type celery from the cultivated varieties. Among the cultivated varieties, black celery “Sedano Nero di Torricella Peligna” exhibited a significantly different composition in volatile profile in both leaves and petioles compared to the white celery and the prevalent commercial variety. The chemical components of aroma, potentially useful for the classification of celery according to the variety/origin, were identified.

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Influences of Smoking in Traditional and Industrial Conditions on Flavour Profile of Harbin Red Sausages by Comprehensive Two-Dimensional Gas Chromatography Mass Spectrometry

Foods ◽

10.3390/foods10061180 ◽

2021 ◽

Vol 10 (6) ◽

pp. 1180

Author(s):

Xiaoyu Yin ◽

Qian Chen ◽

Qian Liu ◽

Yan Wang ◽

Baohua Kong

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Volatile Compounds ◽

Solid Phase ◽

Meat Products ◽

Principal Component ◽

Quality Characteristics ◽

Gas Chromatography Mass Spectrometry ◽

Two Dimensional ◽

Chromatography Mass Spectrometry

Smoking is mainly used to impart desirable flavour, colour and texture to the products. Various food smoking methods can be divided into traditional and industrial methods. The influences of three different smoking methods, including traditional smouldering smoke (TSS), industrial smouldering smoke (ISS) and industrial liquid smoke (ILS), on quality characteristics, sensory attributes and flavour profiles of Harbin red sausages were studied. The smoking methods had significant effects on the moisture content (55.74–61.72 g/100 g), L*-value (53.85–57.61), a*-value (11.97–13.15), b*-value (12.19–12.92), hardness (24.25–29.17 N) and chewiness (13.42–17.32). A total of 86 volatile compounds were identified by headspace solid phase microextraction combined with comprehensive two-dimensional gas chromatography mass spectrometry (GC × GC-qMS). Among them, phenolic compounds were the most abundant compounds in the all sausages. Compared with sausages smoked with smouldering smoke, the ILS sausages showed the highest content of volatile compounds, especially phenols, alcohols, aldehydes and ketones. Principal component analysis showed that the sausages smoked with different methods had a good separation based on the quality characteristics and GC × GC-qMS data. These results will facilitate optimising the smoking methods in the industrial production of smoked meat products.

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Changes in Phenols, Polysaccharides and Volatile Profiles of Noni (Morinda citrifolia L.) Juice during Fermentation

Molecules ◽

10.3390/molecules26092604 ◽

2021 ◽

Vol 26 (9) ◽

pp. 2604

Author(s):

Zhulin Wang ◽

Rong Dou ◽

Ruili Yang ◽

Kun Cai ◽

Congfa Li ◽

...

Keyword(s):

Octanoic Acid ◽

Solid Phase ◽

Principal Component ◽

Hexanoic Acid ◽

Morinda Citrifolia ◽

Gas Chromatography Mass Spectrometry ◽

Aroma Characteristics ◽

Volatile Profiles ◽

The Difference ◽

Aroma Components

The change in phenols, polysaccharides and volatile profiles of noni juice from laboratory- and factory-scale fermentation was analyzed during a 63-day fermentation process. The phenol and polysaccharide contents and aroma characteristics clearly changed according to fermentation scale and time conditions. The flavonoid content in noni juice gradually increased with fermentation. Seventy-three volatile compounds were identified by solid-phase microextraction coupled with gas chromatography–mass spectrometry (SPME-GC-MS). Methyl hexanoate, 3-methyl-3-buten-1-ol, octanoic acid, hexanoic acid and 2-heptanone were found to be the main aroma components of fresh and fermented noni juice. A decrease in octanoic acid and hexanoic acid contents resulted in the less pungent aroma in noni juice from factory-scale fermentation. The results of principal component analysis of the electronic nose suggested that the difference in nitrogen oxide, alkanes, alcohols, and aromatic and sulfur compounds, contributed to the discrimination of noni juice from different fermentation times and scales.

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