Non-volatile cysteine sulphoxides and volatile organosulphur compounds in cloves of garlic (Allium sativum L.) and elephant garlic (Allium ampeloprasum L.) local accessions from northern and central Italy.

BACKGROUND: Garlic (Allium sativum L.) and other species of genus Allium are popular vegetables and food seasonings, owing to their spicy flavour and richness in health-promoting compounds. Several local garlic types are still grown on a small scale in different Italian regions, not being however yet properly characterized for their chemical composition. RESULTS: In the present investigation ten garlic and four elephant garlic (Allium ampeloprasum L.) populations cultivated in northern and central Italy were evaluated for their alk(en)yl cysteine sulphoxide (ACSO) and volatile compound profiles. Three non-volatile ACSOs (methiin, alliin, and isoalliin) and 27 volatile compounds were identified and quantified. A high and significant within-type variability was detected, with total ACSOs in the range 2759-5756, 4533-15 520, and 6565-10 643 mg kg-1 of fresh weight (f.w.). in elephant, white and red garlic, respectively. Elephant garlic showed a total sulphoxide content and a relative alliin amount significantly lower than white and red garlic. Remarkable within-type differences were also assessed for volatile compound content, ranging 260-599, 333-981, and 618-845 mg kg-1 f.w. in elephant, white, and red garlic, respectively. Diallyl trisulphide was the major individual compound, accounting for more than 0.30 mg mg-1 of volatiles in all the analysed samples. The three garlic types were clearly separated by discriminant analysis of analytical traits. CONCLUSION: This study investigated for the first time different Italian garlic and elephant garlic populations with respect to non-volatile and volatile organosulphur compound content, allowing the possibility of selecting garlic accessions according to the bioactive content. © 2022 Society of Chemical Industry.

Extraction of volatile organic compounds from leaves of Ambrosia artemisiifolia L. and Artemisia annua L. by headspace-solid phase micro extraction and simultaneous distillation extraction and analysis by gas chromatography/mass spectrometry.

This study was designed to analyze the volatile organic compounds in the leaves of Ambrosia artemisiifolia L. and Artemisia annua L. from Korea. For extraction of volatile compounds, headspace-solid phase micro extraction (HS-SPME) and simultaneous distillation extraction (SDE) were applied and analyzed by gas chromatography/mass spectrometry (GC/MS). From the results, SDE extraction was found to give the highest concentration of volatile compounds with an average concentration of 1,237.79 mg/kg for A. annua L. leaves compared to 1,122.73 mg/kg by HS-SPME technique. A total of 116 volatile organic compounds were identified, including 76 similar volatile organic compounds detected by both the methods of extraction in leaves of subject species at varying concentrations. Among these 33 volatile organic compounds were reported for the first time from the subject plant species. Thus the present research findings extend the characterization of volatile organic compounds from leaves of A. annua L. and A. artemisiifolia L. species and reported some distinguishing compounds which may be used for their discrimination.

Analysis of volatile compounds in rooibos tea (Aspalathus linearis) using different extraction methods and their relationship with human sensory perception.

This study aimed to comparatively analyze the volatile flavor of rooibos tea (Aspalathus linearis) obtained by two commonly used flavor extraction methods, simultaneous distillation-extraction (SDE) and steam distillation under reduced pressure (DRP). The tea obtained by the two extraction methods, were analyzed by gas chromatography-mass spectrometry to identify volatile aroma-related compounds. Descriptive sensory analysis of the extracted rooibos tea flavor was carried out by a trained panel (n = 7). Fifty volatile compounds were identified, including 26 and 25 aroma-active compounds by SDE (45.9 µg/g) and DRP (37.5 µg/g), respectively. SDE recovered larger quantities of alcohols, acids, and esters, whereas DRP was useful for analyzing thermally unstable volatile compounds, including various alcohols, aldehydes, and hydrocarbons. Descriptive sensory analysis revealed that ketones and phenolic compounds may be responsible for the sensory attributes woody and grassy green, whereas the aldehydes and acidic compounds may contribute to floral and fruity.

Analysis of aroma-active volatiles in an SDE extract of white tea.

White tea is a famous Chinese tea that is cooked at boiling point before drinking. The simultaneous distillation-extraction (SDE) was used to collect volatile compounds during tea cooking. The SDE extract was dominated with green, floral, roasted and woody notes, and weak sweet note. There were 32 volatile compounds identified via gas chromatography-mass spectrometry analysis, and 19 of them had strong fragrance based on the gas chromatography-olfactometry analyzed results. Hexanal, 2-hexenal, cis-3-hexen-1-ol, and camphene were the main contributors to the green note. The floral note was mainly contributed by 2-hexanone, benzeneacetaldehyde, trans-linalool oxide, and linalool, and the sweet note was induced by trans-ß-damascenone. The roasted note was mainly contributed by 2-pentyl-furan. The woody note was mainly contributed by trans-α-ionone and trans-ß-ionone. Four putative reaction pathways, including amino acid degradation, carotene degradation, Maillard reaction, and glycosides hydrolysis, were figured out to explain the generation of aromatic-active volatiles at high temperatures. This study added our knowledge on tea aroma under cooking as well as other thermal treatments.

Comparison of SDE and SPME for the analysis of volatile compounds in butters.

The current study aimed to compare the effectiveness of two extraction techniques, namely simultaneous distillation-extraction (SDE) and solid-phase microextraction (SPME), in evaluating key aroma compounds in butters. Volatile compounds' contributions to butter flavors were evaluated employing both odor active values (OAVs) and gas chromatography olfactometry (GC-O). The results showed that the species of volatile compounds detected by the two techniques were almost the same, whereas their volatile profiles were obviously different. Using SDE method, methyl ketones took up the largest proportion of the volatile compounds, followed by fatty acids. Using SPME method, the most abundant compounds were the fatty acids, followed by lactones. More methyl ketones were detected in the SDE extract owing to lipid degradation as a consequence of the high temperature during extraction. Lactones were considered to be the key aroma compounds, especially δ-decalactone, which was identified by both OAVs and GC-O.

Analysis of Volatile Constituents in Platostoma palustre (Blume) Using Headspace Solid-Phase Microextraction and Simultaneous Distillation-Extraction.

Hsian-tsao (Platostoma palustre Blume) is a traditional Taiwanese food. It is admired by many consumers, especially in summer, because of its aroma and taste. This study reports the analysis of the volatile components present in eight varieties of Hsian-tsao using headspace solid-phase microextraction (HS-SPME) and simultaneous distillation-extraction (SDE) coupled with gas chromatography (GC) and gas chromatography-mass spectrometry (GC/MS). HS-SPME is a non-heating method, and the results show relatively true values of the samples during flavor isolation. However, it is a kind of headspace analysis that has the disadvantage of a lower detection ability to relatively higher molecular weight compounds; also, the data are not quantitative, but instead are used for comparison. The SDE method uses distillation 2 h for flavor isolation; therefore, it quantitatively identifies more volatile compounds in the samples while the samples withstand heating. Both methods were used in this study to investigate information about the samples. The results showed that Nongshi No. 1 had the highest total quantity of volatile components using HS-SPME, whereas SDE indicated that Taoyuan Mesona 1301 (TYM1301) had the highest volatile concentration. Using the two extraction methods, 120 volatile components were identified. Fifty-six volatile components were identified using HS-SPME, and the main volatile compounds were α-pinene, ß-pinene, and limonene. A total of 108 volatile components were identified using SDE, and the main volatile compounds were α-bisabolol, ß-caryophyllene, and caryophyllene oxide. Compared with SDE, HS-SPME sampling extracted a significantly higher amount of monoterpenes and had a poorer detection of less volatile compounds, such as sesquiterpenes, terpene alcohols, and terpene oxide.

Chemical Composition and Antimicrobial Activities of Artemisia argyi Lévl. et Vant Essential Oils Extracted by Simultaneous Distillation-Extraction, Subcritical Extraction and Hydrodistillation.

Artemisia argyi Lévl. et Vant essential oil could be used as a good antimicrobial flavouring agent and applied in the food industry. In this study, three methods, including simultaneous distillation-extraction (SDE), subcritical extraction and hydrodistillation, were applied to extract A. argyi essential oil. Compared with subcritical extraction (1%) and hydrodistillation (0.5%), SDE gave a higher yield (1.2%). Components of the essential oils were analysed with gas chromatography-mass spectrometry (GC-MS), and the most abundant ingredients were caryophyllene oxide, neointermedeol, borneol, α-thujone and ß-caryophyllene. These five components accounted for 82.93%, 40.90% and 40.33% for SDE, subcritical extraction, and hydrodistillation, respectively. Based on agar disc diffusion and minimum inhibitory concentration (MIC) assays, SDE oil showed a significant inhibitory effect towards Listeria monocytogenes, Escherichia coli, Proteus vulgaris, Salmonella enteritidis and Aspergillus niger. Furthermore, electron microscope observations (SEM) confirmed that SDE oil could obviously deform cell morphology and destroy the structure of cell walls. Performances showed that SDE was a promising process for extracting A. argyi essential oil with both high yield and antimicrobial activity.

[Determination of 10 volatile N-nitrosamines in meat products by gas chromatography-tandem mass spectrometry].

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was established for the determination of 10 volatile N-nitrosamines in meat products. The meat samples were extracted by simultaneous distillation extraction (SDE), and then a cleanup step involving the frozen fat removal method was applied. The analytes were quantified by the external standard method in multiple reaction monitoring (MRM) mode. Under the optimized conditions, the correlation coefficients of the standard calibration curves were greater than 0.99 in the range of 1.00-1000 µg/L. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were 0.01-0.02 µg/kg and 0.04-0.07 µg/kg, respectively. The average spiked recoveries of the 10 volatile N-nitrosamines were 74.8%-94.3% at spiked levels of LOQ level, 1.0 and 2.0 µg/kg,and the relative standard deviations were less than 8.3%. Six volatile N-nitrosamines (N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine (NDEA), N-nitrosopyrrolidine (NPYR), N-nitrosopiperidine (NPIP), N-nitrosodibutylamine (NDBA) and N-nitrosodi-n-propylamine (NDPA)) were detected in different types of meat products, and each volatile N-nitrosamine in pickled meat products had the highest detection values. The developed method has the advantages of simplicity, sufficient extraction, high sensitivity, and low reagent dosage, in addition to proving suitable for the daily testing requirements of a large number of samples in the laboratory.

Discrimination of Aroma Characteristics for Cubeb Berries by Sensomics Approach with Chemometrics.

The dried cubeb berries are widely used as medicinal herb and spicy condiment with special flavor. However, there is a significant definition discrepancy for cubeb berries. In this study, an efficient analytical method to characterize and discriminate two popular cubeb fruits (Litsea cubeba and Piper cubeba) was established. The aroma profiles of cubeb berries were evaluated by different extraction methods including hydro-distillation, simultaneous distillation/extraction, and solid-phase micro-extraction followed by gas chromatography-mass spectrometry-olfactometry (GC-MS-O). In total, 90 volatile compounds were identified by HD, SDE, and SPME combined with GC-MS. Principal component analysis was further applied and discriminated ambiguous cubeb berries by their unique aromas: Litsea cubeba was characterized by higher level of d-limonene ("fruit, citrus"), citral ("fruit, lemon") and dodecanoic acid; α-cubebene ("herb") was identified as a marker compound for Piper cubeba with higher camphor ("camphoraceous"), and linalool ("flower"). Flavor fingerprint combined with PCA could be applied as a promising method for identification of cubeb fruits and quality control for food and medicinal industries.

Effects of CO2 pretreatment on the volatile compounds of dried Chinese jujube (Zizyphus jujuba Miller)

Abstract The aim of this study was to investigate whether anaerobic metabolites could induce volatile compounds and improve aroma of dried jujube (Ziziphus jujuba Miller). Jujube fruits were incubated in a polyvinyl chloride bag containing 5% CO2 and 95% N2 for up to 168 h at 25 °C and 3 samples were randomly removed every 6 h and oven dried to a moisture content of ≅ 20%. The volatile compounds of control and 5% CO2-pretreated Chinese jujube fruits were extracted by simultaneous distillation extraction and identified by gas chromatography-mass spectrometry(GC-MS). The acetaldehyde and ethanol contents were determined by gas chromatography (GC). The results indicated that a large accumulation of acetaldehyde and ethanol caused changes in aroma composition of dried jujube products and 5% CO2 pretreatment led to an increase in the levels of some compounds, particularly esters, acetaldehydes, and ethanol, whereas the amount of acids were decreased significantly. Principal component analysis showed that integrative scores of 5% CO2 pretreatment at 120 h were the highest, and aroma quality was better than that of the control. Relatively low concentrations of anaerobic respiration metabolites are good for jujube fruit aroma composition.

GC-MS Profiling of Volatile Components in Different Fermentation Products of Cordyceps Sinensis Mycelia.

The fermentation products of Cordyceps sinensis (C. sinensis) mycelia are sustainable substitutes for natural C. sinensis. However, the volatile compositions of the commercial products are still unclear. In this paper, we have developed a simultaneous distillation-extraction (SDE) and gas chromatography-mass spectrometry (GC-MS) method for the profiling of volatile components in five fermentation products. A total of 64, 39, 56, 52, and 44 components were identified in the essential oils of Jinshuibao capsule (JSBC), Bailing capsule (BLC), Zhiling capsule (ZLC), Ningxinbao capsule (NXBC), and Xinganbao capsule (XGBC), respectively. 5,6-Dihydro-6-pentyl-2H-pyran-2-one (massoia lactone) was first discovered as the dominant component in JSBC volatiles. Fatty acids including palmitic acid (C16:0) and linoleic acid (C18:2) were also found to be major volatile compositions of the fermentation products. The multivariate partial least squares-discriminant analysis (PLS-DA) showed a clear discrimination among the different commercial products as well as the counterfeits. This study may provide further chemical evidences for the quality evaluation of the fermentation products of C. sinensis mycelia.

Analysis of chemical composition of volatile oil in Ramulus Mori by GC-MS / 国际药学研究杂志

Objective To extract the volatile oil of Ramulus Mori and analyze the chemical composition of the volatile oil. Methods The volatile oil of Ramulus Mori was extracted by simultaneous distillation extraction(SDE)and direct distillation extraction(DDE)method, and the chemical composition was identified by GC-MS. Results Nineteen compounds were identified in the volatile oil extracted by SDE, which accounted for 94.49% of the total amount of detection. There were alkyl, acids, aldehydes, ketones, esters, alcohols and other substances in the volatile oil. And 16 compounds were determined in the volatile oil extracted by DDE, accounting for 97.12% of the total amount detected. There were furan, carboxylic acids, esters, aldehydes, alcohols, phenols, ketones, alkene and acyl halide. The chemical compositions of the volatile oil extracted by SDE were more than those extracted by DDE. Conclusion The chemical constituents of volatile oil of Ramulus Mori can be more fully identified by the combination of the two extraction methods.

Analysis of chemical composition of volatile oil in Ramulus Mori by GC-MS / 国际药学研究杂志

Objective To extract the volatile oil of Ramulus Mori and analyze the chemical composition of the volatile oil. Methods The volatile oil of Ramulus Mori was extracted by simultaneous distillation extraction(SDE)and direct distillation extrac?tion(DDE)method,and the chemical composition was identified by GC-MS. Results Nineteen compounds were identified in the vol?atile oil extracted by SDE,which accounted for 94.49%of the total amount of detection. There were alkyl,acids,aldehydes,ketones, esters,alcohols and other substances in the volatile oil. And 16 compounds were determined in the volatile oil extracted by DDE,ac?counting for 97.12 % of the total amount detected. There were furan,carboxylic acids,esters,aldehydes,alcohols,phenols,ke?tones,alkene and acyl halide. The chemical compositions of the volatile oil extracted by SDE were more than those extracted by DDE. Conclusion The chemical constituents of volatile oil of Ramulus Mori can be more fully identified by the combination of the two ex?traction methods.

A study revealing the key aroma compounds of steamed bread made by Chinese traditional sourdough.

Aroma of Chinese steamed bread (CSB) is one of the important parameters that determines the overall quality attributes and consumer acceptance. However, the aroma profile of CSB still remains poorly understood, mainly because of relying on only a single method for aroma extraction in previous studies. Therefore, the objective of this study was to determine the volatile aroma compounds of five different samples of CSB using three different aroma extraction methods, namely solid-phase microextraction (SPME), simultaneous distillation-extraction (SDE), and purge and trap (P&T). All samples showed a unique aroma profile, which could be attributed to their unique microbial consortia. (E)-2-Nonenal and (E,E)-2,4-decadienal were the most prevalent aromatic compounds revealed by SDE, which have not been reported previously, while ethanol and acetic acid proved to be the most dominant compounds by both SPME and P&T. Our approach of combining three different aroma extraction methods provided better insights into the aroma profile of CSB, which had remained largely unknown in previous studies.

Determination of phthalate esters in teas and tea infusions by gas chromatography-mass spectrometry.

Phthalate esters (PAEs), a group of environmental pollutants which are carcinogenic to human body, have been detected in teas. In this work, five PAEs in teas and tea infusions were quantitatively determined by a modified simultaneous distillation extraction (SDE) coupled with gas chromatography-mass spectrometry. After the optimization of SDE, the proposed method afforded a wide range of linearity and high linear regression coefficients with the limits of detection range of 0.24-3.72 µg/kg. The average recoveries were 79.83-116.67% for tea samples and 78.22-101.64% for tea infusions with all the relative standard deviations below 20%. The total content of five PAEs in teas was 1.135-3.734 mg/kg and the total dissolving ratio of five PAEs from tea to infusion was 19.05-28.07% for the selected tea samples. The risk assessment result of all the selected tea samples demonstrated that the population with the habit of drinking tea won't cause risk to human health.

Recent findings in the chemistry of odorants from four Baccharis species and their impact as chemical markers.

Baccharis is a widespread genus belonging to the Asteraceae family that includes almost 400 species exclusively from the Americas. Even when studied in detail, the taxonomic classification among species from this genus is not yet fully defined. Within the framework of our study of the volatile composition of the Baccharis genus, four species (B. trimera, B. milleflora, B. tridentata, and B. uncinella) were collected from the 'Campos de Cima da Serra' highlands of the Brazilian state of Rio Grande do Sul. The aerial parts were dried and extracted by the simultaneous distillation extraction (SDE) procedure. This is the first time that SDE has been applied to obtain and compare the volatile-extract composition in the Baccharis genus. Characterization of the volatile extracts allowed the identification of 180 peaks with many coeluting components; these latter being detailed for the first time for this genus. The multivariate statistical analyses allowed separating the volatile extracts of the four populations of Baccharis into two separate groups. The first one included the B. milleflora, B. trimera, and B. uncinella volatile extracts. The three species showed a high degree of similarity in their volatile composition, which was characterized by the presence of high contents of sesquiterpene compounds, in particular of spathulenol. The second group comprised the extract of B. tridentata, which contained α-pinene, ß-pinene, limonene, and (E)-ß-ocimene in high amounts.

Effect of edible coating on the aromatic attributes of roasted coffee beans.

Coffee is known throughout the world for its distinct aroma and flavour which results from a number of volatile compounds present in it. It is very difficult to arrest the aromatic compounds once the roasting process is complete and it becomes even more challenging to store the beans for a longer time with the retained volatiles as these compounds are easily lost during industrialized processing such as the grinding of roasted coffee beans and storage of ground coffee. Thus, an attempt was made to minimise the loss of volatile from roasted coffee beans by coating with Carboxymethyl cellulose (CMC), Hydroxypropylmethyl cellulose (HPMC) and Whey protein concentrate. Coffee volatiles were analysed by Gas chromatography and 14 major compounds were identified and compared in this study. Results showed an increase in the relative area of major volatile compounds in coated roasted coffee beans when compared with unroasted coffee beans for consecutive two months. Moreover, effect of coating on textural properties and non-volatiles were also analysed. The results have indicated that edible coatings preserve the sensory properties of roasted coffee beans for a longer shelf life and cellulose derivatives, as an edible coating, exhibited the best protecting effect on roasted coffee beans.

Antibacterial and antioxidant activities and chemical compositions of volatile oils extracted from Schisandra chinensis Baill. seeds using simultaneous distillation extraction method, and comparison with Soxhlet and microwave-assisted extraction.

The volatile oils were isolated from dried Schisandra chinensis Baill. seeds by Soxhlet extraction (SE), microwave-assisted extraction (MAE), and simultaneous distillation extraction (SDE), and fractions were identified by gas chromatography-mass spectrometry (GC-MS) and high-performance liquid chromatography (HPLC). The essential oils were assessed for their antioxidant and antibacterial activities. GC-MS results also revealed that the major ingredients in the oil extracted by SDE were terpenoids compounds such as ylangene (15.01%), α-phellandrene (8.23%), ß-himachalene (6.95%), and cuparene (6.74), and the oil extracts of MAE and SE mainly contained aromatics such as schizandrins, wuweizisu C, and gomisin A. HPLC analysis results confirmed that more schizandrin was obtained through extraction by MAE (996.64 µg/g) and SE (722.13 µg/g). SDE oil extract showed more significant antioxidant activity than MAE or SE oil. Only volatile oil from SDE showed good antibacterial activity against all tested strains.

Aroma-active components of yeast extract pastes with a basic and characteristic meaty flavour.

BACKGROUND: Aroma-active compounds, together with sugars, amino acids, fat and nucleotides, are the main chemical species determining the characteristic aroma and taste of food. For selecting yeast extract pastes products with a less undesirable aroma, the aroma-active compounds that affect the overall consumer acceptance of yeast extract pastes products were analysed in this work. RESULTS: The aroma-active compounds of yeast extract pastes were extracted by using dynamic headspace extraction or simultaneous distillation extraction, and were detected by gas chromatography-olfactrometry-mass spectrometry in conjunction with dynamic headspace dilution analysis or aroma extract dilution analysis. Sensory results revealed that a meaty, roasted aroma was the dominant of overall aroma. The important aroma-active compounds referred in this work were mainly aldehydes, acids, ketones, furan derivatives, pyrazines, and sulfur-containing compounds. Of these, six volatile compounds such as 3-methylbutanal, 2,3-butanedione, 2,3,5-trimethyl-pyrazin, acetic acid ethenyl ester, 2-acetyl-1-pyrroline and (E,E)-2,4-decadienal had never been reported before as key aroma-active compounds of yeast extract pastes. CONCLUSIONS: The key aroma-active compounds were identified in basic and characteristic meaty flavour yeast extract pastes, and their characterisation was determined.

A comparative study of volatile components in green, oolong and black teas by using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry and multivariate data analysis.

The difference of volatile components in green, oolong and black teas was studied by using comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS). Simultaneous distillation extraction was proved to be a suitable technique to extract the analytes with interest. A total of 450 compounds were tentatively identified with comparison to the standard mass spectra in available databases, retention index on the first dimension and structured chromatogram. 33 tea samples, including 12, 12 and 9 samples of green, oolong and black tea were analyzed by using GC×GC-TOFMS. After peak alignment, around 3600 peaks were detected. Partial least squares - discriminant analysis and hierarchical cluster analysis were used to classify these samples, then non-parametric hypothesis test (Mann-Whitney U test) and the variable importance in the projection (VIP) were applied to discover the key components to distinguish the three types of tea with significant difference amongst them. 74 differential compounds are defined to interpret the chemical differences of 3 types of tea. This study shows the power of GC×GC-TOFMS method combined with multivariate data analysis to investigate natural products with high complexity for information extraction.