Analysis of Volatile Compounds and Identification of Characteristic Aroma Components of <i>Toona sinensis</i>(A. Juss.) Roem. Using GC-MS and GC-O

In this study, volatile compounds present in Toona sinensis (A. Juss.) Roem (TS) were investigated and their characteristic aromatic components were identified using Headspace Solid-phase Microextraction (HS-SPME) followed by Gas Chromatography-Mass Spectrometry (GC-MS) and Gas Chromatography-Olfactometry (GC-O). The optimum conditions for extracting the volatiles from TS were achieved with the experimental parameters including the use of a 65 μm polydimethylsiloxane/divinyl benzene (PDMS/DVB) fibre, an extraction temperature of 40℃ and an extraction time of 30 min. Under these conditions, 56 volatile compounds were separated and 53 were identified by GC-MS. Among them, 21 sulfide compounds (42.146%) and 27 terpenes(55.984%) were found to be the major components. The sample was analyzed by GC-O and 26 elutes were sniffed and their sensory descriptions evaluated by an odor panelists. Analysis of the data indicated, two compounds cis and trans isomers of 2-Mercapto-3,4-dimethyl-2,3-dihydrothiophene were major contributors to the characteristic aroma of TS.

Volatile components of Rhizoma Alpiniae Officinarum using three different extraction methods combined with gas chromatography-mass spectrometry

Volatile components from Rhizoma Alpiniae Officinarum were respectively extracted by three methods including hydrodistillation, headspace solid-phase microextraction （HS-SPME） and diethyl ether extraction. A total of 40 （hydrodistillation）, 32 （HS-SPME） and 37 （diethyl ether extraction） compounds were respectively identified by gas chromatography-mass spectrometry （GC/MS） and 22 compounds were overlapped, including β-farnesene, 7-muurolene, 2,6-dimethyl-6- （4-methyl-3-pentenyl）bicyclo[3.1.1]hept-2-ene, eucalyptol and cadina-1（10）, 4-diene and so forth, varying in relative contents. HS-SPME is fast, sample saving and solvent-free and it also can achieve similar profiles as those from hydrodistillation and solvent extraction. Therefore, it can be the priority for extracting volatile components from medicinal plants.

Volatile components,total phenolic compounds,and antioxidant capacities of worm-infected Gomphidius rutilus

This study evaluated the effects of worm infection on the volatile components,total phenolic compounds,and antioxidant capacities of Gomphidius rutilus.G.rutilus without worms(GW),G.rutilus infected by a small amount of worms(GS;infected area<50%),and G.rutilus infected by a large amount of worms(GL;infected area>50%)were investigated.The volatile components of G.rutilus were analyzed by simultaneous distillation–extraction(SDE)and headspace solid-phase microextraction(HS-SPME)using gas chromatography–mass spectrometry(GC–MS).A total of 17 and 19 types of volatile compounds were detected,including ketones,alcohols,benzene,alkenes,aldehydes,esters,acids,and alkanes.Alcohols comprised the most abundant compound in GL,GS,and GW.The relative content of 1-octen-3-ol was the highest in all mushrooms.The concentration of eight-carbon(C8)compounds relative to the total volatile compounds varied widely,ranging from 40%(GW)to 64.34%(GS)and 84.42%(GS)and to 91.59%(GL),respectively,among the three samples.The antioxidant capability and the total phenolic contents of G.rutilus were evaluated in this study.The highest total phenolic content(TPC)of 192.23 mg GAE/g was found in GL,which differed significantly(P<0.05)from the latter two samples,whereas the lowest value of 156.11 mg GAE/g was found in GW.ABTS radical cation scavenging activity,FRAP ferric reducing antioxidant capacity(FRAP)radical scavenging activity,and oxygen radical absorbance capacity(ORAC)were investigated to screen the antioxidant properties of extracts.The contents of total phenolic compounds and their antioxidant capacities in vitro showed significant correlations(P<0.01).Among the three types of samples,the phenolic compounds of GL exhibited the highest antioxidant capacity,showing the values of 0.089 mM TE/g for ABTS,0.949 mM Fe^2+E/g for FRAP,and 1.952 M TE/g for ORAC.However,regarding the total antioxidant capacity,GS exhibited the highest antioxidant capacity,showing the values of 0.002648 mM TE/g for ABTS,0.004437 mM Fe^2+E/g for FRAP,and 0.256μM TE/g for ORAC.In conclusion,HS-SPME was more suitable for the extraction of volatile aroma components from G.rutilus.GL had the most abundant aroma components.GL had the highest TPC and antioxidant capacity compared with those of GS and GW,whereas GS showed the opposite results.Interestingly,GS was found to have the highest total antioxidant capacity in vitro.Based on these measured indicators,worm infection had no negative effect on the quality of G.rutilus.Therefore,worm-infected G.rutilus can also be consumed by humans.

Ultrasonic Nebulization Extraction Coupled with Gas Chromatography-Mass Spectrometry for Analysis of Volatile Components in Traditional Chinese Patent Medicine

The ultrasonic nebulization extraction（UNE） was developed and applied to the extraction of volatile components from traditional Chinese patent medicine Xiaoyao Pills. Several parameters of ultrasonic nebulization extraction including the sample particle size, solvent volume, extraction time and ultrasonic power were studied and selected. As a result, 2.4 g of sample with particle size of 80 mesh was extracted with 15 mL of n-hexane for 20 min at an ultrasonic power of 35 W. The volatile components were analyzed by gas chromatography-mass spectrometry （GC-MS） under the optimal conditions and 57 compounds were identified. The precision, repeatability and stability of the proposed method were also studied. Compared with ultrasonic-assisted extraction（UAE） and hydrodistillation（HD） extraction, the proposed method is more efficient, faster and easier to be operated at room temperature with smaller sample and energy consumption. It is suggested that the ultrasonic nebulization extraction can be used as a novel alternative method for the extraction of volatile components from traditional Chinese patent medicine.

Analysis on Volatile Components of Flowers and Leaves of Thymus mongolicus by SPME-GC/MS

[Objectives] To analyze volatile components of flowers and leaves of Thymus mongolicus. [Methods]Volatile components of collected T. mongolicus flower and leaves were separated by headspace solid-phase microextraction( SPME) and identified by gas chromatography/mass spectrometry( GC/MS) and normallized by peak area. [Results] A total of 24 and 14 compounds were identified from flowers and leaves of T. mongolicus in the total ion chromatogram,accounting for 99. 573% and 97. 187% of the total peak area,respectively. Main components of flowers and leaves of T. mongolicus include phenols and terpenes,and thymol accounts for 35. 38% and 49. 13% of flowers and leaves of T. mongolicus,respectively. [Conclusions] SPME-GC/MS can be applied in analyzing volatile components of flowers and leaves of T. mongolicus,to provide basis for further development and utilization of T. mongolicus.

Headspace Solid-Phase Micro-Extraction Gas Chromatography/Mass Spectrometry(HS-SPME-GC/MS)-Based Untargeted Metabolomics Analysis for Comparing the Volatile Components from 12 Panax Herbal Medicines

Quality control of ginseng currently is mainly based on ginsenoside analysis,but rarely focuses on the volatile organic components.In the current work,an untargeted metabolomics approach,by headspace solid-phase micro-extraction gas chromatography/mass spectrometry(HS-SPME-GC/MS),was elaborated and further employed to holistically compare the compositional difference of the volatile components simultaneously from 12 Panax herbal medicines,which included P.ginseng(PG),P.quinquefolius(PQ),P.notoginseng(PN),red ginseng(PGR),P.ginseng leaf(PGL),P.quinquefolius leaf(PQL),P.notoginseng leaf(PNL),P.ginseng flower(PGF),P.quinquefolius flower(PQF),P.notoginseng flower(PNF),P.japonicus(PJ),and P.japonicus var.major(PJvm).Chromatographic separation was performed on an HP-5MS elastic quartz capillary column using helium as the carrier gas,enabling good resolution within 1 h.We were able to characterize totally 259 volatile compounds,including 82 terpenes(T),46 alcohols(Alc),29 ketones(K),25 aldehydes(Ald),21 esters(E),and the others.By analyzing 90 batches of ginseng samples based on the untargeted metabolomics workflows,236 differential ions were unveiled,and accordingly 36 differential volatile components were discovered.It is the first report that simultaneously compares the compositional difference of volatile components among 12 Panax herbal medicines,and useful information is provided for the quality control of ginseng aside from the well-known ginsenosides.

Analysis of the Volatile Components in Flowers of <i>Paeonia lactiflora</i>Pall. and <i>Paeonia lactiflora</i>Pall. var. <i>Trichocarpa</i>

Paeonia lactiflora Pall. var. trichocarpa is a variety of Paeonia lactiflora Pall., and is currently the peony herb’s principal cultivar group. Here, we study the differences in aromatic components and flowers of different varieties between two groups of cultivars, providing a reference for applying natural fragrance substances of peonies, breeding fragrant flower types, and developing and using improved varieties. Headspace solid-phase microextraction (HS-SPME), gas chromatography-mass spectrometry (GC-MS), peak area normalization for each component relative to content, component library (NIST14/NIST14S) retrieval, and a literature review were used to analyze the volatile compounds in flowers of eight peony varieties, such as “Gaoganhong”, and ten comospore peony varieties, such as “Jinshanhong”. Results showed that the main volatile compound constituents in flowers of the two groups were terpenes and alcohols. Additionally, the content of eucalyptol, caryophyllene, α-Pinene, citronellol, and 3-Hexen-1-ol, acetate, (Z) was high. Peony cultivars contained linalool, (1R)-2,6,6-trimethylbicyclo[3.1.1]hept-2-ene, and 1,4-dimethoxybenzene, while comospore peony varieties contained 1,3,6-octatriene, 3,7-dimethyl-, (Z)-, phenylethyl alcohol, and geraniol. In this study, the differences between the volatile components of flowers of different peony varieties were clarified, laying a foundation for further molecular biology research into the floral fragrance of peonies and the cultivation of new varieties of aromatic peonies. At the same time, it also provides a theoretical basis for the development and application of peony flower by-products.

Analysis of Volatile Components in Fresh Fruit of Morinda citrifolia L.from Different Origins Based on HS-SPME-GC/MS

[Objectives]This study was conducted to clarify the differences of volatile components in fresh fruit of Morinda citrifolia L.from different origins.[Methods]The method of HS-SPME-GC/MS detection was used to determine the volatile chemical components in fresh fruit of M.citrifolia.[Results]52,52 and 45 volatile components were identified from the fresh fruit of M.citrifolia from Xisha,Wanning and Haikou,respectively.Among them,the number and content of the identified esters were relatively high,mainly methyl caprylate,ethyl caprylate,4-pentenyl caproate,3-methylbuten-2-enyl caprylate,methyl caproate,and ethyl caproate.There were also fatty acids,alcohols,phenols,ketones,aldehydes and other substances.There were 33 common ingredients in the fruit from the three origins,mainly including caprylic acid,caproic acid,capric acid,methyl caprylate,ethyl caprylate,4-pentenyl caproate,3-methylbutene-2-enyl caprylate,methyl caproate,ethyl caproate,methyl caprate and hexyl caproate.[Conclusions]The types and contents of volatile components in fresh fruit of M.citrifolia from different origins were significantly different.

HS-SPME-GC-MS Analysis on Volatile Components in Different Cultivars and Different Parts of Artemisia argyi

[Objectives] To analyze and compare the difference in volatile components of different cultivars and different parts of Artemisia argyi by using headspace solid phase microextraction( HS-SPME) and provide scientific basis for comprehensive development and rational utilization of Artemisia argyi. [Methods]Firstly,HS-SPME was used to extract the volatile components from the leaves,seeds,and stems of seven-tip Artemisia argyi,five-tip Artemisia argyi,and golden Artemisia argyi. Their chemical composition was analyzed by gas chromatographymass spectrometry( GC-MS),and the relative mass fraction of each component was determined by area normalization method. [Results] For the same variety of Artemisia argyi,the content of volatile components in leaves was higher than in seeds and stems except camphor,and the content of volatile components in seven-tip Artemisia argyi leaves was higher than in five-tip Artemisia argyi and golden Artemisia argyi leaves.HS-SPME-GC-MS analysis showed that eucalyptol,camphor,thujone,α-pinene,1-caryophyllene and caryophyllene oxide with higher content were detected in different parts of the different cultivars of Artemisia argyi. [Conclusions]Seven-tip Artemisia argyi leaves were the best medicinal parts of the three cultivars,followed by seven-tip Artemisia argyi seeds.

Analysis of volatile chemical components of Radix Paeoniae Rubra by gas chromatography-mass spectrometry and chemometric resolution

The volatile chemical components of Radix Paeoniae Rubra (RPR) were analyzed by gas chromatography-mass spectrometry with the method of heuristic evolving latent projections and overall volume integration. The results show that 38 volatile chemical components of RPR are determined, accounting for 95.21% of total contents of volatile chemical components of RPR. The main volatile chemical components of RPR are (Z, Z)-9,12-octadecadienoic acid, n-hexadecanoic acid, 2-hydroxy- benzaldehyde, 1-(2-hydroxy-4-methoxyphenyl)-ethanone, 6,6-dimethyl-bicyclo[3.1.1] heptane-2-methanol, 4,7-dimethyl-benzofuran, 4-(1-methylethenyl)-1-cyclohexene-1-carboxaldehyde, and cyclohexadecane.

Determination of volatile components in cut tobacco with gas chromatography-mass spectrometry and chemometric resolution

Chromatography-mass spectrometry(GC-MS)was used to analyze the volatile components of cut tobacco samples with the help of heuristic evolving latent projections(HELP).After extracting with simultaneous distillation and extraction method,the volatile components in cut tobacco were detected by GC-MS.Then the obtained original two-dimensional data were resolved into pure mass spectra and chromatograms.The qualitative analysis was performed by similarity searches in the national institute of standards and technology(NIST)mass database with the obtained pure mass spectrum of each component and the quantitative results were obtained by calculating the volume of total two-way response.The accuracy of qualitative and quantitative results were greatly improved by using the two-dimensional comprehensive information of chromatograms and mass spectra.107 of 141 separated constituents in the total ion chromatogram of the volatile components were identified and quantified,accounting for about 88.01% of the total content.The result proves that the developed method is powerful for the analysis of complex cut tobacco samples.

Analysis of volatile components in herbal pair herba schizonepetae-ramulus cinnamomi

Analysis of volatile components in herbal pair (HP) herba schizonepetae-ramulus cinnamomi (HS-RC), single herb HS and RC was carried out by gas chromatography-mass spectrometry (GC-MS) data and chemometric resolution method (CRM). The two-dimensional data obtained from GC-MS instruments were resolved into a pure chromatogram and a mass spectrum of each chemical compound by CRM. In total, 47, 61 and 51 chemical components in volatile oil of HS, RC, and HP HS-RC were respectively determined qualitatively and quantitatively, accounting for 90.52%, 88.37%, and 88.72% total contents of volatile oil of HS, RC, and HP HS-RC, respectively. The number of the volatile components of HP HS-RC is almost the addition of that of two single herbs, but their relative contents are changed.

Identification of Volatile Oil Components of Nardostachys jatamansi DC. Root and Rhizome,Herb

[Objectives] Volatile oil components of traditional drug use site " root and rhizome" of N. jatamansi and herb were identified and contrasted,which aimed to provide the basis for rationally using wild N. jatamansi resource. [Methods]Volatile oil components from different sites of N. jatamansi were identified and isolated by GC-MS. [Results] There were 56 kinds of volatile oil components from different sites of N. jatamansi,in which 39 components from herb of N. jatamansi,39 components from root and rhizome of N. jatamansi,and there were 22 common components. But 1 component in higher concentration had obvious difference. [Conclusions] The herb of N. jatamansi could not completely replace " root and rhizome" of N. jatamansi as the medicine,which was consistent with prior detection result of each physicochemical index from different sites of N. jatamansi. The research could provide the reference for making quality standard of N. jatamansi medicine and rational basis for its further research and development.

Analysis of volatile components in a Chinese fish sauce,Fuzhou Yulu, by gas chromatography-mass spectrometry

Volatile components of Fuzhou Yulu, a Chinese fish sauce, were analyzed by gas chromatography-mass spectrometry (GC-MS), and two pretreatment methods, i.e., purge and trap (P&T) GC-MS and ethyl acetate extraction followed by GC-MS, were compared. P&T-GC-MS method determined 12 components, including sulfur-containing constituents (such as dimethyl disulfide), nitrogen-containing constituents (such as pyrazine derivatives), aldehydes and ketones. Ethyl acetate extraction fol- lowed by GC-MS method detected 10 components, which were mainly volatile organic acids (such as benzenepropanoic acid) and esters. Neither of the two methods detected alcohols or trimethylamine. This study offers an important reference to determine volatile flavor components of traditional fish sauce through modern analysis methods.

Analysis of Volatile Components in Different Parts of Polygala japonica Houtt.

[Objectives] To analyze the volatile components in different parts of Polygala japonica Houtt. and compare the differences of these volatile components. [Methods] The volatile components in different parts of P. japonica Houtt. were analyzed by the headspace solid-phase microextraction( HS-SPME) combined with GC-MS,and the relative percentage of each component was determined by peak area normalization. [Results] Thirty kinds of volatile components were identified from the leaves and rhizomes of P. japonica Houtt.,mainly including olefins,aromatic hydrocarbons,alkanes and esters. [Conclusions] The volatile components in different parts of P. japonica Houtt. were different,and there may be difference in the medicinal value of volatile components in different parts,thus it is required to take an overall consideration of these differences in the development and utilization of P. japonica Houtt.

Analysis of the Volatile Components of Polygonum chinense L.Extracted with Different Solvents by GC-MS

[Objectives]This study was conducted to investigate the volatile components of Polygonum chinense L.[Methods]The volatile components of the methanol extract,ethyl acetate extract,chloroform extract and petroleum ether extract of P.chinense were analyzed and determined by gas chromatography.[Results]The volatile components of the methanol extract from P.chinense were the most,and phenolic acids and ketones accounted for a relatively high proportion,among which pyrogallic acid had the highest content.The ethyl acetate extract contained the second most volatile components,mostly acids and esters,of whichβ-sitosterol had the highest content;the chloroform and petroleum ether extracts had relatively few types of volatile components,most of which were alkanes,and the content ofγ-sitosterol shared by the two was the highest.The common substances of the four extracts were palmitic acid and phytol.[Conclusions]This study provides a theoretical basis for the quality evaluation of P.chinense and a scientific basis for its resource development.

GC-MS Analysis of Volatile Components Extracted from Fruit of Artemisia argyi

[Objectives] To analyze the volatile components extracted from fruit of Artemisia argyi.[Methods] The volatile components from fruit of Artemisia argyi were extracted by steam distillation( SD) and headspaces solid-phase microextraction( HS-SPME). The components were separated and analyzed by gas chromatography-mass spectrometry( GC-MS) with the area normalization method to determine the relative percentage content of each component.[Results]33 compounds were isolated and 29 compounds were identified by SD accounting for about93. 02% of the total volatile components; and 35 compounds were isolated and 30 compounds were identified by HS-SPME accounting for about99. 01% of the total volatile components. 11 kinds of the volatile components were identified by the two methods together and the content of β-thujone was highest.[Conclusions] There were some differences between SD and HS-SPME,and the two methods were applied to the extraction of different types of volatile components,and combination of the two methods to analyze the volatile components in fruit of Artemisia argyi could help us to get more comprehensive information.

Effect of inoculating mixed starter cultures of Lactobacillus and Staphylococcus on bacterial communities and volatile flavor in fermented sausages

The objective of this study was to explore the effects of the inoculation of mixed starter cultures of Lactobacillus and Staphylococcus(labeled L-S)on microbial community and flavor in fermented sausages during the ripening process.Culture-dependent(colony count)and culture-independent(high-throughput sequencing)methods were employed to evaluate bacterial communities.Volatile compounds were identified by gas chromatography-mass spectrometry,and the results were analyzed by principal component analysis(PCA).The identified bacteria with high relative abundance included Lactobacillus and Pediococcus,and the relative abundances of Leuconostoc and Weissella in fermented sausages were remarkably decreased at the end of the ripening process.At the end of ripening,2-nonenal,tetradecanal,ethylstearate and terpinyl acetate played substantial roles in the flavor development of the L-S fermented sausages.Sensory evaluation showed a high score in the L-S fermented sausages.Sausages can be inoculated with L-S starter culture to improve the safety and flavor of meat products.

Volatile Compounds Fingerprints for White Duck down and White Goose down Determined by Gas Chromatography-Ion Mobility Spectrometry

This work first describes a simple approach for the untargeted profiling of volatile compounds for distinguishing between white duck down (WDD) and white goose down (WGD) based on resolution-optimized GC-IMS combined with optimized chemometric techniques, namely PCA. The detection method for down samples was established by using GC-IMS. Meanwhile, the reason of unpleasant odors caused by WDD was explained on the basis of the characteristic volatile compounds identification. GC-IMS fingerprinting can be considered a revolutionary approach for a truly fully automatable, cost-efficient, and in particular highly sensitive method. A total of 22 compounds were successfully separated and identified through GC-IMS method, and the significant differences in volatile compounds were observed in three parts of WDD and WGD samples. The most characteristic volatile compounds of WGD belong to aldehydes, whereas carboxylic acids from WDD were detected generated by autoxidation reaction. Meanwhile, the main reason of unpleasant odor generation was possibly attributed to the high concentration of volatile carboxylic acids of WDD. Therefore, the constructed model presents a simple and efficient method of analysis and serves as a basis for down processing and quality control.

Effects of the fertilizer and water management on amino acids and volatile components in Cabernet Sauvignon grapes and wines

The amino acids and the volatile substances in grapes and wines play important roles in their quality,and the concentrations of these substances can be changed by how a vineyard is managed,e.g.,irrigation and fertigation regimes.This study aimed to evaluate the effect of fertilizer and water management on the distribution of amino acids,the volatile component profiles,and the sensory characteristics of Cabernet Sauvignon grapes and wines.The results showed that the amino acid concentration in grape berries was the highest under the 100%local fertilizer rate(HF)and 100%water irrigation quota(HW)treatment,and the volatile component concentration in wine was the highest under HF and 80%water irrigation quota(MW)treatment.The effect of irrigation on the amino acid content in grapes was greater than that of fertigation.The synergistic effect of fertilizer and water on arginine,serine,and glutamine in grape berries was significant.The interactive effect of fertigation and irrigation on the volatile substance in grapes was greater than that of fertigation and irrigation alone.The influence of irrigation on volatile substances in wines was greater than that of fertigation.In addition,there was also a correlation between the concentrations of multiple amino acids in grapes and volatile components in wines.Principal component analysis showed that the wine from the HFMW treatment had the best quality among all treatments.