Flash Evaporation and Headspace Solid-phase Microextraction for the Analysis of the Essential Oils in Traditional Chinese Medicine,Houttuynia Cordata Thunb

We have investigated the use of flash evaporation, headspace solid-phase microextraction (HS-SPME) and steam distillation (SD) as sample concentration and preparation techniques for the analysis of volatile constituents present in Houttuynia cordata Thunb. The samples were analyzed by gas chromatography (GC) and identified by mass spectrometry (MS). Comparison studies were performed. It was found that the results obtained between Headspace solid-phase microextraction HS-SPME and SD techniques were in good agreement. Seventy-nine compounds in Houttuynia cordata Thunb were identified by MS. In flash evaporation, thirty-nine compounds were identified. Discrimination in the response for many constituents studied was not observed, which can be clearly observed in SD and HS-SPME techniques. As a conclusion, HS-SPME is a powerful tool for determining the volatile constitutes present in the Houttuynia cordata.

Determination of Aromatic Components of Rosa davurica Pall. by Headspace Solid Phase Microextraction Combined with GC-MS

[Objectives] To determine the aromatic components of Rosa davurica Pall. [Methods] 42 kinds of aromatic components were identified from the flowers of R. davurica by headspace solid phase microextraction( HS-SPME) combined with gas chromatography-mass spectrometry( GC-MS). The main compounds were alcohols( 54. 88%) and aldehydes( 19. 55%). [Results] The top five components with the highest relative content were phenylethyl alcohol( 12. 69%),geraniol( 9. 85%),citronellol( 8. 80%),nerol( 7. 84%) and 2-n-pentylfuran( 7. 45%). [Conclusions] Headspace solid phase microextraction( HS-SPME) combined with gas chromatography-mass spectrometry( GC-MS) can provide basis for further development and utilization of R. davurica.

Integration of GC-MS Based Non-Targeted Metabolic Profiling with Headspace Solid Phase Microextraction Enhances the Understanding of Volatile Differentiation in Tobacco Leaves from North Carolina, India and Brazil

In this report, gas chromatography-mass spectrometry (GC-MS) based non-targeted metabolomics is used to develop appropriate headspace solid phase microextractions (HS-SPME) to enhance the understanding of volatile complexity of flue-cured tobacco leaves. Non-targeted metabolic profiling of GC-MS shows that the extraction condition of HS-SPME at 100?C for 30 min provides a better metabolite profile than other extraction conditions tested. GC-MS and principal component analyses (PCA) show that among five types of fibers tested, 100 μm polydimethylsiloxane (PMDS), 65 μm polydimethylsiloxane/divinylbenzene (PMDS/DVB) and 75 μm carboxen/polydimethylsiloxane (CAR/ PMS) provide a better reproducible metabolite profile. Based on an appropriate PDMS extraction condition optimized, we use GC-MS analysis and PCA to compare metabolite profiles in flue-cured leaves of tobacco plants grown in North Carolina, India and Brazil, respectively. The resulting data of PCA show that the global metabolic profiles in North Carolina samples are separated from those in Brazil and India samples, two groups of which are characterized by a partially overlapped pattern. Several peaks that were differentially accumulated in samples were annotated to known metabolites by deconvolution analysis, such as norsolanadione, solavetivone and rishtin. Norsolanadione is detected only in Brazil samples. Solavetivone is detected in samples of India and Brazil but not in those of North Carolina. Rishtin is detected in samples of North Carolina and India but not in Brazil samples. These data indicate that not only can a non-targeted metabolic profiling approach enhance the understanding of volatile complexity, but also can identify marker volatile metabolites in tobacco leaves produced in different growth regions.

HS-SPME-GC-MS技术分析不同加工阶段的甲鱼腥味成分变化

为研究不同加工方式对甲鱼腥味成分的影响,采用HS-SPME-GC-MS技术对甲鱼预煮、卤制、烘烤不同加工阶段的腥味物质进行分析。结果表明,经NIST/Willey质谱数据库检索和文献对照,新鲜甲鱼共检出48种挥发成分,确定36种成分,包括烃类21种、醛类12种、醇类化合物5种、芳香类5种、羧酸类3种、酮类1种、酯类1种。其中以己醛的百分含量最多,为29.1%,有青草味;庚醛占10.69%,具有强烈的油脂氧化味;壬醛占12.58%,提供鱼腥味;占2.02%的对二甲苯有刺激味;占2.36%的1-辛烯-3-醇具有土腥味。认为己醛、壬醛、庚醛、1-辛烯-3-醇等共同形成了甲鱼的腥味。通过预煮、卤制、烘烤等加工工艺后,腥味成分已减少至只能检测出己醛和壬醛,且含量都不超过1%。表明经预煮、卤制、烘烤等加工可以有效控制甲鱼的腥味。

Study on the Aromatic Components of Green Plum Wine by HS-SPME-GC-MS

In order to better blend green plum wine and study aromatic components of green plum wine,a qualitative analysis on aromatic components of soaked base liquor,green plum soaked wine,green plum juice,and fermented wine of green plum juice by Head Space Solid-phase Microextraction( HS-SPME) and Gas Chromatograph Mass Spectrometer( GC-MS) was studied in this paper. Experiment results indicated that14,32,17,and 46 kinds of aromatic components were identified respectively from four samples. Different aromatic components determined the special flavor and taste of green plum wine. Unique aromatic components generated in soaking process include benzaldehyde,1-butanol,2-methyl-,S-(-),benzoic acid ethyl ester,and 5-( hydroxymethyl). Special aromatic components in green plum juice were furfural,phenylethyl alcohol,and benzyl alcohol. The aromatic components in fermented wine of green plum juice mainly included phenylethyl alcohol( 6. 941%,relative content of peak area,same below),1-butanol,3-methyl-( 6. 940%),octanoic acid,ethyl ester( 3. 734%),decanoic acid,ethyl ester( 2. 590%),hexanoic acid,ethyl ester( 2. 479%),ethyl 9-decenoate( 2. 080%),and 5-hydroxymethyl( 1. 756%). This study was expected to provide scientific basis and data reference for quality improvement of green plum wine.

应用顶空-固相微萃取结合气相色谱-质谱联用技术分析传统锦州虾酱中挥发性物质

传统锦州虾酱是以白虾和乌虾为原料,在高盐条件下经长时间发酵形成海产风味食品。采用HPSPME/GC-MS结合保留指数方法分析虾酱中的挥发性物质,并对萃取条件进行优化。从DVB/PDMS、CAR/PDMS和DVB/CAR/PDMS筛选出最佳萃取头,同时采用正交试验优化SPME参数条件,确定适宜萃取条件为75μm CAR/PDMS萃取头,样品质量为5.0 g,萃取温度为70℃,萃取时间为50 min。对虾酱的风味物质分析得到44种挥发性物质,分别为醛类、酮类、酯类、酸类、酚类、烷烃类、吡嗪类和其他化合物。其中白虾虾酱主要呈香物质是醛类、吡嗪类和酚类等低阈值化合物,3-甲硫基丙醛、四甲基吡嗪和吲哚可能是白虾虾酱有别于乌虾虾酱的特有风味物质。乌虾虾酱主要呈香物质是醛类、酯类、酸类和酚类等低阈值化合物,酸类化合物是乌虾虾酱有别于白虾虾酱特有的风味物质,酯类化合物也可能是乌虾虾酱中风味物质的增味剂。

酱油挥发性成分固相微萃取条件的优化

顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)是提取挥发性成分比较常用的方法。为了确定提取酱油挥发性成分的SPME萃取头,分别以挥发性成分的累积峰面积标准化值和峰面积相对标准偏差的平均值与标准偏差为指标,考察了不同型号萃取头的萃取灵敏度和重复性,确定采用65μm PDMS/DVB提取酱油挥发性成分;并以各类挥发性成分峰面积和总峰面积为指标,优化了其萃取条件,确定萃取条件为:样品用量8 m L,萃取温度60℃,萃取时间60 min。利用优化方法对酱油挥发性成分进行提取,经气相色谱-质谱联用(gas chromatography-mass spectrometry,GC-MS)分析,共鉴定出86种挥发性成分,其中最主要的为酯类物质,其次为醇类、醛类和酸类。挥发性成分峰面积的平均相对标准偏差为8.14%,方法重复性较好。

林芝松口蘑与红菇蜡伞子实体香气成分比较

研究采用顶空固相微萃取技术联合气质联用技术分别对松口蘑和红菇蜡伞子实体香气成分进行分析测定和比较分析,以期建立准确、快速、高效的鉴别方法。结果显示,松口蘑检测到74种香气成分,红菇蜡伞检测到72种香气成分,松口蘑相较红菇蜡伞检测到特有的香气成分14种,包括乙醛、庚醛等6种醛类,2(5H)-呋喃酮1种酮类,3-苯丙醇1种醇类,正己酸乙酯、丙位戊内酯2种酯类,萜品烯和异松油烯等4个烯烃类;红菇蜡伞相较松口蘑,检测到特有的香气成分16种,包括2-丁基-2-辛烯醛1种醛类,3-羟基-2-丁酮、甲基庚烯酮等4种酮类,丁醇等5种醇类,(1-羟基-2,4,4-三甲基戊-3-基) 2-甲基丙酸酯1种酯类,异丁酸、丁酸等3种羧酸类,邻甲酚1种酚类,乙二醇单丁醚1种醚类,N-甲基吡咯烷酮1种含氮化合物。经过主成分分析,得到红菇蜡伞中的主要特征性香气成分为:己醛、3-羟基-2-丁酮、3-辛烯酮、2-甲烯基丁内酯、异戊酸;松口蘑中为:异戊醛、庚醛、壬醛、2,5,2-三甲基吡嗪、2,6,2-三甲基吡嗪。同时对松口蘑与红菇蜡伞干品挥发性香气成分相对含量对比发现,松口蘑主要香气成分含量关系为醛类>烯烃类>醇类>酯类,红菇蜡伞主要香气成分含量关系为醛类>醇类>烯烃类>酯类。通过松口蘑与红菇蜡伞子实体干品香气成分的比较分析可为市售的2种产品的快速检验鉴别奠定理论基础。

酱香型大曲的挥发性组分时空性特征的分析

6种不同酱香型大曲的理化参数及挥发性组分的研究结果表明,酱香型大曲的挥发性组分具有显著的时空性特征(大曲生产地点和储存时间)。酱香型大曲主要挥发性组分包括芳香族、酯类、含氮化合物等。基于挥发性组分对不同类型的酱香型大曲进行主成分分析(principal components analysis,PCA)和聚类分析等统计分析,能有效地辨析其时空性特征。酱香型大曲生产地域之间的差异能够显著改变主要挥发性组分的种类,而相同地域不同生产企业和不同生产地点的酱香型大曲中的挥发性组分含量也差异较大。茅台原产曲的曲心和曲表的含氮化合物类挥发性组分的比例分别是52.83%和22.05%,其中较高的吡嗪类含氮组分是茅台原产曲的重要特征,而源于其他生产域的酱香型大曲中挥发性组分则以酯类为主(51.55%~79.49%)。同时酱曲主要挥性发组分种类及含量因陈曲时间而异。

Differential volatile organic compounds in royal jelly associated with different nectar plants

The aim of this work was to distinguish volatile organic compound（VOC） profiles of royal jelly（RJ） from different nectar plants. Headspace solid-phase microextraction（HS-SPME） was used to extract VOCs from raw RJ harvested from 10 nectar plants in flowering seasons. Qualitative and semi-quantitative analysis of VOCs extracts were performed by gas chromatography-mass spectrometry（GC-MS）. Results showed that VOC profiles of RJ from the samples were rich in acid, ester and aldehyde compound classes, however, contents of them were differential, exemplified by the data from acetic acid, benzoic acid methyl ester, hexanoic acid and octanoic acid. As a conclusion, these four VOCs can be used for distinguishing RJ harvested in the seasons of different nectar plants.

GC-MS, GC-O and OAV analyses of key aroma compounds in Jiaozi Steamed Bread

Jiaozi Steamed Bread(JSB)has a unique aroma as a traditional staple food in China.The volatile compounds in JSBwere extracted by simultaneous distillation and extraction(SDE)and headspace solid-phasemicroextraction(HS-SPME).These volatile substances were analyzed by gas chromatography-mass spectrometry(GC-MS)and gas chromatographyolfactometry-mass spectrometry(GC-O-MS).The results demonstrated that 61 volatile compounds were identified totally in samples,of which 15 were confirmed as potent aroma compounds with odor active values(OAVs)>1.The 15 potent aroma compounds were ethanol,1-butanol,1-pentanol,1-hexanol,heptanol,1-octen-3-ol,3-methyl-1-butanol,hexanal,heptanal,nonanal,(E)-2-heptenal,benzaldehyde,(E,E)-2,4-decadienal,2-pentylfuran and naphthalene.The SDEmethod had better linearity with coefficients of determination(R2)equal to or higher than 0.9991.Furthermore,the SDE method also achieved lower sensitivity and better repeatability and recovery than HS-SPME.This work provides reference method and parameters for future research on the flavor of JSB for commercial products.

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.

Volatile profile analysis and quality prediction of Longjing tea(Camellia sinensis) by HS-SPME/GC-MS

This study aimed to analyze the volatile chemical profile of Longjing tea, and further develop a prediction model for aroma quality of Longjing tea based on potent odorants. A total of 21 Longjing samples were analyzed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS).Pearson's linear correlation analysis and partial least square (PLS) regression were applied to investigate the relationship between sensory aroma scores and the volatile compounds. Results showed that 60 volatile compound scould be commonly detected in this famous green tea. Terpenes and esters were two major groups characterized,representing 33.89% and 15.53% of the total peak area respectively. Ten compounds were determined to contribute significantly to the perceived aroma quality of Longjing tea, especially linalool (0.701), nonanal (0.738), (Z)-3-hexenyl hexanoate (-0.785), and β-ionone (-0.763). On the basis of these 10 compounds, a model (correlation coefficient of89.4% and cross-validated correlation coefficient of 80.4%) was constructed to predict the aroma quality of Longjingtea. Summarily, this study has provided a novel option for quality prediction of green tea based on HS-SPME/GC-MStechnique.

Aroma changes of black tea prepared from methyl jasmonate treated tea plants

Methyl jasmonate（MeJA） was widely applied in promoting food quality.Aroma is one of the key indicators in judging the quality of tea.This study examined the effect of exogenous MeJA treatment on tea aroma.The aroma components in black tea prepared from MeJA-treated fresh tea leaves were extracted using headspace solid-phase microextraction（HS-SPME） and were analyzed using gas chromatography-mass spectrometry（GC-MS） and GC-olfactometry（GC-O）.Forty-five volatile compounds were identified.The results revealed that the MeJA-treated black tea had higher levels of terpene alcohols and hexenyl esters than the untreated tea.Moreover,several newly components,including copaene,cubenol,and indole,were induced by the MeJA treatment.The activities of polyphenol oxidase and β-glucosidase in fresh tea leaves changed after the MeJA treatment.Quantitative real-time polymerase chain reaction（qRT-PCR） analysis indicated that the gene expression levels of polyphenol oxidase and β-primeverosidase were upregulated by two and three folds,respectively,by the MeJA treatment（P0.01）; however,the gene expression of β-glucosidase was downregulated to a half level.In general,the aroma quality of the MeJAtreated black tea was clearly improved.

Butyltin compounds in vinegar collected in Beijing:Species distribution and source investigation

Forty-eight vinegar samples including white vinegar, rice vinegar and mature vinegar were collected from several markets in Beijing. Butyltin compounds were determined by headspace solid-phase microextraction coupled with gas chromatography and flame photometric detector after in situ ethylation with sodium tetraethylborate. Butyltin species were detected in sixteen vinegar samples and ranged from 0.012 to 14.10 lag Sn L 1. The detection rate of white vinegar is higher than that of rice vinegar and mature vinegar. Vinegar samples with relatively high butyltin concentration (〉1.5 μg Sn L-1) were those stored in plastic bags, indicating that the plastic bag was one of the possible sources of butyltin contamination. This was further confirmed by the leaching experiments of three selected plastic bags, and monobutyltin was detected in the leaching solvents. According to the estimation, the average daily intake of total butyltin compounds through vinegar consumption is about 0.04 ng Sn/kg b.w., much lower than the Tolerable Daily Intake (TDI) of 100 ng Sn/kg b.w. set by the European Food Safety Authority (EFSA).