不同萃取头固相微萃取分析小米清酒挥发性成分的研究

采用PA、PDMS、PDMS/DVB、CAR/PDMS和DVB/CAR/PDMS 5种萃取头,并通过固相微萃取（SPME）与气质联用（GC-MS）对小米清酒中挥发性成分进行提取、鉴定,运用聚类热图分析不同SPME萃取头提取小米清酒挥发性成分差异。结果表明：5种萃取头SPME检测到小米清酒挥发性成分含有醇、酯、醛、碳氢化合物、含苯衍生物和其他化合物,使用不同萃取头进行固相微萃取能得到较为相似的主挥发性成分：1-戊醇、苯乙醇、正己酸乙酯、丁二酸二乙酯、辛酸乙酯、十六烷,DVB/CAR/PDMS萃取头检测效果最好。聚类热图显示,不同萃取头SPME提取到的挥发性成分效果差异较大,按萃取效果可分为PA萃取头、PDMS萃取头和复合萃取头（PDMS/DVB、CAR/PDMS和DVB/CAR/PDMS）三类,使用不同种萃取头SPME可较为全面地了解小米清酒挥发性成分构成。     

固相微萃取结合气质联用法分析一种奶味香精中的挥发性成分

应用固相微萃取法采用3种不同萃取纤维,结合气相色谱-质谱联用技术,剖析1种国外奶味香精样品中的挥发性成分。结果表明;以Carboxen/聚二甲基硅氧烷(carboxen/polydimethylsiloxane,CAR/PDMS)为萃取纤维的方法鉴定出39种挥发性成分,以聚二甲基硅氧烷/二乙烯基苯(polydimethylsiloxane/divinylbenzene,PDMS/DVB)为萃取纤维的方法鉴定出41种挥发性成分,以二乙烯基苯/Carboxen/聚二甲基硅氧烷(Divinylbenzene/Carboxen/Polydimethylsiloxane,CAR/PDMS/DVB)为萃取纤维的方法鉴定出40种挥发性成分;3种纤维萃取的分析结果相互补充,共鉴定出51种挥发性成分,其中酯类、醛酮类和内酯类化合物的含量最高,分别为26.12%、25.95%和15.16%,是该种奶味香精的主要组成成分。     

Identification of volatile flavor compounds in Chinese Sinkiang camel-naizi using different solid phase microextraction fibers

Volatile components of Chinese Sinkiang camel-naizi (CSCN) were analyzed using solid phase microextraction-gas chromatography/mass spectrometry (SPME-GC/MS). A total of 45 volatile compounds were identified by using 3 fibers, including 17 alcohols, 4 aldehydes, 13 acids, 8 esters, 1 sulfur-containing compound, 1 lactone, and 1 ketone. Among all the compounds identified, various alcoholic compounds accounted for 78.91% of the total volatiles, and the amount of various esters was only next to that of alcohols, which accounted for 15.01% of the total volatiles. The content of acids, lactone, aldehydes, ketone, and sulfur-containing compound accounted for 6.08%. All of these volatiles constituted the characteristic flavor of raisin-like, fruity, sweet, cheesy, and yogurt-like note of CSCN. The extraction performances of 3 types of SPME fibers (75 μm CAR/PDMS, 65 μm PDMS/DVB, and 50/30 μm DVB/CAR/PDMS) were compared in this study. Of the 3 fibers, the DVB/CAR/PDMS fiber extracted the most volatiles, and the CAR/PDMS fiber the least. The DVB/CAR/PDMS fiber showed the best performance in trapping compounds of CSCN with different polarities.     

Chemical analysis of French beans (Phaseolus vulgaris L.) by headspace solid phase microextraction (HS-SPME) and simultaneous distillation/extraction (SDE)

Headspace Solid Phase Microextraction (HS-SPME) involving divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fibre and simultaneous distillation/extraction (SDE) techniques were applied to study the volatile and semi volatile compounds of thawed and cooked Phaseolus vulgaris L. A total of 104 compounds were detected by GC and GC/MS. Thereof, 76 compounds were identified for the first time in this species. The major differences between HS-SPME and SDE were found in the content of identified alcohols (23.62% SDE versus 62.20% SPME), terpenoids (39.15% SDE versus 2.45% SPME), heterocyclic compounds (13.78% SDE versus 1.21% SPME), hydrocarbons (2.22% SDE versus 13.87% SPME) and esters (0.98% SDE versus 12.98% SPME). The SPME technique was found to be useful for rapid and routine quality controls of thawed French beans, while SDE is favourable to study the entire set of flavour volatiles in the corresponding cooked samples.     

Influence of the Type of Extraction Conditions and Fiber Coating on the Meat of Sauced Duck Neck Volatile Compounds Extracted by Solid-Phase Microextraction (SPME)

In this paper, extraction of sauced duck neck meat volatile compounds by solid-phase microextraction (SPME) was optimized. Three extraction temperatures (30, 45, 60 °C), three extraction times (15, 30, 45 min), and three different fiber coatings (divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS), polydimethylsiloxane/divinylbenzene (PDMS/DVB), and polydimethylsiloxane (PDMS)) were assayed. There were 82 volatile compounds identified and quantified, which belonged to nine families of chemicals including alcohols, acids, esters, ketones, aldehydes, aromatic compounds, heterocycles, monoterpenes, oxygenated monoterpenes, and sesquiterpenes. The major volatile compounds of sauced duck neck came from spices addition, oxidation, Maillard reaction, etc. Almost all the compounds were extracted by the DVB/CAR/PDMS fiber at 45 °C, and the optimal time of extraction in this case was 15 min, during which DVB/CAR/PDMS fiber reached equilibration. Among the fibers tested, DVB/CAR/PDMS fiber favored the extraction of a wide range of compounds with low and high boiling point. On the other hand, PDMS/DVB fiber absorbed more polar and high retention index (RI) aromatic compounds.     

同时蒸馏萃取-气质联用分析养殖暗纹东方鲀肉中的挥发性成分

分别以二氯甲烷和乙醚作溶剂,同时蒸馏萃取(SDE)养殖暗纹东方鲀肉中的挥发性成分,结合气质联用(GC-MS)对挥发性成分进行定性,以2,4,6-三甲基吡啶内标定量分析,并结合主成分分析法(PCA)对挥发性成分进行数据挖掘。结果表明:乙醚为溶剂时,总共鉴定到了57种成分,含量较高的是十四醛(4 963.71ng/g)、十八醛(1 171.51ng/g)、(Z)-13-十八醛(2 007.21ng/g)、乙酸乙酯(1 148.44ng/g)、十六酸(4 639.90ng/g)等;以二氯甲烷为溶剂时,总共鉴定到了78种成分,主要是十六醛(2 381.77ng/g)、2,3-丁二酮(1 267.40ng/g)、十六酸(545.08ng/g)等。比较得出,二氯甲烷溶剂在定性方面有优势,乙醚溶剂在定量方面效果较好。2种溶剂萃取一共检测出96种化合物,其中醛类29种、酮类11种、醇类16种、含氮含硫及杂环类化合物22种、酯类7种、酸类3种、烷烃类8种。     

同时蒸馏萃取结合GC-MS分析红托竹荪挥发性成分

采用同时蒸馏萃取法提取红托竹荪中的挥发性成分,用气相色谱一质谱联用（GC—MS）对挥发性成分进行了分析。结果表明通过双柱定性,以乙醚为溶剂时鉴定出81种成分,以二氯甲烷为溶剂时鉴定出89种成分;两种溶剂共计鉴定出108种挥发性成分,其中醛类11种、酮类8种、醇类9种、酚类2种、酯类15种、酸类23种、烃类17种、杂环类17种、其他类6种,其中含量较大的有亚油酸、棕榈酸、棕榈油酸、十五烷酸、11-顺-十八碳烯酸、醋酸、乙偶姻、肉豆蔻酸、十五碳酸、天然麝香葵子等。     

HS-SPME-GC-MS分析新疆胡麻油挥发性成分的技术优化

采用顶空固相微萃取-气相色谱-质谱(headspace solid phase microextraction-gas chromatography-mass spectrometry,HS-SPME-GC-MS)联用技术对新疆胡麻油挥发性成分测定分析进行优化,以期获得HS-SPME-GCMS分析胡麻油挥发性香气的最佳条件。结果表明,采用DVB/CAR/PDMS萃取头,在磁力搅拌条件下,胡麻油SPME最佳萃取条件为萃取温度50℃、萃取时间40 min、解吸时间4 min,在该条件下采用HS-SPME-GC-MS鉴定出的胡麻油挥发性物质达到46种,主要包括醛类、酮类、醇类、酸类、酯类、烷烃类、杂环类及其他类物质,其中醛类、杂环类和醇类总相对含量较高,分别为30.14%、12.73%和9.25%,分离鉴定效果较好。     

Analysis of volatile composition of siriguela (Spondias purpurea L.) by solid phase microextraction (SPME)

In order to investigate the volatile composition of the siriguela fruit (Spondias purpurea L.), the pulp of the fresh fruit was submitted to solid phase microextracton (SPME) using different fibers, divinylbenzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS), carbowax-divinylbenzene (CW/DVB), carboxen-polydimethylsiloxane (CAR/PDMS) and polydimethylsiloxane (PDMS) fibers. DVB/CAR/PDMS showed to be the more efficient qualitative and semi-quantitatively fiber in trapping these compounds. It was made possible to identify ketones, alcohols, aldehydes, esters and terpenic hydrocarbons in the headspace. The major compounds identified were hexanal, trans-2-hexenal, 3-hexen-1-ol, 2-hexen-1-ol, ethyl acetate and hexyl acetate. To have a clear picture of the retention indices of these compounds a new protocol, in which the standard hydrocarbon mixture is submitted to SPME, was developed and successfully used.     

Analysis of volatile compounds in traditional smoke-cured bacon(CSCB) with different fiber coatings using SPME

The volatile compounds of Chinese traditional smoke-cured bacon (CSCB) were studied using SPMS-GC/MS. There were 48 volatile compounds identified and quantified, which belonged to several classes of chemical: 1 alkane, 16 aldehydes, 5 ketones, 9 alcohols, 4 thioethers and thiols, 3 furans and 10 phenols compounds. All the volatile compounds except for alkane was responsible for CSCB characteristic flavor. The major volatile compounds of CSCB came from smoking, oxidation and Maillard reaction, etc. Many volatile compounds were not reported in previous paper isolated by steam distillation method or nitrogen purge-and-steam distillation method on CSCB. It should be because of different method of isolating volatile substances from CSCB. Among the fibers tested, CAR/PDMS (carboxen/polydimethylsiloxane) fiber coating showed the highest area counts for most volatile compounds. CAR/PDMS coating extracted better those compounds whose linear retention indices (LRI) was lower than 926 (on average) and DVB/CAR/PDMS (divinylbenzene/carboxen/polydimethylsiloxane) those with higher LRI.     

基于HS-SPME-GC-MS和PCA的不同萃取头对鸡肉香精香气成分萃取效果比较

为提高鸡肉香精香气成分分析的可靠性,比较不同纤维涂层萃取头萃取鸡肉香精香气成分的效果,采用顶空固相微萃取(headspace solid-phase micro-extraction,HS-SPME)结合气相色谱质谱联用仪(gas chromatography-mass spectrometry,GC-MS)检测技术对热反应鸡肉香精中的挥发性风味物质种类和组成进行提取分析,通过灵敏性及主成分分析(principal component analysis,PCA)法比较香气成分数量及含量建立香气品质评价模型,研究不同纤维涂层萃取头(75μm CAR/PDMS、65μm DVB/PDMS、85μm PA、50/30μm DVB/CAR/PDMS)与所萃取挥发性物质间的相关性。结果表明,75μm CAR/PDMS萃取头为萃取鸡肉香精样品挥发性物质的最优萃取头,萃取得到样品中共含有146种挥发性物质,包括醇类24种(16.44%)、醛类16种(10.96%)、吡嗪类12种(8.22%)、呋喃(酮)类13种(8.91%),含硫化合物10种(6.85%)等多种香气物质,检测到2-甲基-3-呋喃硫醇、2-甲基-3-戊烷硫醇、(E,E)-2,4-癸二烯醛、(E,E)-2,4-庚二烯醛及反式-2-壬烯醛等关键肉香味化合物。     

发酵牛肉肠挥发性成分固相微萃取条件优化分析

利用固相微萃取法和气相色谱-质谱法分析发酵牛肉肠中的挥发性风味物质。通过单因素和正交试验对其萃取条件进行优化,所得最佳萃取条件为DVB/CAR/PDMS萃取头、萃取时间60 min、萃取温度65 ℃、样品萃取量3 g、解吸时间2 min。在此条件下,检测到发酵牛肉肠中的挥发性成分共88 种,分别为17 种醛类、23 种醇类、9 种酮类、7 种酸类、16 种烃类、10 种杂环类、3 种酯类和3 种其他种类的物质。     

同时蒸馏萃取-气相色谱-质谱联用分析汉麻叶挥发性成分

采用同时蒸馏萃取法结合气相色谱-质谱联用对汉麻叶的挥发性成分进行分析,考察以二氯甲烷为萃取溶剂,不同萃取时间对分析结果的影响。结果表明:最佳萃取时间为4h,从汉麻叶中鉴定出44种挥发性成分,占挥发油总组分的86.04%,其中酮类7种(4.67%)、酚类2种(6.13%)、醛类4种(3.88%)、醇类8种(15.35%)、烃类13种(29.40%)、杂环化合物类2种(0.97%)、其他8种(25.64%)。在鉴定出的成分中含量较多的是石竹烯氧化物(14.36%)、石竹烯(8.08%)和α-石竹烯(7.05%)等。     

欧姆加热对豆浆风味物质的影响

为研究欧姆加热对豆浆挥发性物质的影响,采用顶空固相微萃取结合气相色谱-质谱联用技术,对豆浆的风味物质进行分析,利用内标法对各风味物质成分定量分析。通过对比50/30?μm二乙基苯/碳分子筛/聚二甲基硅氧烷（divinylbenzene/carboxen/polydimethylsiloxane,DVB/CAR/PDMS）、100?μm PDMS、65?μm PDMS/DVB 3 种萃取头对豆浆风味物质的萃取效果,筛选出最佳的萃取头,并在最适条件下分析豆浆的风味物质成分,为排除热效应对实验结果的影响,2?种热处理历程尽可能保持一致。结果表明：65?μm PDMS/DVB纤维萃取头较100?μm PDMS和50/30?μm DVB/CAR/PDMS纤维萃取头更适宜豆浆风味物质的测定;从豆浆样品中共检测到35?种挥发性物质,其中醛类物质16?种,醇类物质5?种,酮类物质3?种,酯类物质1?种,杂环烃类物质10?种,主要包括己醛、（E）-2-庚烯醛、1-辛烯-3-醇等,这些物质共同组成豆浆的特征香气;不同加热处理对豆浆风味物质种类的影响不大,但是对特征香气含量有显著影响（P＜0.05）;欧姆加热处理组样品中己醛、1-辛烯-3-醇、（E）-2-辛烯醛的含量分别比传统加热处理组约低45.55%、58.60%、25.56%,且在欧姆加热处理样品组中未检测到（E）-2-己烯醛和正己醇,而这些物质是豆腥味的主要组成成分。因此,利用欧姆加热方式加热豆浆可以显著降低豆浆的豆腥味。本研究可以为欧姆加热技术在豆浆加工业中的应用提供理论依据。     

Volatile compounds of dry-fermented sausages as affected by solid-phase microextraction (SPME)

The analysis of volatile compounds from the headspace of dry-fermented sausages was done by solid-phase microextraction (SPME). The effects of exposure time and fibre coating were investigated. A total of 90 different compounds were extracted by the two fibre coatings and these were identified. Sixty-six compounds were extracted by divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) coating and were identified, while 24 more were found with the carboxen/polydimethylsiloxane (CAR/PDMS) fibre. These 24 volatile compounds were mainly of low molecular weight. Four of the major compounds extracted: acetic acid, ethanol, hexanal and butanoic acid, were in high proportions in the two fibre coatings. However, the main differences were a higher affinity of DVB/CAR/PDMS for aldehydes while, for CAR/PDMS fibre, the higher affinity was for ester compounds. The extraction yields of dry fermented sausages volatile compounds varied according to the fibre coating used and the time of exposure, although competition effects were detected due to the high generation of lipid oxidation products, such as hexanal.     

SDE and SPME Analysis of Flavor Compounds in Jin Xuan Oolong Tea

Simultaneous distillation‐extraction (SDE) and solid phase micro extraction (SPME) are procedures used for the isolation of flavor compounds in foods. The purpose of this study was to optimize SDE conditions (solvent and time) and to compare SDE with SPME for the isolation of flavor compounds in Jin Xuan oolong tea using GC‐MS and GC‐O. The concentration of volatile compounds isolated with diethyl ether was higher (P < 0.05) than for dichloromethane and concentration was higher at 40 min (P < 0.05) than 20 or 60 min extractions. For SDE, 128 volatiles were identified using GC‐MS and 45 aroma active compounds using GC‐O. Trans‐nerolidol was the most abundant compound in oolong tea. The number of volatiles identified using GC‐MS was lower in SPME than SDE. For SPME, 59 volatiles and 41 aroma active compounds were identified. The composition of the volatiles isolated by the 2 methods differed considerably but provided complementary information.     

刺梨汁中挥发性成分测定及其呈香贡献分析

为全面剖析刺梨中挥发性成分的组成及其呈香贡献,采取顶空固相微萃取(headspace-solid phase micro-extraction,HS-SPME)和溶剂辅助风味蒸发(solvent-assisted flavor evaporation,SAFE)结合GC-MS对刺梨汁挥发性成分进行分析,通过香气活度值(...     

Comparison of isolation methods for the determination of buckwheat volatile compounds

Five different isolation techniques were combined with gas chromatographic–mass spectrometric determination of aroma compounds from buckwheat: dynamic headspace (DHS) with cryotrapping or sorbent trapping, solid-phase microextraction (SPME), headspace sorptive extraction (HSSE), solvent extraction (SE) and simultaneous distillation–extraction (SDE). Optimisation of each technique is presented, as well as comparison of the chemical profiles obtained by them. Solvent extraction with methanol resulted in the isolation of rather polar and less volatile compounds and was deemed least suitable for the odour-active compounds. Only SPME with DVB/CAR/PDMS fibre was suitable for the isolation of highly volatile compounds in a wider polarity range. DHS extracted the smallest number of compounds, but with the comparable chemical profile as obtained by SDE, which was chosen as the most suitable technique to obtain the aroma compounds of cooked buckwheat. The applied isolation techniques are complementary in their ability to extract a representative aroma profile of buckwheat.     

Volatile Components in Salt-Fermented Fish and Shrimp Pastes

Volatile compounds in salt-fermented anchovy, big-eyed herring, hair tail viscera, and shrimp pastes were compared by simultaneous steam distillation-solvent extraction/gas chromatography/mass spectrometry (SDE/GC/MS). A total of 155 volatile compounds were detected. Of these, 111 were positively identified consisting mainly of aldehydes, ketones, alcohols, esters, aromatics, nitrogen-, and sulfur-containing compounds. Lipid-derived components, such as aldehydes, alcohols, and esters, comprised the majority of volatile compounds from fish pastes, while heterocyclic nitrogen-containing compounds, such as pyrazines, were predominant in shrimp paste.     

血浆蛋白粉对猪肉凝胶中挥发性风味物质的影响

采用顶空固相微萃取与气质联用方法,分析血浆蛋白粉对猪肉凝胶挥发性风味物质的影响。结果表明:选用75μm CAR/PDMS萃取头,55℃萃取40min,可得到较好的萃取效果;猪肉中添加血浆蛋白粉后,从其凝胶中新检出挥发性风味物质16种,包括酮类1种、醇类3种、酸类2种、碳氢化合物7种、杂环类1种、醚类1种和酯类1种。