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。     

萃取头对甜面酱中挥发性成分分析的影响

采用顶空固相微萃取(HS-SPME)与气质联用(GC-MS)相结合对甜面酱中挥发性成分进行了初步分析,比较了4种不同涂层纤维的萃取头(30μm PDMS,65μm PDMS/DVB,75μm CAR/PDMS,50/30μm DVB/CAR/PDMS)对甜面酱挥发性成分的萃取效果和特点。结果表明:在相同实验条件下,50/30μm DVB/CAR/PDMS萃取头萃取到的色谱总峰面积和化合物种类最多,而75μm CAR/PDMS萃取头可以萃取到最多的香气成分。因此50/30μm DVB/CAR/PDMS萃取头最适合甜面酱挥发性成分的检测,同时可以用75μm CAR/PDMS萃取头来进行补充。     

SPME萃取头对大菱鲆鱼肉挥发性成分萃取效果分析

采用DVB/CAR/PDMS、PDMS/DVB和CAR/PDMS 3种萃取头进行顶空-固相微萃取(HS-SPME),提取新鲜大菱鲆鱼肉的挥发性成分,结合气质联用仪(GC-MS)进行分析鉴定,确定最佳的萃取头.结果表明,3种萃取头固相微萃取法共检测出81种挥发性成分,主要是醛、酮、醇、烯烃、烷烃和胺类化合物.使用DVB/CAR/PDMS、PDMS/DVB和CAR/PDMS萃取头分别检测出51、37和29种挥发性成分,其中使用DVB/CAR/PDMS萃取头检测出的挥发性物质总峰面积最大且种类最多.因此,DVB/CAR/PDMS萃取头较适合于大菱鲆鱼肉挥发性成分的提取.     

不同萃取头对分析普洱熟茶挥发性成分的影响

采用100μm PDMS、85μm PA、75μm CAR/PDMS、70μm CW/DVB、65μm PDMS/DVB、50/30μm DVB/CAR/PDMS 6种萃取头提取普洱熟茶挥发性成分,经气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)对挥发性成分进行鉴定,分析比较了6种萃取头提取挥发性成分的差别。6种萃取头共检测出83种挥发性化合物,醇类10种,醛类8种,甲氧基苯类9种,碳氢类30种,酮类10种,酯类8种,含氮类5种,酚类2种,酸类1种。试验发现75μm CAR/PDMS无论从萃取化合物数量还是总峰面积,均明显优于其他5种萃取头。因此,根据获得挥发性物质数量和总峰面积,CAR/PDMS萃取头更适于提取分析普洱熟茶中挥发性香气成分。     

基于SPME-GC-MS与PCA的不同萃取头萃取刺梨汁香气成分效果比较

为提高刺梨汁香气成分气相色谱分析的准确可靠性,比较不同纤维涂层萃取头萃取刺梨汁香气成分的效果及灵敏度。采用50/30μm DVB/CAR/PDMS、75μm CAR/PDMS、65μm PDMS/DVB、100μm PDMS 4种萃取头进行刺梨汁香气成分的富集和浓缩处理,气质联用仪检测其香气成分,通过主成分分析法,对其香气成分的数量、含量进行比较,建立香气品质评价模型。结果表明,刺梨汁香气成分以酯类、醇类、萜烯类为主,不同萃取头萃取的化合物存在明显差异,50/30μm DVB/CAR/PDMS萃取化合物59种,相对含量最多为93.96%,其中酯类、醇类呈香物质含量最高;65μm PDMS/DVB萃取出38种化合物,相对含量为91.19%;100μm PDMS萃取出29种化合物,相对含量92.79%;75μm CAR/PDMS萃取出26种化合物,相对含量92.08%。在4种纤维涂层萃取头中,以50/30μm DVB/CAR/PDMS为富集刺梨汁香气成分的最佳萃取纤维。     

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。     

顶空固相微萃取-气相色谱-质谱联用法分析椪柑芳香水中挥发性成分

采用顶空固相微萃取-气相色谱-质谱联用法(HS-SPME-GC/MS)分离鉴定椪柑芳香水中的挥发性成分,研究固相微萃取头种类(PDMS/DVB 65μm,CAR/PDMS 75μm和DVB/CAR/PDMS 50/30μm)、吸附温度(30~50℃)、吸附时间(5~30 min)和样品体积(2~10 m L)对椪柑芳香水分离效果的影响。试验结果表明,采用DVB/CAR/PDMS固相微萃取头,样品体积8 m L,在温度40℃下吸附20 min,能达到最佳吸附效果。椪柑芳香水中主要的挥发性成分为:d-柠檬烯40.85%,乙醇17.17%,α-萜品醇15.61%,1-辛醇6.20%,β-月桂烯3.48%,3-甲基-1-丁醇3.01%,β-芳樟醇2.93%,樟脑2.88%,辛酸乙酯2.34%,α-蒎烯1.47%,占峰面积总和的95.94%。对顶空固相微萃取法进行重复性试验,10种挥发性成分的相对标准偏差(RSD)均低于7.0%,表明应用HS-SPMEGC/MS联用技术可对椪柑芳香水中挥发性成分进行快速、准确地分析。     

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。     

不同固相微萃取萃取头在浓香型白酒风味分析的对比研究

以PEG、PA、PDMS/DVB、CAR/PDMS和DVB/CAR/PDMS等5种萃取头为对象,比较了不同萃取头对浓香型白酒挥发性风味物质萃取的效果和特点。结果表明,复合涂层萃取头在检出物数量及丰度方面均优于单涂层的萃取头;PEG对缩醛类物质和己酸乙酯的萃取效率最低;PA萃取头对醇类化合物的吸附能力较强;PEG和PA萃取头对酸类的萃取效果较好;DVB/CAR/PDMS萃取头对己酸乙酯吸附能力最强;CAR/PDMS和DVB/CAR/PDMS萃取头对呋喃类、醛及缩醛类均有较高的吸附能力。     

SPME萃取头对茶油挥发物萃取效果的影响

固相微萃取目前被广泛地用来测定液态、气态,甚至固态物质的挥发组分,不同待测物的性质决定了萃取头的种类选择.采用4种常用的SPME涂层萃取头(100μmPDMS、85μmPA、65 μmaPDMS/DVB、50/30 μm DVB/CAR/PDMS)对荼油挥发物的提取性能进行了比较研究,结果表明:65 μmPDMS/DVB萃取头对较高沸点物质如苯甲醛、正辛醛、正辛醇、正壬醛、正壬醇的吸附比50/30 μmDVB/CAR/PDMS萃取头要灵敏,但50/30μmDVB/CAR/PDMS萃取头对较低沸点物质的吸咐要灵敏很多.DVB/CAR/PDMS涂层萃取头所得的总峰面积的平均值最大,其余依次是PDMS/DVB、PA、PDMS;DVB/CAR/PDMS、PDMS/DVB、PA、PDMS对挥发物吸咐总峰面积与挥发物总量之间存在有线性关系,其相关系数(R2)分别是0.9939、0.9888、0.9176、0.9917;因此,65 μmPDMS/DVB和50/30μm DVB/CAR/PDMS的萃取头较适用于茶油挥发物的提取.     

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.     

Influence of the type of fiber coating and extraction time on foal dry-cured loin volatile compounds extracted by solid-phase microextraction (SPME)

Extraction of dry-cured loin volatile compounds by solid-phase microextraction (SPME) was optimized. Two different fiber coatings: carboxen/polydimethylsiloxane (CAR/PDMS) and divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS), and three extraction times (15, 30 and 45 min) were assayed. Between the fibers tested, CAR/PDMS coated fibers extracted between two and three times more total amount of volatile compounds than the DVD/CAR/PDMS coating (1314 × 10⁶ vs. 526 × 10⁶ area units). Fifty five compounds were extracted by the CAR/PDMS fiber, while only 48 of these were found with the DVB/CAR/PDMS fiber. On the other hand, 6 additional volatile compounds were extracted by the CAR/PDMS coating, all of them being of low molecular weight. Three of the major compounds extracted, hexanoic acid, methyl ester; butanoic acid, 3-methyl-, methyl ester and hexanal, were found in high proportion in both fiber coatings. The effect of exposure time was more marked for the DVD/CAR/PDMS fiber than for the CAR/PDMS coating. Fifteen minutes of extraction provided a volatile compounds profile with lower area counts for most compounds and significantly different to that obtained with 30 and 45 min of extraction. The extraction yields of dry-cured loin volatile compounds varied according to the fiber coating used and the time of exposure. Therefore, extraction conditions should be selected depending on the objective of the study. Finally, it can be concluded that both porous fibers tested, CAR/PDMS and DVB/CAR/PDMS, provide a similar volatile compounds profile for dry-cured foal loin.     

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.     

顶空固相微萃取分析金黄色葡萄球菌挥发性代谢产物的条件优化

采用65 μm聚二甲基硅氧烷/二乙基苯（polydimethylsiloxane/divinylbenzene,PDMS/DVB）、75 μm碳分子筛/聚二甲基硅氧烷（carboxen/polydimethylsiloxane,CAR/PDMS）萃取头和50/30 μm二乙基苯/碳分子筛/聚二甲基硅氧烷（divinylbenzene/carboxen/polydimethylsiloxane,DVB/CAR/PDMS）萃取头,20、30 min和40 min 3 种萃取时间,50、65 ℃和80 ℃ 3 种萃取温度,分别对金黄色葡萄球菌胰蛋白胨大豆肉汤（tryptone soy broth,TSB）培养物的挥发性代谢产物进行萃取,经气相色谱-质谱检测,以建立适宜于金黄色葡萄球菌挥发性代谢物的萃取分析方法。结果表明,50/30 μm DVB/CAR/PDMS萃取头能更好地满足各类化合物的萃取需要,获得更加全面的化合物信息,并且在萃取温度80 ℃条件下萃取30 min,得到的金黄色葡萄球菌挥发性代谢物的数量和响应强度较高。因此,萃取金黄色葡萄球菌挥发性代谢产物的最适条件为：50/30 μm DVB/CAR/PDMS萃取头、萃取温度80 ℃、萃取时间30 min。在该萃取条件下,检测出金黄色葡萄球菌在TSB中产生的主要挥发性物质为乙醇、1-癸醇、3-羟基-2-丁酮、丙酮、乙酸、苯甲醇、3-甲基-1-丁醇、吲哚、1-辛醇和正辛酸等。该萃取方法的建立可为细菌挥发性代谢产物的分析提供参考。     

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。     

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.     

Optimisation of solid phase microextraction (SPME) for the analysis of volatile compounds in dry‐cured ham

Solid phase microextraction (SPME) has been shown to be an effective tool for analysing volatile compounds. The aim of this study was to optimise the conditions for the application of SPME in the analysis of volatile compounds in dry‐cured ham. The effects of exposure time and fibre coating were investigated while maintaining the dry‐cured ham at 30 °C to avoid artefact generation due to possible temperature effects. A divinylbenzene/Carboxen on polydimethylsiloxane (DVB/CAR/PDMS) coating showed the best extraction performance for medium‐ and high‐molecular‐weight analytes, whilst a Carboxen on polydimethylsiloxane (CAR/PDMS) coating gave the best results for low‐molecular‐weight compounds. A total of 70 different compounds were extracted by the two fibre coatings and identified. Sixty compounds were extracted by the DVB/CAR/PDMS fibre, whilst only 41 of these were found with the CAR/PDMS fibre. On the other hand, 10 additional volatile compounds were extracted by the CAR/PDMS coating, all of them being of low molecular weight. Two of the major compounds extracted, hexanal and 2‐pentanone, were found in high proportion in both fibre coatings. The extraction yields of dry‐cured ham volatile compounds varied according to the fibre coating used and the time of exposure. Therefore extraction conditions should be selected depending on the objective of the study. © 2002 Society of Chemical Industry