固相微萃取和气—质联用技术在快速测定苹果挥发性成分中的应用

固相微萃取技术(SPME)是一种新型的样品前处理方法。在挥发性成分测定中,它集取样、萃取、进样和浓缩为一体,不仅简化了传统前处理方法的步骤,而且在样品处理过程中由于无需有机溶剂,因此不会造成二次污染。本实验是采用SPME和GC╱MS(气质联用仪)技术分析苹果中的香气成分,分析总离子色谱图,共鉴定出48种挥发性成分,按峰面积计算占其香气成分的98％。     

绿茶香气成分研究

以绿茶为原料,采用固相微萃取(SPME)、液液萃取(LLE)、同时蒸馏萃取(SDE)和顶空蒸馏萃取(HDE)4种方法提取绿茶的香气成分并进行了GC-MS分析。结果表明,SPME适宜于分析绿茶的易挥发性香气成分;直接液液萃取不适用于绿茶香气的提取;HDE和SDE适宜于分析绿茶的中等挥发性香气成分,但HDE法的香气品质高于SDE法。结果表明SPME和HDE结合可以有效地分析绿茶的香气成分。     

固相微萃取在发酵酒香气检测上的应用

1香气物质的萃取方法-固相微萃取和顶空固相微萃取 1.1固相微萃取(SPME)简介[1] 固相微萃取法(Solid-Phase Microextraction,SPME)是加拿大学者Arhturhe和Pa wliszyn首创的一项样品分析前处理新技术.     

萃取方法对樱桃酒香气成分的影响

利用顶空固相微萃取(SPME)、搅拌棒吸附萃取(SBSE)和液液萃取(LLE)方法结合GC-MS对樱桃酒香气成分进行分析,对比研究3种方法对樱桃酒香气成分萃取的特性。结果表明:不同的萃取方法得到的香气物质各不相同,其中SPME能富集到更高含量的香气成分,SBSE对痕量和超痕量的挥发物有较好的萃取效果,而LLE能富集到较多的香气种类。采用3种方法共提取到87种香气物质,共同检测到的成分20种,通过偏最小二乘回归法分析(PLSR)不同的香气提取方法和香气物质之间的相关性。     

SPME和P&T对西瓜汁香气成分萃取条件优化及二者的比较分析

为了充分萃取西瓜汁的香气成分,避免萃取方法及条件对西瓜汁香气成分分析的影响,本研究优化了前处理方法中PT的时间和温度、SPME中的萃取纤维、温度和时间,并将这两种方法的萃取效果进行了比对分析。研究表明,PT的平衡温度50℃、吹扫时间30min能达到最佳的萃取效果;SPME优化的最佳萃取条件是:CAR/DVB/PDMS纤维、平衡温度40℃、平衡时间40min。这两种方法的对比研究表明,SPME对西瓜汁的萃取效果明显优于PT。     

HS-SPME arrow-GC/MS结合化学计量学分析烟草香气突变体中特征香气成分

为明确特征香韵烟草突变体(萨姆逊香)与对照中烟100中香气成分的差异,优化烟草挥发性香气成分检测方法,通过考察箭型固相微萃取(SPME arrow)萃取头类型、平衡时间、萃取时间和萃取温度等样品前处理条件,建立了测定烟草中挥发性香气成分的顶空-箭型固相微萃取-气相色谱质谱联用(HS-SPME arrow-GC/MS)方法;采用该方法对两个材料进行了检测,并结合主成分分析(PCA)和偏最小二乘-判别分析(PLS-DA)方法分析了萨姆逊香烟草突变体中的特征香气成分。结果表明:①SPME arrow优化萃取条件为120μm×20 mm活性炭/聚二甲基硅氧烷(CAR/PDMS)萃取头,70℃下平衡40min,萃取40 min;在此条件下,质控样(QC)中相对标准偏差30%的色谱峰数量占总峰数量的89.3%。②从两个材料中共筛选出差异香气成分33种,萨姆逊香突变体材料中29种成分的含量高于中烟100。该方法操作简单,重现性好,结果稳定可靠,适用于烟叶特征香气成分的分析。     

固相微萃取GC-MS技术在梨香气成分分析中的应用研究

用固相微萃取技术(SPME)提取梨果实中香气成分,对影响萃取效果的因素及实验参数进行探讨、优化,确定了最佳萃取条件,同时结合GC/MS对提取的成分进行分析鉴定,为梨果实中香气成分的快速测定提供技术保证。     

新疆库尔勒香梨的香气成分分析

采用SDE(同时蒸馏萃取)和SPME(固相微萃取)两种萃取技术分离新疆库尔勒香梨的香气成分,用GC/MS分析鉴定,对总离子流色谱的峰面积进行归一化定量。通过比较两种分离技术的检测结果,同时结合GC-Olfactometry(GC-嗅探方法)对香气成分进行感官描述,得出:SPME方法分离的己醛、己酸乙酯、丁酸乙酯、乙酸乙酯、乙酸己酯、乙醇、油酸乙酯、(E)2-己烯醛、α-法尼烯、甲酸辛酯、乙酸丁酯、反-2-顺-4-癸二烯酸乙酯等化合物够较好地体现出库尔勒香梨固有的香气。     

不同萃取方式分析武夷水仙茶挥发性成分

分别采用同时蒸馏萃取(SDE)、静态顶空(SHS)和固相微萃取(SPME)三种不同香气萃取方式提取香气物质,进行气相色谱-质谱(GC-MS)分析,结合保留指数法对武夷水仙茶的挥发性物质进行了研究。三种萃取方法共鉴定出179种挥发性成分,其中SDE法121种、SPME法114种及SHS法61种。三种方法共有化合物有21种,SDE和SPME法共有化合物有72种,SHS和SDE共有化合物有25种,SHS和SPME共有化合物有37种。进一步分析已确定的挥发性成分,SDE比SPME多分离出醇类5种、烷烃类6种、酸类2种、酯类1种、酚类1种及醌类1种;SPME比SDE多分离出杂环类2种、醛类4种、芳香烃类1种及烯类2种。结果表明,SDE和SPME两种方法结合提取茶叶中的香气物质可以更全面,共鉴定出162种化合物。以花香、果香、木香、坚果香、烘焙香、焦糖香的香气物质为主。     

1-MCP处理对南果梨20℃贮藏期香气成分的影响

利用固相微萃取技术(solid phase micro extraction,SPME)与气相色谱- 质谱(gas chromatography-mass spectrometry,GC-MS)相结合对1-methylcyclopropene(1-MCP)处理南果梨20℃贮藏香气成分进行研究。结果表明：南果梨香气成分的释放与果实的后熟程度有很大的关系,总体上呈现先上升后略下降的趋势;1-MCP 处理延长了南果梨20℃贮藏期,但减少了香气成分种类;处理组检出果实香气的种类比对照组减少了27.8%,其中酯类香气种类比对照果减少了31.3%。     

Solid phase microextraction of stale flavour volatiles from the headspace of UHT milk

Solid phase microextraction (SPME) offers a solvent‐free and less labour‐intensive alternative to traditional flavour isolation techniques. In this instance, SPME was optimised for the extraction of 17 stale flavour volatiles (C3–11,13 methyl ketones and C4–10 saturated aldehydes) from the headspace of full‐cream ultrahigh‐temperature (UHT)‐processed milk. A comparison of relative extraction efficiencies was made using three fibre coatings, three extraction times and three extraction temperatures. Linearity of calibration curves, limits of detection and repeatability (coefficients of variation) were also used in determining the optimum extraction conditions. A 2 cm fibre coating of 50/30 µm divinylbenzene/Carboxen/polydimethylsiloxane in conjunction with a 15 min extraction at 40 °C were chosen as the final optimum conditions. This method can be used as an objective tool for monitoring the flavour quality of UHT milk during storage. Copyright © 2005 Society of Chemical Industry     

Relationships of Overall Estery Aroma Character in Lagers with Volatile Headspace Congener Concentrations

In lager beers the intensity of “estery” aroma character is regarded as an important component of sensory quality, but its origins are somewhat uncertain. Overall “estery” aroma intensity was predicted from capillary gas chromatographic (GC) data following solid phase micro extraction (SPME) of headspaces. Estery character was scored in 23 commercial lagers using rankrating, allowing assessors (13) constant access to a range of appropriate standards. From univariate data analysis, all assessors behaved similarly and lagers fell into three significantly different groups: low (1), high (1) and intermediate (21). The quantification of 36 flavour volatiles by SPME of headspaces was reproducible and principal component analysis explained 91% total variance. Multiple linear regression could utilise only a restricted (26) set of flavour volatiles, whereas partial least square regression, that considered all flavour components, showed significant differences and improved prediction. However, an artificial neural network that could compensate for non‐linearities and interactions in ester perception gave the most robust prediction at R² = 0.88.     

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.     

Contribution to aroma potential of Andean blackberry (Rubus glaucus Benth.)

Free and glycosidically bound volatiles of purees from Andean blackberry (Rubus Glaucus Benth.) fruit were determined. Free volatile compounds were extracted by two techniques: solvent extraction and Solid-Phase Micro-Extraction (SPME). The glycosidically bound volatiles were isolated using Solid Phase Extraction (SPE) technique. The analysis of free volatiles and enzymatically released aglycons were performed by GC-MS. Fifty five volatile compounds were identified and quantified from solvent extraction. The major class was the carboxylic acids (68.8%), dominated by palmitic acid (16.8%) and benzoic acid (15.0%). Alcohols were highly represented (23.4%), with 2-heptanol (10.6%) and terpinen-4-ol (5.7%) being prevalent compounds of this class. Using HS-SPME, among the seventy-one identified compounds, alcohols (47.3%) including 2-heptanol (17.9%) and terpinen-4-ol (20.0%), and esters (39.8%) with ethyl and methyl benzoate (33.9 and 3.8% respectively) were the two predominant classes. ??-damascenone, a potent flavour compound was detected using SPME method. Fifty-three aglycons were identified, acids (57.4%), norisoprenoids (15.4%), terpenic alcohols (10.3%) and some aliphatic and shikimic alcohols (15.0%) predominated in the glycosidically bound fraction. Acetylenic precursors of ??-damascenone were present at noticeable level in the glycosidic fraction.     

Profile of Volatile Compounds in 12 Chinese Soy Sauces Produced by a High‐Salt‐Diluted State Fermentation

There have been limited studies on the flavour compounds in Chinese soy sauces. In order to obtain wider information about the chemical composition of the volatile fractions in 12 brands of Chinese soy sauces produced by high‐salt‐diluted state fermentation (HSDSF) and to compare them, a headspace solid microextraction method coupled to gas chromatography‐mass spectrometry (HS‐SPME‐GC‐MS) method was proposed and developed. A 50/30μm Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) fibre was used for extraction of volatiles. The adsorption time and temperature of the SPME fibre were optimized separately for various aroma compounds in the soy sauce (50°C and 40 min for alcohols and esters; 40°C and 50 min for ketones, aldehydes and pyrazines; 60°C and 50 min for acids, phenols and furans). From the study, a total of 80 compounds were identified in the 12 samples, of which 34 volatiles were in common. Alcohols and acids were the main volatiles present in the soy sauces. Dominant volatile alcohols were ethanol, 2/3‐methyl butanol and β‐phenylethyl alcohol; and important acids were acetic acid, butanoic acid, and 3‐methylbutanoic acid. Miscellaneous, esters, furans and phenols also made large contributions to the total volatiles of the soy sauces. According to the scatter point plot obtained from principal component analysis, the 12 soy sauces could be classified into four groups.     

顶空固相微萃取气质联用测定蒜油挥发性成分

以蒜油挥发性成分的总峰面积及总峰面积与峰数的比值为评价指标,比较了不同萃取头、吸附温度、吸附时间及解吸时间对固相微萃取的萃取效率的影响,得到最佳萃取条件:85μmPA萃取头、吸附温度40℃、吸附时间35min、解吸时间3min,结果表明:固相微萃取技术有效地吸附了蒜油中的挥发性成分,经NIST质谱数据库检索和文献对照,共确定27种成分,并且不需溶剂,分析简单、快速、经济。     

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.     

Rapid Analysis of Flavor Volatiles in Apple Wine Using Headspace Solid‐Phase Microextraction

Flavor volatiles are important components of alcoholic beverages. In this study, headspace solid‐phase microextraction and gas chromatography—mass spectrometry (HS‐SPME‐GC‐MS) were investigated for the determination of flavor‐contributing volatiles for apple wine. HS‐SPME parameters were defined, including fiber coatings, extraction time, and extraction temperature. Good linearity, recoveries, and repeatability of the SPME method using carboxen‐polydimethylsiloxane (carboxen‐PDMS) fiber were obtained with r² values, recoveries, and relative standard deviations ranging from 0.9112 to 0.9960, 80.23% to 110.21%, and 1.5% to 6.4% respectively using standard solution. No significant effects of ethanol concentration on headspace concentrations of analytes were observed when ethanol concentration changed from 0% to 12% (v/v), indicating that the HS‐SPME‐GC‐MS method can be used for the determination of flavor volatiles in apple wine with an alcohol content below 12% (v/v) as well as in apple juice, and the method enables the monitoring of volatiles in mash during fermentation.     

Analytical comparison and sensory representativity of SAFE, SPME, and Purge and Trap extracts of volatile compounds from pea flour

Pisum sativum is of great economic and nutritional interest due to its protein content. Nevertheless, pea products are underused as a protein source in human food because of their strong beany flavour. Therefore, the objective of this study was to select an efficient and representative method to extract volatile molecules of pea flour. In the first step, three extraction methods were chosen: solid phase micro extraction (SPME); Purge and Trap extraction and solvent assisted flavour evaporation (SAFE). The corresponding extracts were analysed by gas chromatography coupled with mass spectrometry. In the second step, the sensory representativity of the extracts was assessed either by direct gas chromatography-olfactometry for SPME and for Purge and Trap extracts, or by sniffing for the aqueous SAFE extract. It appeared that SAFE extraction was the most suitable method because of its good extraction capacities and its high sensory representativity of the global odour of pea flour.     

顶空固相微萃取和同时蒸馏萃取法分析猪肉汤的挥发性成分

采用顶空固相微萃取法(HS-SPME)和同时蒸馏萃取法(SDE)提取清炖猪肉汤中挥发性成分,结合气相色谱-质谱联用技术(GC-MS)进行分析,结果共检测出77种挥发性化合物,其中烃类和醛类最多,均有22种,其次是醇类17种和酸类6种,另外酯类、酮类和杂环类分别有4、3、3种。HS-SPME法和SDE法分别鉴定出42种和49种挥发性组分。两种提取方法相比较,采用SPME法提取到醛类的种类明显多于SDE法,而烃类、醇类和酯类的种类明显少于SDE法。SDE法适合对高沸点、低挥发性物质的分离;SPME法具有快速简便、不使用溶剂和样品检测非破坏性等优点,适合易挥发性化合物的检出。只有将两种方法结合起来,才能得到对产品的挥发性物质的综合评价。