SPME及其与GC/MS联用在我国烟草分析中的应用进展

概述了固相微萃取技术的发展、基本原理、萃取条件和GC条件的选择以及固相微萃取与气相色谱/质谱联用在我国烟草分析中的应用进展。     

酿酒原料青稞中挥发性化合物的研究

建立了顶空-固相微萃取（HS-SPME）结合气相色谱-质谱联用技术（GC/MS）分析青稞中挥发性化合物的方法,采用这一方法对瓦蓝、肚里黄、白青稞、黑老鸭等四种青稞酒原料进行分析,分别获得28种、25种、24种和24种组分的定性结果,不同青稞品种间化合物种类接近又各具特点。这一研究拓展了固相微萃取技术在酿酒原料分析中的应...     

气相色谱-质谱联用分析砂梨及其果醋的香气成分

通过响应曲面法以固相微萃取对砂梨香气成分的萃取条件进行了优化,得出最优萃取条件为:选用PDMS/DVB(65μm)涂层纤维头,萃取温度46℃,萃取时间45min,盐添加量11%,样品量3.4g。以此萃取条件,运用HS-SPME结合GC/MS联用技术,对水晶梨及果醋的香气组分进行分析,鉴定出砂梨果实中的32种香气组分和果醋中的15种香气组分。     

食品风味物质分离技术研究进展

食品风味物质是构成食品特色的重要组成部分，也是区分不同食品的重要依据，综述了近年来发展的物质提取和分离技术，包括固相微萃取、超临界CO2高压萃取法、固相微萃取GC—MS及GC—Millimass分析技术、GC—Olfactometry检测技术、HPLC—MS联析、电子鼻检测技术。     

溶剂棒液相微萃取—气相色谱质谱—闻香法测定德州扒鸡风味成分

建立了溶剂棒液相微萃取技术与气相色谱—质谱仪联用,同时结合气相色谱嗅闻联用技术共同测定德州扒鸡风味成分的方法。在溶剂棒液相微萃取条件优化的基础上,确定了最佳实验条件:以正辛醇为萃取剂,萃取液体积3μL,萃取温度20℃,萃取时间15min,搅拌速度1000r/min。与固相微萃取—气相色谱—质谱法相比,溶剂棒液相微萃取法定性了34种成分,固相微萃取法定性了28种成分,其中共同鉴定组分20种,溶剂棒液相微萃取法操作简单快速,实验结果好,重复性好,可用于德州扒鸡中风味成分的分析。     

笃斯越橘果酱特征香气成分分析

以笃斯越橘果酱为研究对象,采用2种萃取方法结合气相色谱质谱联用技术同时辅以气相色谱嗅闻联用技术分离鉴定其香气成分。结果:液液萃取法鉴定出32种化合物,固相微萃取法鉴定出61种化合物,2种萃取方法检测出的香气化合物组分含量和种类存在差异,固相微萃取法更适合作为笃斯越橘果酱香气分析的萃取技术。根据固相微萃取果酱香气组分含量计算出各组分香气值,其中紫罗兰酮、(E,E)-2,4-壬二烯醛、正己醛、反-2-癸烯醛、苯乙醛等19种物质对笃斯越橘果酱香气有贡献,赋予产品花香、木香、脂肪味、水果香、坚果香、青草香、焦糖味等特征香气。结果表明,来源于果实的香气组分是构成笃斯越橘果酱典型风味的重要物质基础,应采用适度的热加工工艺以降低生产过程中该类组分的损失。     

固相微萃取条件优化及发酵菜粕风味物质分析

研究固相微萃取与气质联用研究发酵菜粕的风味物质及比较不同品种菜粕发酵前后风味物质的变化,以峰面积及峰数为指标,通过萃取头、萃取温度、吸附时间和样品量的优化,确定了固相微萃取和气质联用研究发酵菜粕风味固相微萃取的条件,并比较了3种代表性菜粕发酵前后风味物质及硫苷组分和含量的变化。结果表明,固相微萃取最佳条件是:50/30μm DVB/CAR/PDMS(DCP)萃取头,温度70℃,吸附30 min,样品量2 g,其中萃取头和吸附温度显著影响萃取效率。发酵前后菜粕的挥发性组分及含量变化都较大,发酵后风味物质的总量都显著增加,硫苷的含量明显降低,表明发酵不但显著增加了风味物质的含量改变了风味,而显著降低了抗营养物质硫苷的含量。     

固相微萃取在乳制品风味分析中的应用

固相微革取（SPME）是在固相萃取（SPE）的基础上发展起来的新型革取分离技术。它操作简单、并能最大限度体现样品真实风味等特点使其被广泛的应用于乳制品风味成分分析。本文介绍了固相微萃取技术的原理、装置、操作．论述了其在乳制品风味分析中工作备件选择厦优化措施，以及十年来固相微萃取技术与气相色谱（GC）、质谱（MS）、多变量统计分析（MVA）等现代分析仪器和分析技术联用在乳制品风味分析领域，包括乳制品挥发性风味成分分析、乳制品种类鉴定、乳制品质量评价及乳制品货架期预测等方面的应用．并对其未来发展进行了展望。     

固相微萃取-气相色谱-质谱法测定纺织品中多氯联苯含量

为了建立利用固相微萃取／气相色谱／质谱联用技术测定纺织品中26种多氯联苯组分的试验方法,研究了极性、非极性、双极性萃取头对多氯联苯的萃取效率以及萃取条件,包括萃取时间、萃取温度、溶液酸度、离子强度、解析时间和温度、GC—MS仪器条件,并选择了100μm聚二甲基硅氧烷（PDMS）萃取纤维头研究其检测的线性范围为0．1～200ng／L;试验结果表明,实际样品回收率在89．7％～96．8％之间。     

白酒酿造副产物黄水中挥发性化合物的研究

采用同时蒸馏萃取（SDE）和顶空-固相微萃取（HS-SPME）结合气相色谱-质谱联用技术（GC/MS）对黄水中挥发性组分进行了分析研究。采用HS-SPME和SDE方式分别获得41种和37种组分的定性结果,具有较好的一致性,并印证了发酵副产物黄水对成品酒风味形成的贡献。这些结果拓展了SPME和SDE技术在白酒分析研究中的应用,为白酒酿造过程的量化评价提供了有效手段。文中除列表分析结果外,还对SPME和SDE方法的特点、黄水中的定性组分与白酒香味组分的相关性作了研讨。     

固相微萃取与同时蒸馏萃取法分析香精成分比较

分别采用同时蒸馏萃取法与固相微萃取法对烟草香精中的香味成分进行萃取 ,再用气相色谱 /质谱联用法和气相色谱法进行了定性和定量 ,并对这 2种萃取方法鉴定出的化学成分、重复性和定量值进行了比较。结果显示 :同时蒸馏萃取法具有良好的重复性和较高的萃取量 ,适合于烟用香精香味成分的定量分析 ;固相微萃取法具有快速简便、不使用溶剂和样品检测非破坏性等优点 ,适合于香精的剖析定性。     

运用顶空固相微萃取技术分析宣威火腿中的挥发性化合物

采用固相微萃取结合气相色谱 /质谱分析方法对宣威火腿中的挥发性化合物进行了提取和分析。试验结果表明 ,固相微萃取的时间和温度影响提取挥发性化合物的效果 ,试验选取 60℃、60min为提取条件 ,萃取物经气谱 /质谱分析 ,共鉴定出 72种化合物 ,其中烃类 2 8种、醛类 7种、醇类 4种、酸类 10种、酯类 5种、酮类 3种、杂环化合物 14种、酚类 1种。     

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.     

Application of solid phase extraction techniques to analyse volatile compounds in wines and other enological products

Aroma compounds are most closely associated with the volatile fraction of foods. Common analytical separation procedures employed to analyse volatile compounds need, even today, that prior to GC analysis of an aroma or a fragrance, these compounds be concentrated or/and isolated from the non-volatile matrix. This step constitutes a problem that has still not been satisfactorily resolved and for this, several sample preparation methods can be found into the bibliography. This review gives a brief overview of solid phase extraction techniques to analyse volatiles. Procedures such as solid phase extraction (SPE), solid phase microextraction (SPME), stir bar sorptive extraction (SBSE), and the recent solid phase dynamic extraction (SPDE) will be discussed and critically evaluated. Contemporary applications of these techniques to the study of volatile compounds in wine and other enological products will be presented.     

Evaluation of four isolation techniques for honey aroma compounds

The analysis of the volatile fraction of honey provides useful information for the determination of the botanical and geographical origin. However, the results obtained vary greatly upon the extraction procedure employed. Four different isolation techniques were compared, that is hydrodistillation (HD), micro‐simultaneous steam distillation–solvent extraction (MSDE), ultrasound‐assisted extraction (USE) and solid‐phase microextraction (SPME). From the data obtained, USE and SPME seem to be more suitable for the isolation of potent marker compounds. HD and MSDE have main drawbacks because of the drastic conditions used that lead to the formation of artefacts and the degradation of sensitive compounds. These drawbacks are avoided when employing USE and SPME. Copyright © 2004 Society of Chemical Industry     

固相微萃取和气-质联用技术在快速测定苹果中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，它可进一步完成取样、萃取和浓缩，简化了传统前处理方法的烦琐步骤，而且不会造成二次污染。实验采用SPME技术和GC／S(气质联用仪)技术分析了苹果中的香气成分，色谱图中共鉴定出48个成分，占其香气成分的98％。     

Maillard模式反应牛肉香精挥发性风味成分分析

应用同时蒸馏萃取（SDE）和固相微萃取（SPME）两种预处理方法，GC-MS分析Maillard模式反应牛肉香精的挥发性风味成分，共分离鉴定出87种挥发性化合物，其中2-甲基-3-呋喃硫醇、四氢-2-甲基-3（2H）-呋喃酮、双二（2-甲基-3-呋喃基）二硫醚、3-甲基-2-乙酰基噻吩等为特征型牛肉香味化合物。两种提取方法互为补充，较为全面的反映了牛肉香精的风味轮廓组成。     

Application of response surface design to optimise the chromatographic analysis of volatile compounds in beer

Solid‐phase microextraction (SPME) combined with gas chromatography and mass spectrometry (GC–MS) is a rapid method for the analysis of different aromatic compounds in beer. However, chromatographic systems are affected by different parameters and optimization is time‐consuming process, but essential for establishing optimal conditions for the quantification of analytes. An automated system consisting of headspace (HS)–SPME extraction combined with GC–MS was optimized for the determination of 19 volatile compounds responsible for important flavours and off‐flavours of beer. The optimisation process consisted of two steps: the SPME fibre type was chosen, and subsequently four extraction parameters (temperature, time, sodium chloride concentration and pH) were optimised by a central composite design model. After optimisation, standard compounds were validated with relative standard deviations not exceeding 15%_rel. The square of correlation coefficient for the calibration curves was ≥0.9559, indicating a linear response and the suitability of these HS‐SPME conditions. Copyright © 2018 The Institute of Brewing & Distilling