HS-SPME coupled to GC/MS for quality control of Juniperus communis L. berries used for gin aromatization

HS-SPME coupled to GC/MS was applied to the analysis of the volatile fraction of Juniperus communis L. berries, which are the principal ingredient used for gin aromatization. Seventy seven compounds were identified by comparison with reference compounds or tentatively identified by comparing their mass spectra and retention index with those reported in mass spectra libraries and literature, respectively. Seventy four were detected by SPME and sixty eight were detected by solvent distillation extraction (SDE). These were mainly mono- and sesquiterpenic compounds that represented more than the 80% of the gin’s volatile composition. A high percent content was due to monoterpenoids, whose analysis could be important for the assessment of sensory quality control of juniper due to their impact on gin aroma. The main monoterpenoids detected in the headspace of the juniper berries from two periods of collection were terpinen-4-ol, p-cymene, β-myrcene, γ-terpinene, α-pinene and limonene. These represented more than the 70% of the sample’s volatile fraction. The proposed SPME method required short times and the low cost of analysis and enabled to detect a number of compounds comparable with SDE or much higher than the number of compounds reported by other extraction techniques. The results suggested the suitability of this technique for the assessment of the volatile composition of juniper berries intended for gin flavouring.     

Extraction of volatile organic compounds from leaves of Ambrosia artemisiifolia L. and Artemisia annua L. by headspace-solid phase micro extraction and simultaneous distillation extraction and analysis by gas chromatography/mass spectrometry

This study was designed to analyze the volatile organic compounds in the leaves of Ambrosia artemisiifolia L. and Artemisia annua L. from Korea. For extraction of volatile compounds, headspace-solid phase micro extraction (HS-SPME) and simultaneous distillation extraction (SDE) were applied and analyzed by gas chromatography/mass spectrometry (GC/MS). From the results, SDE extraction was found to give the highest concentration of volatile compounds with an average concentration of 1,237.79 mg/kg for A. annua L. leaves compared to 1,122.73 mg/kg by HS-SPME technique. A total of 116 volatile organic compounds were identified, including 76 similar volatile organic compounds detected by both the methods of extraction in leaves of subject species at varying concentrations. Among these 33 volatile organic compounds were reported for the first time from the subject plant species. Thus the present research findings extend the characterization of volatile organic compounds from leaves of A. annua L. and A. artemisiifolia L. species and reported some distinguishing compounds which may be used for their discrimination.     

Analysis and characterization of aroma‐active compounds of Schizandra chinensis (omija) leaves

Volatile components from leaves of Schizandra chinensis (omija), a native plant of Korea, were extracted by simultaneous distillation–extraction (SDE) and analyzed by gas chromatography–mass spectrometry (GC‐MS) using two types of capillary column with different polarities (DB‐5MS and DB‐Wax). The GC‐MS analysis of volatile compounds obtained by SDE revealed that germacrene D is the most abundant compound (22.6%) in omija leaves, followed by β‐elemene (17.4%), (E)‐2‐hexenal (8.7%), and (E)‐β‐ocimene (7.2%). Aroma‐active compounds were determined by gas chromatography–olfactometry (GC‐O) using the aroma‐extract‐dilution analysis method. (E,Z)‐2,6‐Nonadienal (cucumber) was the most intense aroma‐active compound due to its higher flavor‐dilution factor (243–729) than any other compound. (Z)‐3‐Hexenal (green/apple), (E)‐2‐hexenal (green/fruity), and (E)‐β‐ocimene (wither green/grass) were also identified as important aroma‐active compounds by GC‐O. In addition, the volatile compounds were extracted by solid‐phase microextraction (SPME), and the quantitative analysis of the SPME samples gave slightly different results, depending on the type of SPME fiber, compared with those from SDE, However, the aroma‐active compounds identified in SPME were similar to those in SDE. Copyright © 2004 Society of Chemical Industry     

SDE和HS-SPME法与GC-MS/O联用分析阳江豆豉的香气活性化合物

采用同时蒸馏萃取法(SDE)和顶空-固相微萃取法(HS-SPME)结合气相色谱-质谱/嗅闻检测技术(GC-MS/O)深入研究阳江豆豉的香气成分,共鉴定出挥发性化合物174种。SDE法对高分子量、低挥发性物质,如呋喃酮、吡喃酮等,有良好的萃取效果;而HS-SPME法能萃取更多的高挥发性化合物,如小分子的酸和酯类。通过GC-O技术在两种方法的萃取物中共嗅闻到46个香气活性区域。其中9种共有化合物(2/3-甲基丁醛、2/3-甲基丁酸、3-甲硫基丙醛、苯乙醛、愈创木酚、3-羟基-2-甲基-4H-吡喃-4-酮和苯乙醇),以及香气强度较高(评分大于2.5分)的单方法检出化合物:SDE法4种(3-羟基-4,5-二甲基-2(5H)-呋喃酮、2-乙酰基-1-吡咯啉、2-丙烯基-3-甲基吡嗪和4-羟基-2,5-二甲基-3(2H)-呋喃酮)、SPME法1种(1-辛烯-3-醇),是阳江豆豉中的关键香气活性物质,对麦芽香、酸奶酪香、烤土豆香、花香、烟熏香、焦糖香和烤香等有贡献。     

Comparative study of different extraction techniques for the analysis of virgin olive oil aroma

Headspace solid-phase microextraction (HS-SPME), simultaneous distillation/extraction (SDE) and closed-loop stripping analysis (CLSA) coupled to gas chromatography/mass spectrometry (GC/MS) were used to study virgin olive oil, with the goal of detecting large numbers of characteristic volatile and semi-volatile compounds. More than one hundred compounds were detected in the olive oil extracts, and their percent amounts obtained by each technique were calculated. Qualitative and quantitative differences of virgin olive oil volatile profiles were observed applying the three extraction techniques. SPME showed a higher affinity for alcohols and ketones, while CLSA achieved the highest percentages of esters and hydrocarbons. Finally, the highest extraction of total terpenoid compounds occurred with SDE and CLSA, where CLSA allowed extracting the highest percentages of the most of them. SDE extraction caused the thermal degradation of the oil sample, which resulted in a high percentage of aldehydic compounds.     

金华火腿挥发性风味物质

采用同时蒸馏提取(SDE)法和顶空固相微萃取(HS SPME)法制备样品,利用 GC MS分离,鉴定了金华火腿的挥发性风味物质. 比较了两种样品制备方法的优劣,鉴定了金华火腿中 143种挥发性风味组分,并分析了风味成分的生成途径.在 SDE的结果中,最丰富的是醛类化合物,出峰面积相对比例为48%,其次是酸类23 45%,酮类 8 52%;在 SPME结果中,出峰面积相对比例较高的是醇、酸和醛类化合物,分别为26 8%、25 84%和 19 83%.两种方法得到的结果差异是由于处理过程的不同造成的,SDE中有2 h的高温蒸煮过程,因而其结果可以表征熟火腿的香气成分;而SPME则直接吸附萃取香气成分,未使香气成分发生变化,因而可以表征生火腿的香气成分,两种方法在研究金华火腿的挥发性风味物质方面可相互补充.     

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.     

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.     

顶空固相微萃取和同时蒸馏萃取应用于GC-MS分析野生刺梨汁挥发性成分的比较研究

采用顶空固相微萃取法(head-space solid phase micro-extraction,HS-SPME)和同时蒸馏萃取法(simultaneous distillation extraction,SDE)提取野生刺梨汁中挥发性成分,经气相色谱-质谱联用仪分析,结果共检测出52种挥发性化合物,其中烃类最多,有17种,其次是酯类12种和醇类7种,另外酸类、酚类、酮类、醛类和杂环类分别有5、3、3、3、2种。HS-SPME法和SDE法分别鉴定出37种和19种挥发性组分。两种提取方法相比较,HS-SPME具有快速简便、不使用溶剂、检测组分丰富和样品检测非破坏性等优点,更适宜于野生刺梨汁挥发性成分的分析。     

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。     

不同方法提取艾纳香叶挥发性成分的气相色谱-质谱分析

采用气相色谱-质谱法(GC-MS)分析水蒸汽蒸馏法(SD)、同时蒸馏萃取法(SDE)和顶空固相微萃取法(HS-SPME)3种方法提取的艾纳香叶挥发性成分。结果表明:3种方法提取艾纳香叶挥发性成分中主要是醇类和烯类化合物,其中萜类物质占较大比例。3种方法的提取物中分别鉴定出化合物50种(SD)、24种(SDE)和49种(HS-SPME)。水蒸汽蒸馏法和同时蒸馏萃取法提取的油状挥发物中主要成分相似,水蒸汽蒸馏法提取油状挥发物与顶空固相微萃取法提取挥发性成分的种类和相对含量相似,同时蒸馏萃取法提取油状挥发物中低沸点化合物较少。     

Effect of heat treatments on the essential oils of kumquat (Fortunella margarita Swingle)

Kumquats (Fortunella margarita Swingle) cultivated in Taiwan are eaten raw or made into candied fruit or fruit tea. For the experiments described in this paper, essential oils were obtained from kumquat peels or whole fruit by cold pressing, steam distillation or heating in water at 90 °C for 15 min followed by steam distillation. The volatile components contained in the essential oils were identified by direct injection (DI) or headspace-solid phase microextraction (HS-SPME) coupled with gas chromatography (GC). A total of 43 compounds were identified, of which 37 were verified by DI/GC and 31 by HS-SPME/GC. Hot water heating increased the yields of essential oils from both peels and whole fruit. The principal constituents of the oils were similar except for the minor compounds, including linalool, terpinen-4-ol and α-terpineol, the levels of which increased after steam distillation. The whole fruit also contained higher levels of terpene alcohols.     

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。     

同时蒸馏萃取与顶空固相微萃取法分析豆豉挥发性成分

采用同时蒸馏萃取法(SDE)和顶空固相微萃取法(HS-SPME)提取豆豉样品中挥发性成分,经气相色谱-质谱联用仪分析后共检测到96种挥发性化合物,其中烃类最多有40种,其次是酯类13种和醛类11种,另外醇类、酸类、酮类、酚类和杂环类分别有9、7、6、7、3种。SDE法和HS-SPME法分别鉴定出60种和43种风味组分,比较两种提取挥发性成分的方法可知,SDE法具有较高的萃取量,适合对高沸点、低挥发性的物质的分离;HS-SPME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。     

Comparison of simultaneous distillation extraction (SDE) and solid‐phase microextraction (SPME) for the analysis of volatile compounds in dry‐cured ham

Simultaneous distillation extraction (SDE) and solid‐phase microextraction (SPME) using a carboxen/polydimethylsiloxane fibre were compared for their effectiveness in the extraction of volatile compounds from dry‐cured ham samples. A higher number of compounds was detected using SPME owing to the use of a solvent delay time in the GC‐MS analysis of SDE extracts. SPME was more efficient in extracting low molecular weight and high volatility compounds, while SDE was able to extract compounds with low volatilities that were not extracted using SPME. Both techniques satisfactorily extracted most volatiles previously highlighted as odour‐active compounds in dry‐cured ham. However, the ratio between some compounds from lipid oxidation and those from degradation of amino acids was much lower in SDE extracts than with SPME, which could be a consequence of the development of Strecker degradation of amino acids during distillation in SDE owing to the high temperatures used. Similarly, diunsaturated aldehydes detected in SDE extracts were absent using SPME, probably owing to oxidation of polyunsaturated fatty acids in SDE as a consequence of the temperature during extraction. Copyright © 2004 Society of Chemical Industry     

顶空-固相微萃取与气质联用法分析草菇中的香味成分

本文以享有“中国蘑菇”之称的草菇为原料，采用碳分子筛-聚二甲基硅氧烷（CAR／PDMS）涂层的固相微萃取头分别萃取新鲜草菇和干草菇蒸馏后的挥发性成分，并通过气质联用仪分析鉴定了其主要的香味成分。结果表明，固相微萃取有效地吸附了草菇中的挥发性成分，经NIST质谱数据库和文献对照，分别从干草菇和新鲜草菇中检测出48和29种成分，其中八碳化合物是最要的风味主体。     

Optimization of equilibrium headspace analysis of volatile flavor compounds of malaysian soursop (Annona muricata): Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS)

Headspace solid-phase microextraction (HS-SPME) coupled to comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) was applied for equilibrium headspace analysis of Malaysian soursop (Annona muricata) volatile flavor compounds. A two-level fractional factorial design (2^5-1) was used to determine the effect of SPME variables, namely, SPME fibers, adsorption temperature, extraction time, amount of salt, sample amount and sample concentration on the extraction efficiency of volatile flavor compounds. A total of 37 volatile compounds were identified, comprising 21 esters, 6 alcohols, 3 terpenes, 2 acids, 2 ketones, 2 aldehydes and an aromatic with different hydrophobicities (log P) ranging between −0.14 and 4.83. Extraction using 10 g of diluted (5% w/w) blended soursop pulp with CAR/PDMS fiber at 25 °C for 30 min and 30% (w/w) of NaCl under stirring mode resulted in the highest extraction efficiency of volatile flavor compounds. The principal component analysis score discriminated the influence of SPME variables on the equilibrium headspace concentration of target volatile compounds.     

Characterization of aroma potential of apricot varieties using different extraction techniques

Aroma compounds are presents in raw foods, freely and glycosidically-bounded (aroma precursors). In the present work, the volatile fraction of eight varieties of apricot were analyzed using simultaneous distillation extraction (SDE), solid phase extraction (SPE) with reverse phase (C18), liquid–liquid extraction (LLE) and headspace-solid phase microextraction (HS-SPME). The free aroma compounds were identified by GC–MS, finding common compounds such as linalool, α-terpineol, β-ionone and γ-decalactone and specific compounds due to the extraction method used. The ANOVA showed a significant effect in the extraction techniques and on the varieties in the free aromatic fraction from apricot as well. In spite of a large number of volatile compounds extracted by SPE, the technique that allowed for the most number of compounds to be extracted was SPME.     

Identification of volatile components in Chinese Sinkiang fermented camel milk using SAFE,SDE, and HS-SPME-GC/MS

The volatile components of Chinese Sinkiang fermented camel milk were isolated by solvent assisted flavour evaporation (SAFE), simultaneous distillation extraction (SDE, dichloromethane and diethyl ether as solvent, respectively) and headspace solid-phase microextraction (HS-SPME, CAR/PDMS, PDMS/DVB and DVB/CAR/PDMS fibre extraction, respectively) and analysed by GC/MS. A total of 133 volatile components were identified under 6 different conditions, including 30 esters, 20 acids, 18 saturated alcohols, 15 unsaturated aliphatic alcohols, 8 saturated ketones, 9 saturated aldehydes, 8 unsaturated aliphatic aldehydes, 6 furans, 5 sulphur-containing compounds, 5 ethers, 5 lactones, 3 other compounds, and 1 unsaturated aliphatic ketone. Three pretreatment methods were compared, assisted by principal component analysis (PCA). The results indicated that the volatile components obtained using different methods varied greatly both in categories and in content, and therefore, a multi-pretreatment method should be adopted together with GC/MS. A total of 71 aroma-active compounds were detected by gas chromatography-olfactometry (GC–O), among which 66 aroma-active compounds were found by SDE (60, dichloromethane as solvent; 24, diethyl ether as solvent), 26 by SAFE.