酿清谷酱香型白酒香气成分的分析及对比

该研究利用顶空固相微萃取（HS-SPME）,结合气相色谱-质谱联用（GC-MS）技术对酿清谷酱香型白酒中香气成分进行检测,对萃取条件进行优化,并与茅台、茅台王子、北大仓和徐朝正品牌酱香型白酒香气成分进行了对比分析。结果表明,最佳萃取条件为顶空固相微萃取时间30 min,萃取温度50 ℃,解吸时间5 min。GC-MS结果表明,从酿清谷酱香型白酒中共鉴定出55种挥发性物质,包括33种酯类、9种酸类、5种醇类、4种酮类、2种醛类、1种烯类和1种苯类,结合气味活度值（OAV）,确定出15种具有香味贡献的主要成分。酿清谷酱香型白酒与四种品牌酱香型白酒香气成分对比有明显差异,主要缺少丁酸乙酯、己酸异戊酯和正戊醇等香气成分。     

顶空固相微萃取-气相色谱-质谱联用法分析黄茶香气成分

建立黄茶香气的分析方法,探讨固相微萃取技术在黄茶香精油制备上的应用,研究固相微萃取头种类、温度、吸附和解吸时间对黄茶香气物质种类和总量的影响。结果表明：采用DVB-CAR-PDMS 固相微萃取头,在80℃下吸附1h,能达到最佳吸附效果;吸附的香气物质在GC-MS 进样口内经230℃热脱附1min,共检测出108 种黄茶香气成分,其物质种类由高到低依次为烃类32 种、酯类20 种、醇和醛类各17 种、酮类8 种、含氧和含氮化合物各4 种、酸类3 种、含硫化合物2 种、酚类1 种;其含量以脂肪族烃、醛类较多,而萜烯类以及芳香族化合物较少。     

HS-SPME-GC-MS analysis of volatile aromatic compounds in alcohol related beverages made with mulberry fruits

Wine aroma is one of the most important parameters responsible for its quality, and hence for consumer acceptance. In order to obtain an appropriate technique to study volatile aroma compounds in mulberry wines, headspace-solid phase microextraction (HS-SPME) comb 40°C for 30 min with a 50/30 μm divinylbenzenecarboxen-polydimethylsiloxane (DVB-CAR-PDMS) fiber. Approximately 80 volatile compounds have been quantified in the mulberry wine, pertaining at several chemical groups, mainly higher alcohols, fatty acids, esters, and some volatile phenols whose concentration range from few to 138.36 mg/L. This work describes a novel methodology for the analysis of mulberry wines by HS-SPME coupled to GC-MS. HS-SPME using a 50/30 μm DVB-CAR-PDMS fiber is provided the higher extraction efficiency (p<0.05) for the volatiles including the most esters, higher alcohols, and fatty acids than by the other fibers.     

响应面法优化固相微萃取生板栗香气成分条件

利用响应面法研究不同萃取参数对生板栗香气成分萃取效果的影响。分别优化固相微萃取的萃取纤维头、萃取温度、平衡时间、萃取时间等因素,测定其对生板栗香气成分的种类、总峰面积的影响。结果表明,最佳萃取条件为65 μm聚二甲基硅烷/二乙烯苯（PDMS/DVB）萃取头、平衡时间18 min、萃取时间50 min、萃取温度58.5 ℃,在此优化条件下经气质联用法检测出生板栗香气成分21种,总峰面积48 382.7。其中醛类占14.40%、醇类占7.06%、酮类占7.72%、酯类占52.97%。     

SPME-GC-MS分离鉴定山核桃的挥发性风味物质

采用顶空固相微萃取方法提取山核桃成品的挥发性风味物质,利用气相色谱-质谱联用技术对提取的挥发性风味物质进行分离鉴定。通过正交试验确定了固相微萃取的最佳萃取条件:使用65μm PDMS-DVD萃取头,萃取温度60℃,萃取时间30 min。采用气质联用技术从山核桃中分析鉴定出33种挥发性风味物质成分,包括杂环类化合物、萜烯类、醛类、酸类、醇类、酯类和酮类,这些物质成分的共同作用构成了山核桃独特的风味。其中杂环类化合物、萜烯类化合物和醛化合物类含量较高,是对山核桃整体风味起关键作用的挥发性风味物质。     

In-needle Microextraction Coupled with Gas Chromatography/Mass Spectrometry for the Analysis of Phthalates Generating from Food Containers

In this study, we fabricated a new device for headspace in-needle microextraction using a stainless steel wire coated with multiwalled carbon nanotube/polyaniline composite by coulometric technique. Then, the coated wire was placed into a stainless steel needle inside. This headspace in-needle microextraction device was applied for the determination of phthalates dissolved in aqueous solution by gas chromatography-mass spectrometry. Multiwalled carbon nanotube/polyaniline composite film of 10 mm length on the surface of stainless steel wire was optimized to polymerize electrochemically when constant potential of 2.0 V was applied during 500 s. Atomic force microscopy and Auger electron spectroscopy showed that polymerization on the surface of wire had smooth, homogeneous, and constant coating thickness of 1.5?±?0.004 μm. The optimum molar ratio of multiwalled carbon nanotube and aniline (C:N) for polymerization was determined at 1: 2 M ratio. The optimum conditions of the proposed method were extraction temperature 50 °C, saturation time 60 min, extraction time 30 min, desorption temperature 230 °C, and desorption time 3 min, respectively. Validation of headspace in-needle microextraction-multiwalled carbon nanotube/polyaniline coupled with GC/MS was also performed including limit of detection, limit of quantitation, dynamic range, recovery, and reproducibility. The proposed device is found to be inexpensive, easy, and rapid to fabricate and could be utilized effectively as the solventless microextraction method for the analysis of phthalates generating from food containers.     

Quantitative Profiling of Volatile and Phenolic Substances in the Wine Vernaccia di Serrapetrona by Development of an HS-SPME-GC-FID/MS Method and HPLC-MS

A headspace solid-phase microextraction coupled to gas chromatography with mass spectrometry and flame ionization detection (HS-SPME-GC-MS/FID) method has been developed for quantifying the main volatiles of the Italian sparkling red wine Vernaccia di Serrapetrona, leading to establish that the divinylbenzene/carboxen/polydimethylsiloxane-coated (gray) fiber, an equilibration time of 15 min, and an extraction time of 15 min at a temperature of 35 °C are the conditions representing the best compromise in terms of sensitivity and time expense, to carry out the analyses. Among the volatiles quantified, 2-phenylethanol, 3-methylbutyl acetate, and ethyl esters levels resulted to be above their odor thresholds, thus being probably responsible for the aroma of this wine with their positive attributes. Phenolic compounds, namely gallic acid, p-coumaric acid, caffeic acid, (+)-catechin, and (+)-epicatechin, were also quantified using high-performance liquid chromatography-MS, thus obtaining an overall characterization of molecules fundamental for both the sensory and the healthy characteristics of the wine. The total phenolic content was found to be in the range of 19.25–61.67 mg l^?1 with the most abundant compound being gallic acid (7.44–25.78 mg l^?1). Main differences in volatile and phenolic compounds between samples were discussed and analyzed by chemometric techniques as principal component analysis.     

顶空固相微萃取-气相色谱-质谱联用分析库尔勒香梨花序香气成分

建立库尔勒香梨花序香气成分的顶空固相微萃取-气相色谱-质谱定性定量方法。花序样品分别经固相微萃取PDMS、CAR/PDMS萃取头富集,经气相色谱梯级升温分离后,进入电子电离源单级扫描质谱,经质谱图库检索定性、归一化法定量。结果表明:2个萃取头最佳富集香气的条件为梨花样品量4 g、萃取温度40℃、萃取时间25 min,检测出不同花期共69种挥发性香气成分,其中包括酯类、醇类、油酸类和含杂原子化合物等。方法前处理简单、重复性好、分析时间短,能适用于梨花香气成分的测定。     

Volatile Constituents of Jambolan (<Emphasis Type="Italic">Syzygium cumini</Emphasis> L.) Fruits at Three Maturation Stages and Optimization of HS-SPME GC-MS Method Using a Central Composite Design

The volatile compounds of jambolan (Syzygium cumini L.) fruit were determined at three different maturity stages (unripe, half-ripe, and ripe) by headspace solid-phase microextraction (HS-SPME)–gas chromatography-mass spectrometry (GC-MS) technique using five different fibers (Fused silica PDMS/DVB, DVB/CAR/PDMS, PEG, Stable flex PDMS/DVB, and PDMS). The optimal extraction conditions were evaluated using different variables such as adsorption temperature (minimum 25 °C, maximum 55 °C), salt quantity (minimum 0, maximum 30.0%), and extraction time (min 10, max 30 min). The major classes of compounds identified were ester, terpene, alcohol, aldehyde, and carboxylic acid. Ninety volatile compounds with characteristics aroma attributes were identified, and the primary compounds linked with development of characteristics aroma of ripe jambolan fruit pulp were trans-β-ocimene, β-ocimene, caryophyllene, humulene, D-α-pinene, L-β-pinene, β-pinene, D-limonene, α-terpineol, neo-allo-ocimene, 2-hexenal (E), δ-cadinene, 3-hexen-1-ol, (Z) β-linalool, terpinolene, eremophilene, valencene, 1-hexanol, longipinene, γ-terpinene, γ-muurolene, endo-borneol, o-cymene, nonanal, terpinen-4-ol, β-terpineol, α-muurolene, fenchol, α-fenchene, β-thujene, benzaldehyde, (E)-2-hexenal, β-cadinene, and decanal.     

HS-SPME-GC-MS分析红提葡萄白兰地挥发性风味化合物

以新疆产区红提葡萄白兰地为研究对象,采用顶空固相微萃取（HS-SPME）优化其萃取条件,结合气相色谱-质谱（GC-MS）联用技术对其挥发性风味化合物进行定性定量分析,并采用气味活度值（OAV）判断其挥发性成分对白兰地整体香气的贡献度。结果表明,最佳萃取条件为：萃取头二乙烯基苯-羰基-聚二甲基硅氧烷（DVB-CAR-PDMS）50/30 μm,萃取温度40 ℃,萃取时间40 min。在该萃取条件下,共检出62种挥发性化合物,其中酯类、醇类、酸类、醛酮类、缩醛类、萜烯类和其他类物质分别有21种、13种、8种、9种、3种、5种、3种,其相对含量分别为51.19%、6.90%、12.94%、5.76%、3.28%、0.51%和19.42%。通过OAV评价得出具有香气贡献的主要化合物（OAV＞1）共10种,以酯类、醛类和酸类为主。     

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.     

HS-SPME-GC-MS分析西林火姜挥发性香气成分

以西林火姜干姜片为原料,通过顶空固相微萃取(headspace solid phase micro-extraction,HS-SPME)结合气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)对萃取头种类、萃取时间和解析时间进行单因素优化,研究其挥发性香气成分。结果表明:3 g西林火姜干姜粉采用100μm PDMS萃取头,萃取40 min,解析3 min萃取挥发性香气成分效果最佳。在此条件下检测到干姜45种香气成分,含量最高的是萜烃类,也有少量酯、酮、醛和醇等。主要的香气成分为姜烯、β-倍半水芹烯、(E,E)-α-法呢烯、β-红没药烯、α-姜黄烯、β-荜澄茄油烯、2-茨醇、α-柠檬醛、β-榄香烯。     

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.     

Determination of Vanillin and Ethyl-Vanillin in Milk Powder by Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

A method for determination of vanillin and ethyl-vanillin in milk powder by auto headspace solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was established. Vanillins in sample were extracted with SPME through a fused-silica fiber coated with divinylbenzene/polydimethylsiloxane. The analytes were desorbed by GC at 260 °C for 5 min and separated on a DB-5MS capillary column and detected by MS with EI source by selected ion monitoring mode (EI-SIM). As a result, the limit of detection of vanillin and ethyl-vanillin was 0.1 and 0.05 mg/kg. The spiked recovery was between 90.0 and 100 %, and the RSD ranged from 1.9 to 5.1 % (n?=?6). This method eliminated the interferences from complicated matrix effectively. The method was successfully applied for quick determination of vanillin and ethyl-vanillin content in milk powder samples.     

SPME-GC-MS分析与鉴别青海亚麻籽油挥发性组分

以青海不同产地的40种亚麻籽为原料,索氏抽提提取亚麻籽油,采用顶空固相微萃取结合气相色谱-质谱联用对亚麻籽油挥发性组分进行分析,通过优化搅拌速率、萃取温度、平衡时间、萃取时间、解吸时间、升温程序确定最佳固相微萃取条件及GC-MS条件。结果表明,采用DVB/CAR/PDMS萃取头,亚麻籽油SPME最佳条件为磁力搅拌速率400 r/min,萃取温度80 ℃,平衡时间20 min,萃取时间40 min,解吸时间5 min,在该萃取条件下可以检测出青海40种亚麻籽油挥发性成分共58种,醛类12种,酸类8种,醇类9种,酮类2种,酯类5种,烷烯类13种,杂环类3种,其他类6种,分离鉴定效果较好;根据聚类分析,醛类物质是将亚麻籽油样品进行区分的主要挥发性组分,该结果为亚麻籽油品质鉴定及开发利用提供了理论依据。     

Effect of the Variables Time and Temperature on Volatile Compounds Extraction of Salami by Solid Phase Microextraction

The aim of this study was to determine the experimental conditions for extracting volatile compounds present in the headspace of a salami sample by solid phase microextraction (Carboxen/PDMS fiber), monitoring the individual aromas of the extracts directly in order to maintain the original aroma of the product. Additionally, extracts were analyzed in gas chromatograph equipped with flame ionization detector and mass spectrometer (GC-FID and GC/MS). Volatile compounds were separated in polar phase capillary column (DB-Wax). Response Surface Methodology was used to explain the effects of both time and temperature on the salami aroma and on the instrumental measurements. Trained judges analyzed the intensity of a characteristic aroma from 12 salami extracts directly in olfactometer coupled with a gas chromatograph. The sensory results generated a multivariate statistical model (R ² = 0.72, p < 0.05) that included linear time and temperature terms. The optimal conditions were determined to be an extraction period of 45 min at 50 °C, as the resulting extract received a mean sensory score of 7.15. This method allowed us to obtain a highly representative aroma of the product in an adequate time.     

HS-SPME/GC-MS测定石榴酒中香气组分的条件优化

该文使用气相质谱联用仪(gas chromatography-mass spectrometry,GC-MS)对石榴酒中的香气成分分析,在进样前对萃取纤维的种类,萃取的样品量,萃取时间,萃取温度4个条件进行优化,以期得到所测定的香气分子较多,重现性较好的GC-MS结果。试验结果表明对5.0 mL石榴酒样品,选取二乙烯基苯/碳分子筛/聚二甲基硅氧烷(divinylbenzene/carbon molecular sieve/dimethicone,DVB/CAR/PDMS)萃取纤维在45.0℃下萃取50 min,能够得到最优且重现性较好的GC-MS分析结果,定性出57种化合物,包括酯类、醇类、酸类、芳香族化合物等。为石榴酒的后续研究提供了基础。     

骏枣精油的超临界CO2萃取工艺及其组成分析

以新疆骏枣为原料,采用超临界二氧化碳萃取技术对骏枣精油进行萃取分离,通过单因素和正交试验优化骏枣精油的萃取工艺,最后采用顶空-固相微萃取(headspace solid phase microextraction,HS-SPME)和气相色谱-质谱联用仪(gas chromatography-mass spectrometry,GC-MS)对骏枣精油成分进行分析。结果表明:超临界二氧化碳萃取骏枣精油最佳工艺为:乙醇作携带剂,萃取压力25 MPa,萃取温度32℃,夹带剂流速0.3 mL/min,萃取时间3 h,骏枣精油的萃取率可达1.224%。经GC-MS分析,共检出68种物质,结构推断59种,占总峰面积的91.737%,其中主要包括酸类、烷烃类、酮类、酯类以及少量的醛类、醇类等。各类物质中焦糖香味的麦芽醇和5-羟甲基糠醛,杏仁气味苯甲酸和糠醛以及奶香味的3-羟基-2-丁酮都可能是骏枣精油的主要香气成分。     

基于直接-气相色谱-嗅闻的整体感官评价模式分析泸香型白酒的关键香气成分

采用顶空固相微萃取(HS-SPME)结合直接-气相色谱-嗅闻(D-GC-O)的方法对泸香型白酒挥发性风味成分进行研究,同时对比静态顶空(SHS)法,从香气成分检测和整体风味角度考察了最优萃取条件,并对泸香型白酒的关键香气成分进行分析。结果显示:最佳萃取方法为HS-SPME:75 μm CAR/PDMS萃取头、萃取温度45℃、平衡时间15 min、萃取时间40 min、加盐量3 g;在此条件下对泸型酒中77种香气成分定量分析,采用GC-O-MS嗅闻鉴定出46种呈香物质,包括酯类22种,醇类7种,酸类4种,芳香类7种,呋喃醛酮类5种,含硫类1种。由香气强度值和香气活性值(OAV)分析共同确定了泸型酒中18种关键香气成分,主要呈现花香、果香、甜香、酸味、青草香、醇香、窖香等。本研究将整体风味作为优选萃取条件的判定依据,在仪器检测风味物质的基础上进一步提供感官数据支撑,保障了最优条件的可信度,所确定的关键香气成分能够较好地代表泸型酒的风格特征。