武陵青花椒壳挥发油成分及脂肪酸分析

分别采用水蒸气蒸馏法和同时蒸馏萃取法提取武陵青花椒壳中的挥发油成分,提取率分别为6.4%和8.5%。再用气相色谱-质谱法(GC-MS)对挥发油成分进行分析,用峰面积归一化法确定各组分的相对含量。两种方法均鉴定出43种化合物,其中水蒸气蒸馏法以β-芳樟醇(66.91%)、反式-橙花叔醇(6.28%)、D-柠檬烯(5.24%)、4-萜烯醇(2.6%)为主,同时蒸馏萃取法以β-芳樟醇(64.32%)、D-柠檬烯(5.97%)、反式-橙花叔醇(4.17%)、反式-9-十八烯酸(3.09%)为主。同时对挥发油进行甲酯化,然后用GC-MS对挥发油中含有的脂肪酸进行了分析,共分离鉴定出6种脂肪酸。结果表明:两种方法提取的挥发油的组成及含量存在差异,挥发油中主要为不饱和脂肪酸。水蒸气蒸馏法对无极性和弱极性的萜烯和萜醇类化合物提取效果较好,而同时蒸馏萃取法适于各种极性化合物,对极性稍强的脂肪酸和酯类有较好的提取效果。     

两种方法提取太行山地区花椒中挥发性化学成分的气相色谱-质谱分析

采用同时蒸馏萃取法和普通水蒸汽蒸馏萃取法,对产自太行山地区的花椒中的挥发油进行提取,测得花椒挥发油含量分别为12.5%、8.9%;并用汽相色谱-质谱联用技术进行分析鉴定,结合计算机质谱图库检索技术对分离的化合物进行结构分析,分别鉴定出45种(同时蒸馏萃取法)和26种(普通水蒸汽蒸馏萃取法)化学组分,分别占总挥发性物质总含量的94.68%和93.98%。应用峰面积归一化法确定了各成分的相对含量。结果表明:同时蒸馏萃取法提取的挥发油中主要含有苎烯(24.75%)、桉叶油素(8.91%)、β-蒎烯(7.81%)等,普通水蒸汽蒸馏萃取法提取的挥发油中主要含有桉叶油素(41.19%)、(+)-α-松油醇(12.25%)等。     

同时蒸馏萃取法和固相微萃取法分析棕榈油与菜籽油复合火锅底料中的风味物质

采用同时蒸馏萃取法和固相微萃取法对棕榈油与菜籽油复合火锅底料中的挥发性风味物质进行提取,并通过气相色谱-质谱联用分析及鉴定。采用2 种方法共鉴定出82 种化合物,其中包括醇类17 种、醛类15 种、酯类9 种、萜烯类16 种、酮类5 种、烃类13 种和其他化合物7 种。其中采用同时蒸馏萃取法检测出58 种化合物,采用固相微萃取法检测出41 种化合物,2 种方法检测出的化合物均以芳樟醇相对含量最大,其次为茴香脑。     

超临界CO2提取葛缕子精油及其成分分析

目的:优化葛缕子精油的提取工艺并对其成分进行分析。方法:以葛缕子籽粒为原料,采用超临界CO₂技术提取葛缕子精油,并通过气相色谱—质谱(GC-MS)对精油挥发性成分进行分析。结果:超临界CO₂提取葛缕子精油的最佳工艺条件为提取釜温度50℃,分离釜温度40℃,提取釜压力30 MPa,分离釜压力0.4 MPa,二氧化碳流速20 g/min,提取时间90 min,此条件下精油得率为4.79%。与同时蒸馏萃取(SDE)法相比,超临界CO₂流体能快速扩散到样品颗粒内部并充分溶解其中的精油成分,具有提取时间短、得率高、无溶剂残留的优点。超临界CO₂法制备的葛缕子精油中,主要成分为D-柠檬烯(50.96%)和香芹酮(46.65%),挥发性成分种类及含量均高于同时蒸馏萃取法的。结论:超临界CO₂法比同时蒸馏萃取法更适合葛缕子精油的提取。     

Characterization of volatile compounds of pu-erh tea using solid-phase microextraction and simultaneous distillation–extraction coupled with gas chromatography–mass spectrometry

Two extraction methods, namely, solid-phase microextraction (SPME) and simultaneous distillation–extraction (SDE) both followed by gas chromatography–mass spectrometry were applied for the determination of a wide range of volatile compounds in pu-erh tea. The conditions of solid-phase microextraction including fiber selections and sampling condition optimization have been previously investigated. By the two methods, 79 volatile compounds belonging to different categories were identified. Among them, 61 volatile compounds were extracted by SDE and 67 by SPME. Qualitative and quantitative differences of pu-erh tea volatile profiles were observed by applying the two aforementioned extraction methods. SDE technique achieved higher percentages of high molecular weight alcohols, acids, and esters of low volatility, whereas SPME technique was found useful for analyzing low molecular weight alcohols, methoxy-phenolic compounds, aldehydes, ketones, and hydrocarbons of high volatility that were closely related to the characteristics of pu-erh tea aroma and its sensory perception. Therefore, SPME technique was a reliable extraction method for controlling pu-erh tea quality flavor.     

辛夷挥发油GC-MS分析及其抗氧化、抗菌活性

采用水蒸气蒸馏（hydrodistillation,HD）法、同时蒸馏萃取（simultaneous distillation extraction,SDE）法、静态顶空（static headspace,SH）法3 种方法对辛夷挥发油进行提取,通过气相色谱结合标准品获得保留指数,气相色谱-质谱联用结合数据库检索进行定性,确定不同方法提取的挥发油的成分和相对含量,并采用1,1-二苯基-2-三硝基苯肼自由基清除法、普鲁士蓝法和新铜试剂法比较HD法和SDE法挥发油的抗氧化能力,以及滤纸片扩散法和96 孔板法测定抗菌活性。结果表明,3 种方法共鉴定出66 种化学成分,其中17 种共有成分。从HD法和SDE法挥发油中分别鉴定出47 种和43 种化合物,SH法对辛夷粉末分析检测到26 种化合物。其中,HD和SDE提取的化合物成分较接近,而SH法获得的挥发成分最少,三者相同成分的相对含量也存在较大差异。HD法和SDE法挥发油均表现出一定的抗氧化活性,对供试菌（金黄色葡萄球菌、单增李斯特氏菌、大肠杆菌、鼠伤寒沙门氏菌）均有抑制作用,对其中的革兰氏阴性菌的抑制效果较好。辛夷挥发油的抗氧化和抗菌研究显示其具有药学研究价值和作为食品天然抗菌剂和食品防腐剂的潜能。     

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.     

Olive oil volatile compounds,flavour development and quality: A critical review

The unique and delicate flavour of olive oil is attributed to the volatile compounds that develop during and after oil extraction from the olive fruit. The formation of these volatile compounds and the fruit characteristics that affect the formation are examined in this review. The role of extraction time -temperature interactions in volatile development and other factors that impact volatile development, such as fruit storage prior to oil extraction, are also considered. The volatile compounds that develop during extraction become less dominant during oil storage with the emergence of volatile compounds from chemical oxidation. The presence or absence of particular volatile compounds partly explains quality differences in olive oils.     

花椒精油亚临界流体萃取工艺优化及GC-MS分析

以甘肃武都大红袍花椒为原料,采用水蒸气蒸馏萃取法（SDE）及亚临界流体萃取法（SFE）提取花椒精油。以花椒精油得率为评价指标,采用单因素试验和正交试验优化SFE萃取工艺,并采用气质联用法（GC-MS）对比分析SDE和SFE花椒精油的香气成分。结果表明,最佳萃取工艺为：萃取3次、萃取温度40℃、萃取时间40 min、料液比1.0∶2.0(g∶mL)。在此优化条件下,SFE花椒精油得率为15.11%,为SDE精油得率的3.7倍。GC-MS分析结果表明,共检测出48种挥发性物质,包括烯烃类20种、酯类8种、醇类8种、醛类3种、芳香烃类2种、呋喃类2种、酮类2种、萜类1种、酸类1种和萘类1种。SDE和SFE分别检出37种、40种挥发性物质,两种提取方法所得精油的组成相似,SFE精油得率较SDE高且留香型持久,是提取花椒精油的有效提取方法。     

The comparison of physico-chemical and textural properties, as well as volatile compounds, from low-fat and regular-fat sausages

In order to determine the optimum method for extraction of the entire flavour profile of sausages, three extraction techniques, solvent extraction (SE), purge and trap (PT), and simultaneous distillation extraction (SDE), were compared. Similarly, to effectively analyse the volatile compounds of low‐fat (<3%) and regular‐fat (approximately 15%) sausages, three isolation techniques were investigated and gas chromatography (GC) and gas chromatography–mass spectrometry (GC/MS) were used for final identification of compounds. A total of thirty‐three volatile compounds were identified in the sausages by SDE, twelve by SE, and nine by PT. In the SE method, fats interfered in the extraction of some volatile components, resulting in lower recovery and longer isolation time when compared with the other two methods. The PT method might not be a good extraction method because of the loss of heterocyclic compounds. However, the SDE method showed greater yields and recognized more volatiles when compared with SE. Furfural, trans‐caryophyllene, and myristicine were the predominant volatile compounds extracted by SDE. These results suggest that the SDE method is the most efficient method in isolating volatile compounds in both regular‐ and low‐fat sausages. The amounts of volatile compounds, such as, 4‐acethyl‐3‐methyl pyrazole, 1,4‐dimethyl benzene, p‐ethylguaiacol and β‐caryophyllene were higher in regular‐fat sausages; however, the amounts of myristicine and hexadecanoic acid were higher in low‐fat sausages.     

提取方法对百里香精油化学成分和抗氧化活性的影响

本文分别采用水蒸气蒸馏法（SD）、同时蒸馏萃取法（SDE）、冷等离子体辅助提取法（CPAE）从百里香叶片中提取精油,通过气相色谱-质谱联用（GC-MS）分析了三种精油中的挥发性成分,测定其精油中的总酚、总黄酮、花青素含量,通过DPPH?、ABTS+?、总抗氧化能力三个抗氧化指标评估了其体外抗氧化性,并将精油中的主要活性成分与抗氧化能力进行相关性分析,比较得出得率更高、抗氧化性更好的提取方法。结果表明,不同提取方法在精油得率上有显著性差异（P<0.05）,SDE法的精油得率最高,达到了1.30%。经GC-MS分析,三种精油共检出了36种组分,主要成分均为2-茨醇（32.194%~32.515%）、香芹酚（17.265%~19.998%）、百里香酚（13.031%~15.202%）和α-松油醇（11.296%~12.012%）,其中,SDE法和CPAE法比SD法制备得到的精油在以上活性成分上含量更高。在总酚、总黄酮、花青素的测定结果中,SDE法制备得到的精油中总酚和花青素含量更高,分别为133.67±0.20 mg GA/g EO、0.32±0.02 mg/g EO,CPAE法制得的精油总黄酮含量最高,达到了54.82 mg Rutin/g EO。在体外抗氧化性实验中,三种精油在实验浓度范围内对各项抗氧化指标都表现出较强的抗氧化性和明显的量效关系,其中,SDE法获得的精油对于自由基的清除效果更佳,在最高实验浓度下清除率均在96%以上。通过抗氧化相关性分析发现,百里香精油的抗氧化活性与酚类等物质的含量密切相关。综上,从各项实验结果来看,SDE法是一种更为可取的提取百里香精油的方法。     

白豆蔻精油超临界CO2萃取工艺优化及挥发性成分分析

以白豆蔻为原料,利用水蒸气蒸馏（SDE）法和超临界流体萃取（SFE）法提取白豆蔻精油。以萃取率为评价指标,采用单因素试验及正交试验优化萃取工艺,并采用气质联用（GC-MS）法分析两种提取方法所得白豆蔻精油的组成。结果表明,最佳萃取工艺条件为：萃取压力25 MPa、萃取温度50 ℃、CO2流量14 mL/min、提取时间4.0 h。在此优化条件下,SFE提取白豆蔻精油得率为6%,为SDE提取精油的1.5倍。GC-MS分析结果表明,共检出挥发性化合物158种,其中SDE和SFE提取精油中分别检出97种、111种,独有化合物分别有47种、61种,共有化合物有50种。两种提取方法所得精油的组成相似,主要成分有桉叶油醇、α-蒎烯、4-异丙基甲苯、顺式十五烯酸、棕榈酸等,但含量差异较大。结果表明SFE是提取白豆蔻精油的有效方法。     

紫苏不同部位精油成分及体外抗氧化能力的比较研究

采用同时蒸馏萃取法提取紫苏不同部位(叶、花蕾、梗和籽)精油,利用气相色谱-质谱法对精油成分进行分析,并比较不同部位精油体外抗氧化能力。结果表明：紫苏叶精油得率相对最高,达到8.21‰。从紫苏叶、花蕾、梗和籽精油中依次鉴定出40、53、29和26种组分,分别占各自精油总量的99.85%、99.25%、96.73%和97.51%。不同部位精油成分和相对含量差异显著,共有组分仅5种,分别是2-己酰呋喃、4-(2-甲基环己烯)-2-丁烯醛、石竹烯、芳樟醇和石竹素,其中相对含量最高的组分均是2-己酰呋喃。紫苏不同部位精油均具有一定的抗氧化能力,紫苏叶精油清除DPPH自由基的能力较强,紫苏籽精油清除羟自由基的能力较强。     

不同方法提取辛夷挥发油化学成分与热失重分析的比较

辛夷是一种传统的中药材,且具有明显的香气特征,可以作为香料使用。本文采用水蒸气蒸馏萃取、同时蒸馏萃取、超临界二氧化碳(CO2)萃取和超声波辅助萃取法对辛夷挥发油进行了提取,采用气相色谱-质谱联用(GC/MS)技术对辛夷挥发油成分进行了鉴定和检测,并对挥发油进行了热失重研究。结果显示,4种不同提取方法的挥发性成分共有61种,主要是萜烯类、醇类、醛酮类和酯类等;通过对4种不同提取方法挥发油的热失重分析发现,水蒸气蒸馏萃取、同时蒸馏萃取和超声波辅助萃取法提取的挥发油的热失重曲线类似,均呈现四个失重阶段,但略有差异;超临界CO2萃取法提取的挥发油热失重曲线为三个失重阶段。4种失重曲线的不同说明4种提取方法提取的挥发性成分存在差异。     

固相微萃取和同时蒸馏萃取法分析海南香草兰挥发性成分

对固相微萃取（solid phase micro-extraction,SPME）技术萃取香草兰中挥发性成分的萃取条件进行优化, 并采用SPME和同时蒸馏萃取（simultaneous distillation extraction,SDE）两种方法对海南地区香草兰豆荚中挥发 性成分进行检测分析。结果表明：SPME最优萃取条件为萃取头75 μm CAR/PDMS、萃取温度80 ℃以及萃取时 间20 min。2 种萃取方法共检测出105 种挥发性成分,其中利用SPME技术检测出挥发性成分73 种,SDE检测出78 种。结果表明：将SPME和SDE两种方法联合使用可以更加全面地检测出香草兰中的挥发性成分。     

SDE和SPME法对鲊海椒发酵中香气组成的比较分析

为确定评价鲊海椒挥发性香气组成的最优方法,以粳米粉为淀粉原料制备鲊海椒,采用固相微萃取（solidphase microextraction,SPME）法和同时蒸馏萃取（simultaneous distillation extraction,SDE）法并结合感官评价比较研究其在发酵过程中风味物质的变化。结果发现,SPME法萃取发酵0、45 d和90 d鲊海椒挥发性成分种类分别为76、131 种和122 种,SDE法挥发性成分分别为23、42 种和82 种;随着发酵时间的延长,SDE法挥发性香气成分增加,而SPME法在发酵45 d时挥发性香气物质种类达峰值并保持稳定。酯类是鲊海椒发酵过程中主要的挥发性成分,采用SPME法和SDE法萃取发酵45～90 d鲊海椒,分别检出挥发性酯类42～50 种（相对含量46.7%～55.3%）和15～27 种（相对含量60.28%～67.28%）;SPME法检出较多醇类、醛类,发酵45～90 d鲊海椒醇类14～21 种（相对含量15.7%～22.6%）和醛类17 种（相对含量5.8%～12.3%）。SPME法可萃取得到更多低沸点、小分子化合物;而SDE法得到更多高沸点化合物;感官评定显示发酵45 d后的鲊海椒色泽鲜艳,具有特殊的酸味和醇香味。结果表明,采用SPME法结合SDE法评价鲊海椒挥发性香气组成更加全面客观,鲊海椒适宜发酵时间为45～90 d。     

SDE-GC-O-MS鉴定浓香葵花籽油香气活性物质

采用同时蒸馏萃取法（SDE）萃取浓香葵花籽油中的挥发性风味物质,利用气相色谱-质谱-嗅闻技术（GC- O-MS）对香气活性物质进行分离鉴定。SDE的最佳萃取条件为：二氯甲烷40 mL,加油量40 g,水添加量 200 mL,萃取时间3 h。经GC-MS分析共鉴定出96种挥发性风味物质,主要为醛类（29.29%）、杂环类（29.10%）、萜烯类（26.79%）、醇类（3.08%）、烯烃类（1.78%）、酮类（1.47%）、烷烃类（0.57%）、酯类（0.43%）和酸类（0.25%）。GC-O鉴定出24种香气活性物质,主要包括吡嗪类物质,赋予浓香葵花籽油烤香味;萜烯类物质,赋予其包括松针味的植物清香。     

同时蒸馏萃取法提取花生油挥发性物质的研究

采用同时蒸馏萃取法结合气相色谱-质谱分析技术（SDE-GC-MS）,对水酶法制备的花生油挥发性物质进行提取和分析,优化同时蒸馏萃取条件。结果表明：花生油总挥发性化合物种类及吡嗪类化合物相对含量均随样品量的增加而增加;二氯甲烷作为萃取溶剂萃取得到的总挥发性化合物种类及吡嗪类化合物相对含量较乙醚多;在花生油用量为30 g时,采用二氯甲烷可以萃取出66种化合物,经质谱分析可鉴定出42种化合物,其中吡嗪类化合物有6种,占总挥发性成分6.73%。     

兔肉挥发性风味成分提取效果的比较

为比较不同提取技术对兔肉挥发性风味物质的提取效果,明确兔肉特征风味物质。采用同时蒸馏萃取（simultaneous distillation extraction,SDE）、固相微萃取（solid phase micro extraction,SPME）和超临界二氧化碳流体萃取（supercritical carbon dioxide fluid extraction,SFE）3 种常用方式,提取兔肉风味物质,定量加入2,4,6-三甲基吡啶,通过气相色谱-质谱法进行定性和定量研究,比较提取率差异,确定兔肉主体风味成分。结果显示：SDE法提取到包括烃、醇、醛、酸、酯、酮、醚和杂环共8 类75 种化合物;SPME法提取到烃、醛、酮和酯共4 类41 种化合物;SFE法提取到烃、醇、醛、酯和杂环共5 类38 种化合物。提取物质种类：SDE＞SFE＞SPME,提取物质量：SFE＞SDE＞SPME,提取量：SPME＞SFE＞SDE。通过气味活度值法,确定己酸、己醛、辛醛、壬醛、2,4-癸二烯醛和1-辛烯-3醇为兔肉主体风味物质。