北细辛超临界萃取物挥发性成分的GC-MS分析

采用超临界流体萃取法(SFE)和水蒸气蒸馏法分别对北细辛根及根茎进行提取分离,分别得5.5%SFE萃取物和2.8%挥发油。应用GC-MS分析,从北细辛SFE萃取物中鉴定出7种化学成分,占萃取物总量的72.70%,其中甲基丁香酚为44.62%;从细辛挥发油中鉴定出19种化学成分,占挥发油总量的88.53%,其中甲基丁香酚为43.02%。两种方法有6种成分完全相同,其中致癌物质黄樟油素SFE法比蒸馏法低2.8倍。北细辛根及根茎超临界萃取物与水蒸汽蒸馏挥发油主要成分相同,但其化学组成存在较大差异,提示药效亦不相同。超临界流体萃取法是剂型改革的有效方法之一。     

小花清风藤挥发油化学成分研究

利用水蒸气蒸馏法提取小花清风藤中的挥发性成分,通过气相色谱质谱联用技术（GC-MS）并结合计算机分析鉴定提取物中挥发油芳香成分,共鉴定出17种化合物,其中有12种烷烃类化合物,1种芳香类化合物,1种醚类化合物,1种杂环类化合物,1种环戊二烯和1种酰胺类化合物。用面积归一化法测定挥发油中各种成分的相对含量,合计占总峰面积的8.8%。实验结果表明：用水蒸气蒸馏提取小花清风藤挥发油时,提取率为4.18%,其最主要成分为烷烃类化合物。     

Analysis of Rhioxma Curcumae Aeruginosae volatiles by solid-phase microextraction with gas chromatography-mass spectrometry

In this paper, a headspace solid-phase microextraction (HS-SPME) method was applied to analyse the volatile compounds in a traditional Chinese medicine (TCM), Rhioxma Curcumae Aeruginosae. SPME parameters such as fibers, extraction temperature, extraction time and desorption time were investigated. Thirty-five volatile compounds were separated and identified. Relative standard deviations (RSDs) were less than 8.4%, showing that the method has a good reproducibility. The volatile constituents were also analyzed by steam distillation (SD) and thirty-seven compounds were identified. The similar results obtained by the two methods showed that SPME is a good alternative for the analysis of volatile constituents in Rhioxma Curcumae Aeruginosae samples and it is a relatively simple, rapid and solvent-free method.     

不同提取方法对黔产水香薷挥发性成分的影响

比较不同提取方法对黔产水香薷挥发性成分影响。采用固相微萃取法、水蒸气蒸馏法提取水香薷挥发性成分,用GC-MS联用仪进行测定,结合NIST05和WILEY275谱库鉴定各化合物,峰面积归一化法测定各成分相对含量。利用两种提取方法供从水香薷中鉴别出67个化合物。从固相微萃取法提取物中检测并鉴定了45个化合物,而从水蒸气蒸馏法提取物种检测并鉴定了55个化合物。其中挥发性相同的化合物有33种,两种不同提取方法得到的挥发性成分虽有差异,但主要成分变化不大。体外抗菌试验表明,水香薷挥发性成分具有抑菌作用。这些研究结果为香料植物水香薷的开发提供了科学依据。     

广西姜黄挥发油两种提取方法的比较研究

以广西姜黄那坡县种植的姜黄为原料,以水蒸汽蒸馏法和以石油醚为溶剂的索氏提取法,分别提取挥发油,并用GC-MS分析法对这些以不同加工途径获取的姜黄挥发油进行成分分析,比较了不同的加工办法对挥发油的加工得率、主要成分和含量的影响。研究表明:广西那坡的姜黄挥发油主要成分为:α-姜黄烯、芳姜黄酮、(-)-姜烯、β-倍半水芹烯、β-姜黄酮、α-姜黄酮、4-(1,5-二甲基-4-己烯基)-2-环己烯酮、β-没药烯。     

Comprehensive two‐dimensional gas chromatography–mass spectrometry analysis of volatile constituents in Thai vetiver root oils obtained by using different extraction methods

Introduction – Vetiver root oil is known as one of the finest fixatives used in perfumery. This highly complex oil contains more than 200 components, which are mainly sesquiterpene hydrocarbons and their oxygenated derivatives. Since conventional GC‐MS has limitation in terms of separation efficiency, the comprehensive two‐dimensional GC‐MS (GC × GC‐MS) was proposed in this study as an alternative technique for the analysis of vetiver oil constituents. Objective – To evaluate efficiency of the hyphenated GC × GC‐MS technique in terms of separation power and sensitivity prior to identification and quantitation of the volatile constituents in a variety of vetiver root oil samples. Methodology – Dried roots of Vetiveria zizanioides were subjected to extraction using various conditions of four different methods; simultaneous steam distillation, supercritical fluid, microwave‐assisted, and Soxhlet extraction. Volatile components in all vetiver root oil samples were separated and identified by GC‐MS and GC × GC‐MS. The relative contents of volatile constituents in each vetiver oil sample were calculated using the peak volume normalization method. Results – Different techniques of extraction had diverse effects on yield, physical and chemical properties of the vetiver root oils obtained. Overall, 64 volatile constituents were identified by GC‐MS. Among the 245 well‐resolved individual components obtained by GC × GC‐MS, the additional identification of 43 more volatiles was achieved. Conclusion – In comparison with GC‐MS, GC × GC‐MS showed greater ability to differentiate the quality of essential oils obtained from diverse extraction conditions in terms of their volatile compositions and contents. Copyright © 2009 John Wiley & Sons, Ltd.     

贵州产辣蓼挥发性成分分析

采用固相微萃取法和水蒸气蒸馏法提取出贵州产辣蓼的挥发性成分,运用GC-MS联用技术对挥发性成分进行分析鉴定,并采用峰面积归一法确定各成分的相对含量。固相微萃取物中鉴定出48个化合物,主要有β-石竹烯(27.02%),正癸醇(14.39%),十二醛(12.96%)等,水蒸气蒸馏物中鉴定出27个化合物,β-红没药烯(19.00%),补身树醇(15.25%),十二醛(14.41%)等。辣蓼中挥发性成分经两种不同提取方法成分存在明显差异。与文献数据比较,不同省区产的辣蓼挥发性成分差异很大。体外抗菌试验表明,辣蓼挥发性成分具有抑菌作用,这些研究结果为辣蓼的有效利用提供了依据。     

大蒜化学成分的气-质联用分析

本文采用环己烷、乙酸乙酯和正丁醇对大蒜（Allium sativum L.）新鲜鳞茎的95%乙醇提取物进行萃取,并与水蒸气蒸馏法提取的挥发油成分进行比较,用GC-MS对其成分进行定性和定量分析.在环己烷萃取物中共检出112个成分,鉴定了38个化合物,占环己烷萃取物总量的80.08%;在乙酸乙酯萃取物中检出86个成分,鉴定了26个化合物,占乙酸乙酯萃取物总量的56.70%;在正丁醇萃取物中未检出挥发性成分.在水蒸气蒸馏法提取的挥发油中共检出109个成分,鉴定了29个化合物,占挥发油总量的83.58%.大蒜95%乙醇提取物的环己烷和乙酸乙酯萃取物及大蒜挥发油中皆以含硫化合物为主.在环己烷和乙酸乙酯萃取物中,阿霍烯的含量分别为生药的0.00395%和0.00145%,大蒜中阿霍烯含量达0.00540%.     

The Fragrance Components of the Jasrninnm sambac (L.) Alton collected by Simultaneous Steam Distillation and Solvent Extraction

The volatile fragrance components of Jasminum sambac (L.) Aiton flower were collected by a modified simultaneous steam distillation and solvent extraction apparatus (SDE). The obtained extract was concentrated to 100 μL by the gas entrainment method in which the extract was distilled under reduced pressure with the influence of a steam of nitrogen. The concentrate was analyzed by GC-MS with PEG-20 M capillary column, and the Kovats indexes were determined at the same time whereby the nalkanes were added into extract. 28 compounds were identified. The major components were: linalool, benzyl acetate, ciscaryophyllene, cis-3-benzyl benzoate, methyl anthranilate and indole. These results show the components of the extract have no qualitative difference from absolute oil. The advantages of the above procedure were discussed in detail.     

Isolation and Characterization of Antioxidation Enzymes from Cells of Zedoary (Curcuma zedoaria Roscoe) Cultured in a 5-l Bioreactor

In this study, a cell suspension culture system for zedoary (Curcuma zedoaria Roscoe) was developed, using 50 g/l of fresh weight inoculum in a batch culture. The highest cell biomass obtained from a 5-l bioreactor equipped with three impellers after 14 days of culture was utilized to extract secondary metabolites (essential oil and curcumin) and determine the activities of antioxidant enzymes (peroxidase, superoxide dismutase, and catalase). For essential oil and curcumin, zedoary extracts were recovered via a variety of methods: steam distillation, volatile solvents, and Soxhlet. After 14 days of culture using volatile solvents, the optimal yield of essential oil (1.78%) was obtained when using petroleum ether at 40°C in 6 h of extraction, and the best curcumin yield (9.69%) was obtained at 60°C in 6 h via extraction with 90% ethanol. The activities of antioxidant enzymes from zedoary cells were also assessed. The specific activities of peroxidase, superoxide-dismutase, and catalase reached maximum values of 0.63 U/mg of protein, 16.60 U/mg of protein, and 19.59 U/mg of protein after 14 days of culture, respectively.     

水蒸气蒸馏法提取大蒜挥发油的工艺研究

以挥发油提取率为指标,通过单因素和L9(34)正交试验设计确定了水蒸气蒸馏法提取大蒜挥发油的最佳提取工艺及条件。结果表明,各因素作用主次顺序为蒸馏时间(D)>料液比(C)>发酵温度(A)>浸泡时间(B),各因子的最优组合为A2B2C2D3,即以1∶3.5的料液比(m∶V),在35℃时浸泡3h后蒸馏2h为大蒜挥发油的最佳提取工艺,此时挥发油的提取率达到0.32%,证明此方法是大蒜挥发油提取的可靠、易行的科学方法。     

Comparison of Three Different Extraction Methods on Osmanthus Volatile Oil: Aroma and Biological Activity

The osmanthus volatile oil was welcomed by consumers even if the high price since the unique and pleasant odor. Meanwhile, the low yield of osmanthus volatile oil restricts industrial production. In this work, an osmanthus volatile oil was obtained by means of a novel ultrasonic-assisted flash extraction method and was compared with the oil from hydrodistillation and supercritical fluid extraction on yield, aroma, and biological activities. The volatile oil obtained from the ultrasonic-assisted flash extraction was obtained with the petroleum ether and got a high yield at 3.51 % within a 40-min process, an increase of nearly 81 % from the single solvent extraction. This oil also showed a high aroma intensity and aroma compound concentration. Meanwhile, the oil also has the highest antioxidant ability but lower antibacterial activity against oil from hydrodistillation. It was considered that this work was helpful for the optimization of the extraction method of osmanthus volatile oil.     

茯神挥发性成分及其生物活性研究

为研究茯神挥发性成分含量、构成及其生物活性,本实验采用二氧化碳超临界的方法提取茯神低极性成分,以提取率作为响应值,在单因素试验的基础上采用响应曲面法考察提取压力、温度、二氧化碳流速对提取效果的影响,优化提取工艺。运用气相色谱-质谱联用仪(GC-MS)对其主要化学成分进行鉴定,并采用生长速率法测定了挥发油对5种真菌的生物活性。得到提取模型极值点,即提取压力27.26MPa、提取温度55.97℃、提取流速10.68L/min时,提取率达到最大,提取率预测值为1.66mg/g。通过NIST14质谱库检索,鉴定了其中17个主要化合物,运用峰面积归一法确定各个组分的含量,占挥发油总量的84.5%。抗菌实验表明茯神挥发油对采绒革盖菌菌株有低浓度促进高浓度抑制的活性。     

山胡椒挥发油的提取及其抑菌活性研究

目的:研究山胡椒中挥发油最佳提取方法和其抑菌作用。方法:采用水蒸汽蒸馏法、微波萃取法和超临界CO2萃取法三种方法提取干山胡椒果实中的挥发油,研究山胡椒挥发油对7种细菌、4种霉菌、2种酵母的抑菌活性及其最低抑菌浓度(MIC)。结果:水蒸汽蒸馏法提取的山胡椒挥发油为淡黄色液体,提取率为10.0%;微波萃取法提取的山胡椒挥发油为黄褐色液体,提取率为11.6%;超临界CO2萃取的山胡椒挥发油为亮黄色液体,提取率为14.7%。山胡椒挥发油经固相和气相扩散,对细菌、酵母有较强的抑菌能力,对霉菌具有很强的抑制能力。对所有供试菌的最低抑菌浓度(MIC)为0.2%。结论:提取干山胡椒果实中的挥发油的最好方法是超临界CO2萃取法。山胡椒挥发油有较强的抑菌能力,最低抑菌浓度(MIC)为0.2%。     

木香薷精油最佳提取工艺的研究

以富含精油而著称的唇形科植物木香薷(Elsholtzia stauntoni Benth.)为研究试材,采用水蒸气蒸馏法设计不同的试验处理条件,对木香薷不同部位的精油进行提取,研究其最佳提取工艺。结果表明:木香薷精油提取的最佳工艺为切段后水蒸气蒸馏法,馏出液体积为1 500 mL;水蒸气蒸馏法提取精油要优于共沸蒸馏法。在对木香薷不同部位精油提取的比较研究中,以花穗组材料提取的精油量最大,花穗组与茎叶组间提取的精油量无显著差异,光茎组提取的精油量最少。     

GC-MS分析伊犁绢蒿挥发油化学成分

利用水蒸气蒸馏法提取伊犁绢蒿挥发油,出油率为0．25％。采用色谱-质谱-计算机联用技术,从检出的30个成分中鉴定出28个,所鉴定成分占挥发油色谱总峰面积的98．66％。其主要化学成分为α-苎酮(78．74％)、樟脑(6．17％)、桧烯醇乙酸酯(1．94％)、β-苎酮(1．40％)、乙酸乙酯(1．14％)等,占总挥发油成分的89．46％。     

A novel saccharification method of starch using microwave irradiation with addition of activated carbon

Activated carbons were investigated for their heat catalytic effects to improve saccharification of starch by autohydrolysis in water under microwave electromagnetic field, and the results were compared with graphite and carbon nanotubes. The activated carbons with low adsorptive capacity of maltose showed high saccharification rate, while those with high adsorptive capacity exhibited low saccharification. In addition, the former activated carbons decreased the saccharification temperature by 10-30 °C. Maltooligosaccharides produced in the presence of the latter activated carbons were recovered by desorption with 50% aqueous ethanol. The results indicated that both adsorptive capacities of maltooligosaccharides and catalytic effects of hot spots arisen from the uneven surface structure of activated carbons might contribute to the improvement in starch saccharification.     

Unpolluted fractionation of wheat straw by steam explosion and ethanol extraction

An unpolluted process of wheat straw fractionation by steam explosion coupled with ethanol extraction was studied. The wheat straw was steam exploded for 4.5 min with moisture of 34.01%, a pressure of 1.5 MPa without acid or alkali. Hemicellulose sugars were recovered by water countercurrent extraction and decolored with chelating ion exchange resin D412. The gas chromatography (GC) and high-performance liquid chromatography (HPLC) analysis results indicated that there were organic acids in the hemicellulose sugars and the ratio of monosaccharides to oligosaccharides was 1:9 and the main component, xylose, was 85.9% in content. The total recovery rate of hemicellulose was 80%. Water washed materials were subsequently extracted with ethanol. The optimum extraction conditions in this work were 40% ethanol, fiber/liquor ratio 1:50 (w/v), severity log(R)=3.657 (180 degrees C for 20 min), 0.1% NaOH. The lignin yield was 75% by acid precipitation and 85% ethanol solvent was recovered. The lignin was purified using Bj?rkman method. Infrared spectrometry (IR) results indicated that the lignin belonged to GSH (guaiacyl (G) syringyl (S) and p-hydroxyphenyl (H)) lignin and its purity rate reached 85.3%. The cellulose recovery rate was 94% and the results of electron spectroscopy for chemical analysis (ESCA) and infrared spectrometry (IR) showed that hemicellulose and lignin content decreased after steam explosion and ethanol extraction.     

花椒呈香部位的气相色谱指纹图谱研究

采用气相色谱分析技术对代表性产地的13批花椒水蒸气蒸馏-乙醚萃取物进行了比较,建立了花椒水蒸气蒸馏-乙醚萃取物化学成分的指纹图谱,在本文采用的条件下,花椒图谱具有较好的特征性,可作为花椒蒸馏法精油的专属性指纹图谱。     

Bark Essential Oil of Cedrelopsis grevei from Madagascar: Investigation of Steam‐Distillation Conditions

The effect of the distillation time on the yield and chemical composition of the bark essential oil of Cedrelopsis grevei Baill. was investigated. Distillation kinetics were determined for three batches of bark sampled from two sites, i.e., Itampolo (batches IT1 and IT2) and Salary (SAL), located in a region in the south of Madagascar with characteristically large populations of C. grevei. The bark samples were subjected to steam distillation, and the essential oil was collected at 3‐h intervals. The total yield (calculated after 14 h of distillation) varied from 0.9 to 1.7%, according to the batch tested. Moreover, the essential oils obtained were characterized by GC‐FID and GC/MS analyses. During the course of the distillation, the relative percentages of the most volatile components (monoterpenes and sesquiterpene hydrocarbons) diminished progressively, whereas the least volatile ones (oxygenated derivatives) increased at a consistent rate. Principal component analysis (PCA) and agglomerative hierarchical clustering analysis (AHC) of the results, performed on 13 principal components, allowed distinguishing three chemical groups, corresponding to the three batches, irrespective of the distillation time. This indicated that the chemical variability currently observed with commercial samples is not mainly linked to the experimental conditions of the extraction process, as the distillation time did not significantly alter the chemical composition of the essential oils.