超临界CO_2萃取与水蒸气蒸馏法提取太子参挥发油化学成分气质联用研究

目的:分析比较采用超临界CO2流体萃取法与水蒸气蒸馏法提取的太子参提取物中挥发性化学成分的异同。方法:使用水蒸馏提取法和超临界CO2萃取技术从太子参中提取挥发性成分,用归一化法测定其百分含量。用气相色谱-质谱(GC-MS)计算机联用技术分离鉴定其中的化学组成。结果:太子参超临界CO2流体萃取物中初步鉴定了33种成分,主要成分为:亚油酸乙酯(28.70%)、n-十六酸(23.12%)、3-糠醇(5.51%)等;水蒸气蒸馏法提取挥发油初步鉴定了17种成分,主要成分为2-丙基呋喃(22.45%)、3-糠醇(19.78%)、3-乙基-3-甲基戊烷(19.47%)。结论:2种方法提取的挥发油化学成分差异较大,超临界CO2流体萃取法提取的挥发油能更真实、全面地反映太子参药材中的化学成分。     

三种方法提取防风挥发油的气质联用成分分析

目的对3种不同方法提取的防风挥发油化学成分进行分析。方法采用水蒸气蒸馏法（SD）、溶剂提取法（SX）、超临界CO2流体萃取法（SFE-CO2）提取防风挥发油,用气相-质谱（GC-MS）法对化学成分进行鉴定。结果水蒸气蒸馏法提取挥发油共鉴定了13种化学成分;溶剂提取法提取的挥发油共鉴定了18种化学成分;超临界CO2流体萃取法提取的挥发油共鉴定了21种化学成分。结论超临界CO2流体萃取法提取的挥发油更全面地反映药材中的化学成分。     

超临界CO_2流体萃取法与水蒸汽蒸馏法提取蒌蒿挥发性化学成分的研究

目的比较分析水蒸汽蒸馏法和超临界CO2萃取法所提蒌蒿挥发油的化学成分及其含量。方法采用水蒸汽蒸馏法和超临界CO2萃取法提取,运用毛细管气相色谱-质谱联用技术对蒌蒿挥发性成分进行分析,用气相色谱面积归一化法测定各成分的相对百分含量。结果与结论水蒸汽蒸馏法提取蒌蒿挥发油,经毛细管色谱分离出82个峰,并鉴定出71个化合物,其主要化学成分为桉油精、顺式-β-金合欢烯、β-侧柏酮等;超临界CO2萃取法提取蒌蒿挥发油,经毛细管色谱分离出49个峰,并鉴定出40个化合物,其主要化学成分为4-甲基苯甲醇、桉油精、β-侧柏酮等。     

川芎药材超临界CO2萃取与水蒸气蒸馏提取挥发油比较研究

目的 通过对不同工艺下得到的川芎挥发油的比较,阐明提取工艺对其有效成分的影响。方法 分别采用超临界CO₂萃取和水蒸气蒸馏法提取川芎挥发油,再通过气相色谱-质谱(GC-MS)联用技术分析鉴定其中的主要化学成分及相对含量。结果 2种方法所得川芎挥发油样品中共鉴定18种共有成分,水蒸气蒸馏提取物中苯酞类成分约占61%,单萜类成分约占25%,倍半萜类成分约占10%;超临界CO₂萃取物中苯酞类成分约占97%,单萜类成分约占1%,倍半萜类成分约占0.4%。结论 水蒸气蒸馏法对川芎药材中挥发性较强的单萜和倍半萜类保留相对较强,超临界CO₂萃取法对苯酞类有效成分的提取率相对较高,因此在川芎挥发油入药的中药制剂工艺中,应根据制剂的功效充分考虑提取工艺对有效成分的影响。     

Gas chromatography for analysis of essential oils. Characteristics of essential oil of Dracocephalum species and the influence of extraction method on its composition

In this work the essential oil composition of some less known Dracocephalum species was studied and compared the effectiveness, selectivity and influence of different extraction methods (hydrodistillation, Soxhlet extraction with organic solvents and supercritical fluid extraction) on essential oils. For investigations in Hungary and Transylvania cultivated plant material was used. The analysis of essential oils was carried out by GC and GC-MS methods. The components were identified by standard addition, retention factors and mass spectra. The percentile evaluation of each volatile constituents was made on basis of GC-FID chromatograms. The accuracy of measurements was characterized by relative standard deviation. In the essential oil of D. renati Emb. (studied firstly by us) 18.3% of limonene was measured and carvone, citrals and linalyl acetate monoterpenes, methyl chavicol and some sesquiterpene (e.g. bicyclovetivenol) determined in lower quantities. We established that more than 50% of essential oil of D. grandiflorum L. was formed by sesquiterpenes (beta-caryophyllene and- oxide, beta-bourbonene, beta-cubebene, aromadendrene) and the essential oil of D. ruyschiana L. contained pinocamphone isomers in more than 60%. The oxygenated acyclic monoterpenes, the characteristic constituents of Moldavian dragonhead were present in some tenth percent only in D. renati oil. We found significant differences in the composition of the SFE extract and traditional essential oil of D. moldavica L. The supercritical fractions collected at the beginning of the extraction process were richer in valuable ester component (geranyl acetate) than the essential oil obtained by hydrodistillation. The fractions collected at the end of supercritical were poor in oxygenated monoterpenes but rich in minor compounds of traditional oil, e.g. palmitic acid.     

岷当归挥发油提取方法及其化学成分研究

目的分析岷当归挥发油的主要化学成分。方法分别采用超临界CO2流体萃取法(SFE)和水蒸气蒸馏法(SD)提取岷当归的挥发油,并通过GC-MS技术对其进行分析,面积归一化法测定计算各成分的相对百分含量。结果水蒸气蒸馏法提取的挥发油共鉴定出73种成分,占挥发油总成分的58.99%;超临界CO2流体萃取法提取的挥发油共鉴定出25种成分,占挥发油总成分的63.43%,相同成分13种。结论 2种提取方法得到的岷当归挥发油组分与含量差别较大,该实验结果为了解其挥发性成分及进一步开发应用提供依据。     

The essential oil of olibanum

The essential oil of the oleogum resin "Olibanum" was prepared by direct steam distillation as well as by steam distillation of an N-hexane extract. Physical and chemical constants of the oil were determined. GC-MS was used for the analysis of the oil. Thirty-three components were identified in the steam distilled oil by their Kováts indices on stabilized OV-1 columns and by mass spectral data. The oil contains 62.1% esters, 15.4% alcohols, 9.9% monoterpene hydrocarbons, and 7.1% diterpenes. Certain minor constituents of the steam distilled oil failed to show up in the oil prepared by steam distillation of the N-hexane extract. Both oils exhibit antimicrobial activity, the activity of the steam distilled oil being higher than that of the oil prepared by steam distillation of the N-hexane extract.     

Effects of hot water treatment on the essential oils of calamondin

Volatile constituents of calamondin peel or whole fruit were obtained by cold pressing, steam distillation, or hot water treatment at 90°C for 15 minutes followed by steam distillation. The volatile components of the essential oils were identified by direct injection coupled with gas chromatography–flame ionization detector. A total of 54 compounds were identified, including 13 monoterpenes, 7 monoterpene alcohols, 1 monoterpene oxide, 4 monoterpene aldehydes, 2 monoterpene ketones, 4 monoterpene esters, 12 sesquiterpenes, 3 aliphatic alcohols, 6 aliphatic aldehydes, and 2 aliphatic esters, with limonene and β-myrcene as the major compounds. The results showed that hot water treatment increased the yields of essential oils from both peel and whole fruit. The relative percentage of the principle constituents in the various prepared essential oils were similar, except for some minor compounds, including linalool, terpinen-4-ol, α-terpineol, and carvone, the content of which were boosted by steam distillation. Whole fruit contained higher levels of monoterpene alcohols than peel did.     

不同方法提取的佛手挥发油气相色谱-质谱分析结果比较

目的：比较分析水蒸气蒸馏法与超临界流体萃取法（SFE）提取佛手挥发油的化学成分和相对含量。方法：运用气相色谱-质谱技术（GC-MS），结合计算机检索对其化学成分进行分离和鉴定，用色谱峰面积归一化法计算各组分的相对含量。结果：水蒸气蒸馏法中鉴定出18种化学成分，SFE中鉴定出16种化学成分，二者的主要成分均含有D-柠檬烯，相对含量前者为57．87％，后者为81．18％；水蒸气蒸馏法提出成分中还含有25．12％的（＋）-2-蒈烯，而SFE法未检测到该成分。结论：两种提取方法成分结果有所不同，但都含有主要成分D-柠檬烯，含量以SFE法为高。     

Studies on the genotoxic properties of essential oils with Bacillus subtilis rec-assay and Salmonella/microsome reversion assay

Genotoxic properties of essential oils from Anthemis nobilis L., Artemisia dracunculus L., Salvia officinalis L., Salvia sclarea L., Satureja hortensis L., Satureja montana L., Thymus capitatus L., Thymus citriodorus Schreb., Thymus vulgaris L., Citrus bergamia Risso, were studied with Bacillus subtilis rec-assay and Salmonella/microsome reversion assay. The essential oil of Artemisia dracunculus L. "Piemontese" turned out to be active in the rec-assay but not in the Salmonella test. DNA-damaging activity was demonstrated to be due to the estragol component of the oil. Advantages of the combined use of these two short-term microbial assays in genotoxic studies are discussed.     

超临界CO2萃取和水蒸气蒸馏法对火麻仁挥发油提取的比较

目的对不同的提取方法提取火麻仁的挥发油化学成分进行比较研究。方法用超临界CO2萃取法（SFKCO2）和水蒸气蒸馏法（SD）对火麻仁的挥发油进行提取，并运用GC-MS法分析了2种提取物中的挥发油化学成分。结果共鉴定出45个成分，SFKCO2法被鉴定的成分有43个，水蒸气蒸馏法提取挥发油被鉴定成分有36个，两者共有成分34个。结论2种方法得到的火麻仁挥发油的主要成分基本一致。     

气-质联用分析比较麻黄及其炮制品中挥发性成分(英文)

采用气质联用法分析麻黄生品及其炮制品种的挥发油成分。采取水蒸汽蒸馏法和超临界流体萃取技术提取麻黄各品种中的挥发油, 其中通过水蒸汽蒸馏法提取得到的麻黄生品、蜜麻黄和清炒麻黄挥发油中, 鉴定的成分分别为48, 57和48种, 蜜炙和清炒后分别产生14 和 9种新成分通过超临界流体萃取法提取得到的麻黄生品、蜜麻黄和清炒麻黄挥发油中, 鉴定的成分分别为22, 36和28 种, 蜜炙和清炒后分别产生15 和23种新成分。麻黄经炮制后挥发油成分和相对含量均发生了明显变化, 这可能是导致麻黄炮制品功效的改变原因之一。     

Analytical and preparative supercritical fluid extraction of chamomile flowers and its comparison with conventional methods

Supercritical fluid extraction (SFE) was compared with Soxhlet extraction, steam distillation and maceration for the isolation of the active components present in chamomile flowerheads. The obtained fractions were analysed by GC-MS and reversed-phase HPLC. The yield of essential oil achieved by a 30-min extraction with pure CO2 at 90 atm and 40 degrees C was 4.4 times higher than that produced by steam distillation performed for 4 h. The recovery of the flavonoid apigenin obtained by supercritical CO2 after a 30-min extraction at 200 atm and 40 degrees C was 71.4% compared to Soxhlet extraction performed for 6 h and 124.6% compared to maceration performed for 3 days. However, the highly polar flavonoid apigenin-7-glucoside was not extracted by 100% CO2 (recovery values < 1.1%). Its extraction efficiency was markedly improved by the addition of the polar modifier methanol (5%, v/v) to the CO2 fluid, yet the obtained recoveries were unsatisfactory (14.6-19.5%). The SFE method was scaled-up for preparative applications using a pilot plant with three separation stages operating in series. Large-scale SFE was technically feasible with pure CO2 as the extracting fluid. However, the use of CO2 modified with organic solvents was not effective at the pilot-plant scale.     

广陈皮的超临界流体萃取和水蒸气蒸馏挥发油的比较分析

目的:比较两种不同提取方法所得的广陈皮挥发油的挥发性化学成分。方法:分别采用超临界CO2流体萃取(SFE)和水蒸气蒸馏(SD)的方法提取广陈皮的挥发油。运用气相色谱-质谱联用法分离和分析两挥发油的挥发性化学成分,主要成分棕榈酸和D-柠檬烯采用标准品的峰面积增大法进一步确认。结果:从广陈皮SFE和SD挥发油中共鉴定出22个成分,占色谱总流出峰面积的97%以上,两者的提取率分别为5.05%和0.46%。SFE挥发油的主要成分为挥发性较弱、相对分子量较大的棕榈酸,SD挥发油的主要成分为挥发性较强、相对分子量较小的D-柠檬烯。此外,SFE和SD挥发油中均有含量不低的2-甲胺基-苯甲酸甲酯。结论:采用两种方法提取广陈皮所得挥发油的挥发性成分不尽相同,且SFE法的提取率高于SD法;两种方法均能将广陈皮的特征性成分2-甲胺基-苯甲酸甲酯提取出来。     

正交试验优选左金漂浮片中挥发油提取工艺研究

目的优选左金漂浮片中吴茱萸挥发油的最佳提取工艺。方法采用正交试验，以挥发油得率为指标，比较超临界萃取及水蒸气蒸馏两种提取方法的提取效果。结果吴茱萸挥发油水蒸气蒸馏的最佳提取工艺为A3B1C3，超临界萃取的最佳提取工艺为A3B1C3，后者明显优于前者。结论与水蒸气蒸馏法相比，超临界萃取法具有耗时少、效率高和对提取后物料破坏较小等优点，适合于批量生产，便于制剂的后续提取工艺制备。     

Chemical composition and antibacterial activity of the essential oils from flower,leaf and stem of Ferula cupularis growing wild in Iran

Abstract

Context: Ferula cupularis (Boiss.) Spalik et S. R. Downie (Apiaceae) is a common plant in Iran that grows in the foothills of Dena Mountain. In traditional folk medicine, this plant has different applications, but there are no studies proving their uses.

Objective: This study is the first attempt to investigate the chemical composition and antibacterial effect of the essential oils of F. cupularis.

Materials and methods: The essential oils from flower, leaf, and stem of F. cupularis were analyzed by using GC and GC-MS. Antibacterial activity of essential oils was determined by microdilution method against Staphylococcus aureus, Staphylococcus epidermidis, Bacillus subtilis, Escherichia coli, Klebsiella pneumoniae, and Pseudomonas aeruginosa.

Results: The essential oil from flower of F. cupularis contained 15 monoterpene, 13 oxygenated monoterpene, and 2 sesquiterpene hydrocarbons. The leaf essential oil contained 12 monoterpene, 13 oxygenated monoterpene, 2 sesquiterpene, 6 oxygenated sesquiterpene hydrocarbons, and 3 non-terpenoid components. Stem essential oil contained one monoterpene, 23 oxygenated monoterpene, 2 sesquiterpene, and 6 oxygenated sesquiterpene hydrocarbons. The MIC value of stem essential oil was 2.85?mg/mL against both Gram-positive bacteria and Gram-negative bacteria except P. aeruginosa which was inhibited at 22.75?mg/mL. The MIC values of leaf and flower essential oils were higher than 5.69 and 22.75?mg/mL, respectively.

Discussion: This study highlighted the strong antibacterial effect of Ferula cupularis’s essential oil which might be due to its high content of oxygenated monoterpene hydrocarbons.

Conclusion: Our results suggested that this plant may be a good candidate for further biological and pharmacological investigations.     

超临界二氧化碳萃取法与水蒸气蒸馏法提取缬草油的化学成分比较

摘要目的对不同提取方法提取的缬草油化学成分进行比较研究。方法采用超临界二氧化碳（CO2）萃取法和水蒸气蒸馏法从缬草中提取缬草油,用气相色谱 质谱联用（GC MS）法进行化学成分定性与相对含量的比较。结果共鉴定了118种成分,超临界CO2萃取法提取物共鉴定98种,水蒸气蒸馏法提取鉴定了67种,共有成分47种;超临界CO2萃取所得缬草油的收率约为水蒸气蒸馏收率的1.8倍。结论超临界CO2萃取法是缬草油较好的提取方法。     

Review on essential oil extraction from aromatic and medicinal plants: Techniques,performance and economic analysis

Essential oils extracted from herbal plants have many foods, cosmetic and medical industries applications. Present study discussed various conventional extraction techniques (steam distillation, hydro-distillation, hydro diffusion and solvent extraction) and advanced (non-conventional) extraction techniques (solvent free microwave extraction, subcritical extraction liquid and supercritical fluid extraction). Economic analysis, kinetics modelling, and GC-MS analysis of essential oil produced by various extraction techniques have also been presented. India is the biggest producer of Indian basil oil and Japanese peppermint oil, and USA is the major importer and exporter of EOs with 14% (US$390.9 m) of world imports and 17% (US$351.7 m) of world exports. Production cost for Steam distillation, Water distillation, solvent extraction and Supercritical fluid extraction varies from 15.85 - 76.50US$/kg, 7.05-86.4US$/kg, 8.35-8.53US$/kg and 6.71-42.69US$/kg, respectively. Second order model are consistent with experimental data as determination coefficient (R²) is higher than first order model. Non-conventional extraction methods are superior to conventional extraction methods in terms of low cost, time and energy saving, less solvent requirements, shorter extraction time, etc. From the techno-economic and environmental perspective, water distillation with full energy integration is the best method for rosemary oil. In contrast, supercritical fluid extraction is the best method for oregano oil.     

超临界CO_2萃取法提取迷迭香油工艺及其化学组分研究

目的:优化超临界CO2萃取迷迭香油工艺,并分析其主要化学组分。方法:采用正交试验优化超临界CO2萃取迷迭香油工艺的参数,将提取物的化学成分经气相色谱-质谱联用法(GC-MS)进行分离鉴定,并计算各组分的相对百分含量。结果:优化的最佳工艺为萃取压力20MPa,萃取温度45℃,分离压力6MPa,萃取时间120min。迷迭香油中鉴定出21种化学组分,占挥发油总量的97.99%。迷迭香挥发油中含量较高的成分是1,8-桉叶素(27.23%)、α-蒎烯(19.43%)、樟脑(14.26%)、莰烯(11.52%)等。结论:超临界CO2萃取迷迭香油具有提取时间短、提取率高等优点;浙江产迷迭香与西班牙型较为接近。     

Aus glycosidischer Bindung freigesetzte und genuin frei vorliegende Komponenten des etherischen Ols von Solanum tuberosum sowie Artefaktbildung bei seiner Gewinnung1

The composition of essential oils of SOLANUM TUBEROSUM obtained by different methods was investigated. It could be shown that the essential oil is mainly composed of sesquiterpenes. The monoterpene linalool was found to be glucosylated.