超临界CO2流体萃取法与水蒸气蒸馏法提取黑松松塔挥发油化学成分的研究

目的比较两种不同提取方法所得的黑松松塔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)提取黑松松塔的挥发油。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。结果超临界CO2流体萃取法提取的挥发油共鉴定出43种成分,占挥发油总成分的60.78%;水蒸气蒸馏法提取的挥发油共鉴定出37种成分,占挥发油总成分的86.16%;结论采用两种方法提取黑松松塔挥发油组分与含量差别较大,且SFE法的提取率低于SD法。     

固相微萃取法与水蒸气蒸馏法提取蜘蛛香挥发油成分的比较

目的:比较固相微萃取法与水蒸气蒸馏法提取蜘蛛香挥发油成分的差异。方法:采用气相色谱-质谱联用技术分别对水蒸气蒸馏法和固相微萃取法提取蜘蛛香根茎所得挥发油的化学成分进行比较分析。结果:2种提取方法所得挥发油成分差异较大。与水蒸气蒸馏法比较,固相微萃取法所得挥发油成分数目和种类较多。结论:固相微萃取法比水蒸气蒸馏法具有明显的优越性。     

白头翁挥发油化学成分研究

目的研究白头翁挥发油的化学成分。方法应用水蒸气蒸馏、超声两种方法,提取挥发油,运用GC-MS技术,结合计算机检索鉴定其化学成分,并计算出各组分的相对含量。结果从水蒸气蒸馏提取挥发油中鉴定了33个组分,从乙醚超声提取挥发油中鉴定了35个组分。结论烷烃分别占水蒸气蒸馏法和乙醚超声法挥发油的66.15%和42.87%,两种方法提取的挥发油含有15种相同的成分。     

GC-MS分析不同水蒸气蒸馏法提取的莲子心挥发油成分

目的分析比较不同水蒸气蒸馏法所得莲子心的挥发油成分。方法分别采用水蒸气蒸馏装置（SDA）和挥发油测定装置（EODA）的水蒸气蒸馏法提取莲子心挥发油,GC-MS分离鉴定挥发油成分,峰面积归一化法计算百分含量。结果采用SDA法,鉴定出29种成分,占挥发油总量91.56%,主要成分为棕榈酸（28.96%）、9,17-十八碳二烯醛（19.99%）和亚油酸（11.94%）等;采用EODA法,鉴定出18种成分,占挥发油总量77.96%,主要成分为棕榈酸（18.98%）、肉桂酸龙脑酯（12.58%）、2-甲氧基-4-乙烯苯酚（8.25%）等。结论两种水蒸气蒸馏法所得挥发油成分存在较大差异,且SDA较EODA更适合于提取挥发油。     

GC-MS分析不同水蒸气蒸馏法提取的莲子心挥发油成分

目的 分析比较不同水蒸气蒸馏法所得莲子心的挥发油成分。方法 分别采用水蒸气蒸馏装置(SDA)和挥发油测定装置(EODA)的水蒸气蒸馏法提取莲子心挥发油,GC-MS分离鉴定挥发油成分,峰面积归一化法计算百分含量。结果 采用SDA法,鉴定出29种成分,占挥发油总量91.56%,主要成分为棕榈酸(28.96%)、9,17-十八碳二烯醛(19.99%)和亚油酸(11.94%)等;采用EODA法,鉴定出18种成分, 占挥发油总量77.96%,主要成分为棕榈酸(18.98%)、肉桂酸龙脑酯(12.58%)、2-甲氧基-4-乙烯苯酚(8.25%)等。结论 两种水蒸气蒸馏法所得挥发油成分存在较大差异,且SDA较EODA更适合于提取挥发油。     

HPLC和GC-MS检测两种提取法所得当归挥发油的化学成分

目的 比较两种提取方法所得挥发油的化学成分.方法 当归药材用水蒸气蒸馏和石油醚提取,用HPLC和GC-MS两种方法比较提取物.结果 HPLC和GC-MS分析当归两种提取方法所得两种挥发油,分别占100%、50%和34%、43%.石油醚法所得苯酞类化合物的种类比水蒸气蒸馏法的多.后者提取的为小分子易挥发的烯萜类成分,与文献报道相同.石油醚法收率是水蒸气蒸馏提取的2.5倍.结论 两种提取法所得挥发油化学成分有差异,石油醚提取当归挥发油较好.     

超临界二氧化碳流体萃取法与水蒸气蒸馏法提取广西产五月艾挥发油化学成分

目的分析广西产五月艾挥发油的主要化学成分。方法分别采用超临界二氧化碳（CO2）流体萃取法和水蒸气蒸馏法提取广西产五月艾挥发油,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。结果超临界CO2流体萃取法提取的挥发油共鉴定出30种成分,占挥发油总成分的77.69 %;水蒸气蒸馏法提取的挥发油共鉴定出48种成分,占挥发油总成分的86.54 %。结论两种提取方法得到的五月艾挥发油组分与含量差别较大。     

三种不同方法提取金线莲挥发油的效果比较研究

目的 比较三种不同方法索氏提取法、水蒸气蒸馏法与微波辅助萃取法提取金线莲挥发油的提取率.方法 采用索氏提取法、水蒸气蒸馏法与微波辅助萃取法提取金线莲的挥发油,并对各种方法的提取条件进行优化,以最佳条件下挥发油提取率为考察指标,确定最佳提取方法.结果 索氏提取法和水蒸气蒸馏法所得挥发油提取率相差不大,微波辅助萃取法提取率最高为0.06233%.结论 微波辅助萃取法提取金线莲挥发油的提取率最高,可用于金线莲挥发油的提取.     

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。     

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。     

Microwave-assisted hydrodistillation extraction based on microwave-assisted preparation of deep eutectic solvents coupled with GC-MS for analysis of essential oils from clove buds

In recent years, deep eutectic solvents (DESs) as green and sustainable solvents have been widely used in the effective extraction of natural products. Usually, DESs are synthesized by heating and stirring method which takes a long time and energy. In this case, a microwave assisted preparation technique was used to form DESs for saving time and energy. And the DESs as pretreatment solvents were combined with microwave-assisted hydrodistillation (MAHD) for the extraction of essential oils (EOs) from the clove buds in this work. The maximum essential oils yield of 4.60% was obtained with the microwave power of 600 W, the pretreatment time of 5 min and the hydrodistillation time of 40 min using a deep eutectic solvent composed of choline chloride and lactic acid (molar ratio with 1:2). In addition, the essential oil was analyzed by gas chromatography-mass spectrometry (GC-MS), a total of 40 compounds were identified. Compared with MAHD, water-based MAHD and traditional hydrodistillation (HD), the content and composition of essential oil extracted by DES-based MAHD were higher. Thus, the combination of deep eutectic solvents with a microwave-assisted technique in this study provided an eco-friendly way of extracting essential oils.     

Comparison of Microwave-Assisted Hydrodistillation and Hydrodistillation Methods for the Analysis of Volatile Secondary Metabolites

Abstract

Microwave-assisted hydrodistillation (MWHD) and hydrodistillation (HD) were carried out for the analysis of volatile components in whole and ground fruits of Anethum graveolens. L. (dill seed) and Coriandrum sativum. L. (coriander seed). Fruits were distilled using a microwave oven modified to fit a Clevenger apparatus. The effect of microwave energy on the yield and composition of the essential oil was investigated against the classical hydrodistillation. Essential oils of all samples were analyzed by GC-FID and gas chromatography-mass spectrometry (GC-MS). In the whole dillseed oil, the amounts of cis.-isodihydrocarvone (from 7.5% to 10.9%) and carvone (from 45.7% to 69.3%) were increased by microwave energy while limonene (from 17.7% to 4.7%), myristicin (from 8.7% to 5.7%) and dill apiole (from 14.1% to 6.1%) were decreased. Grinding of the material also increased the amounts of main components except for myristicin and dill apiole. A decrease in the linalool content of the coriander oil (from 80.0% to 75.5%) was observed in the microwave-assisted hydrodistilled ground fruits. Microwave-assisted distillation appeared to increase the amounts of fatty acids, for example, tetradecanoic acid (from 2.8% to 8.8%) and hexadecanoic acid (from 1.9% to 6.0%) in coriander oil.     

Sweet bay (Laurus nobilis L.) essential oil and its chemical composition,antioxidant activity and leaf micromorphology under different extraction methods

This research explored the essential oil (EO) of Laurus nobilis. Various parameters were recorded, including the amount of yield, chemical composition and antioxidant activity. The EO was obtained by hydro-distillation (HD), hydro-steam distillation (HSD), microwave-assisted hydrodistillation (MAHD), and ohmic-assisted hydrodistillation (OAHD). The micromorphology of the plant leaves were studied under the different extraction methods. The yields of EOs obtained by the mentioned extraction methods were 1.40, 0.74, 1.00 and 0.83 (% w/w), respectively. The main chemical components in EOs obtained by these methods were eucalyptol (34.4–50.0%), α-terpinenyl acetate (14.9–18.8%), terpinene-4-ol (4.7–6.0%) and sabinene (4.9–5.9%). Two of the extraction methods, i.e. OAHD and MAHD, yielded EOs that contained higher proportions of eucalyptol. SEM images of the leaves were taken after extraction. It was observed that the MAHD method had the most destructive effect on secretory cells, while the HSD method failed to damage numerous cells in the leaves. Generally, the results suggest that MAHD and OAHD can be recognized as clean and faster methods because of their shorter processing time and less energy requirements. The HD and HSD methods extracted EOs with more sesquiterpenes, while the MAHD and OAHD methods yielded higher amounts of oxygenated monoterpenes in the EO.     

Extraction of essential oils from damask rose using green and conventional techniques: Microwave and ohmic assisted hydrodistillation versus hydrodistillation

Damask rose is cultivated as the main species used in the production of rose water and relevant essential oils (EOs) of rose for its fragrance and therapeutic applications. Since the flowers are highly perishable, the extraction of oil should be done rapidly in order to produce rose EO successfully and optimally. Solvent free microwave-assisted extraction (SFME) and ohmic assisted hydrodistillation (OAHD) are advanced and green distillation techniques, which utilize microwave, and ohmic heating processes respectively for the extraction of EOs. In this study, SFME and OAHD of EOs were performed on fresh flowers of damask rose, and the findings were compared with the traditional hydrodistillation (HD). The findings of EO analysis indicated considerable alterations in EOs compounds extracted by SFME and OAHD methods compared with the traditional HD. To reach the desirable temperature of extraction (nearly 100 °C) and to get the first EO droplets’ evaporation with steam, the mixture was heated for 2.50 ± 0.29 min in SFME and for 17.33 ± 0.33 min in OAHD, while for the HD the heating had to take more than 40 min (42.66 ± 0.32 min). The total extraction time of EOs extracted from damask rose by using the green extraction procedures (SFME and OAHD) were compared with HD extraction method. Extraction by SFME occurred much earlier than extraction by OAHD. Also in this study, the analysis of EOs indicated that the chemical profile of damask rose may fluctuate quantitatively with respect to the constituents and structure of the extracted molecules. This would depend on the system of extraction that influences the characteristics of the EOs.     

兴安白芷的挥发油成分分析

目的:研究兴安白芷(Angelica dahurica Benth.et Hook.f.ex Franch.et Sav.的干燥根)挥发油的化学成分,并分析其与祁白芷挥发油成分之间的异同。方法:采用水蒸气蒸馏法提取挥发油,采用毛细管气相色谱-质谱联用技术分析其挥发油成分。结果:从兴安白芷挥发油中检出244个色谱峰,鉴定了76个化合物,占挥发油总量的86.13%。挥发油主要成分为十四烷醇(tetradecanol,19.43%)、α-柠檬烯(α-limonene,15.25%)、3-蒈烯(3-carene,10.94%)、正十二烷醇(1-dodecanol,5.74%)和1R-α-蒎烯(1R-α-pinene,3.85%)。结论:兴安白芷和祁白芷共有成分有38个,占兴安白芷挥发油总量的34.54%,其倍半萜及其衍生物类成分的数目和含量要远远低于祁白芷。     

Hydro-distillation and microwave-assisted distillation of Sideritis raeseri: Comparison of the composition of the essential oil,hydrolat and residual water extract

Sideritis raeseri is widely used as a tea in the traditional medicine of many Mediterranean, Balkan, and Middle East countries. In this study, microwave-assisted hydro-distillation (MAHD) at different power levels (180 W, 360 W, and 600 W) of Sideritis raeseri essential oil was compared in terms of extraction time, yield, qualitative analysis, and operational cost with the conventional method of hydro-distillation (HD). Obtained essential oil, as well as hydrolats and residual water extracts, were chemically characterized. An extraction time of 16–32 min with MAHD at different powers provided yields of 0.61–0.67%, while HD gave 0.01% after 141 min. The main constituents in all essential oils were oxygenated sesquiterpenes, and their content was higher in MAHD (32.93–51.42%) than in oil from HD (17.62%). HD oil was characterized by higher concentration of oxygenated monoterpenes (14.95%) in relation to MAHD oil (8.87–14.16%). The essential oil obtained by MAHD at 600 W has a higher content of diterpenes (13.26%) than HD oil (8.59%). All hydrolats displayed the highest content of oxygenated monoterpenes. The highest contents of 8-hydroxyflavone 7-allosylglucosides compounds in residual water extracts were obtained by applying higher (600 W) microwave power. MAHD could be selected as a more appropriate extraction technique for S. reaseri essential oil than HD with respect to the extraction time, quality, and energy savings above 99%.     

Variations in chemical compositions of essential oil from sour orange (Citrus aurantium L.) blossoms by different isolation methods

The main goal of this research was to study the impact of different extraction methods on the yield and chemical compositions of essential oil (EO) obtained from sour orange blossoms. Seven different methods were used for the purpose of extracting the EOs, namely, commercial hydrodistillation (CoM), hydrodistillation (HD), steam distillation (SD), Ohmic-assisted hydro distillation (OAHD), solvent-less microwave extraction (SLME), solvent-free microwave extraction (SFME), and microwave-assisted hydrodistillation (MAHD). The isolated EOs were analyzed by GC and GC-MS in three replications. The highest EO yield in relation to the extraction time was obtained by the HD method (0.34%) and the lowest one (0.04%) was detected by the SD method. The main compounds and their ranges of concentration in the EOs were as follows: linalool acetate (12.2 ± 0.08–28.9 ± 0.2) %, linalool (22.9 ± 0.07–54. ± 0.2) %, Farnesol (0.2 ± 0.04–10.4 ± 0.07) %, E-nerolidol (0.4 ± 0.1–21.4 ± 0.04) % and geranyl acetate (0.97 ± 0.05–9.3 ± 0.08)%. Moreover, SLME caused a selective extraction of E-nerolidol (21.42%) and farnesol (10.45%). The SFME resulted in a two-fold extraction of linalool (54.08%), compared to the COM which yielded an amount of 22.9%. Significant changes in the amounts of limonene (1?14) % and β-pinene (0–9.6)% were also observed by the extraction methods. Overall, the results suggest that MAHD and SFME can be termed as green technologies because of their less energy requirements and less carbon dioxide emissions. Their high-quality EO and cost effective performance for EO extraction can be of importance to pharmaceutical industries.     

Investigation of the volatile fraction of rosemary infusion extracts

The relative proportions of chemical classes (hydrocarbons, oxides, alcohols, ketones, esters) in the essential oil of rosemary (Rosmarinus officinalis L., Lamicaeae) and in the volatile fraction of the infusion extracts were examined and showed remarkable differences.The volatile compounds of the infusion were isolated by two different methods, hydrodistillation and solid phase extraction (SPE). The main constituents of the volatile fraction of the infusion were (hydrodistillation/SPE): 1,8-cineole (42.4%/44.7%), camphor (31.4%/31.8%), α-terpineol (8.6%/8.1%) and borneol (8.3%/7.8%). The qualitative and quantitative composition of the volatile compounds of the infusion was compared to the essential oil isolated by hydrodistillation directly from the leaves. The major constituents of the essential oil of the leaves were 1,8-cineole (41.6%), camphor (17.0%), α-pinene (9.9%), α-terpineol (4.9%) and borneol (4.8%). Comparison of the total essential oil yield quantified by hydrodistillation of the infusion (0.36% v/w) with the essential oil yield of the leaves (1.84% v/w) revealed that only 19.6% of the initial oil could be extracted by infusion.     

Optimization and comparison of three methods for extraction of volatile compounds from Cyperus rotundus evaluated by gas chromatography-mass spectrometry

The essential oil of Cyperus rotundus has multiple pharmacological activities. Therefore, the extraction with high yield and quality is very important for preparation of essential oil of C. rotundus. In this paper, three methods, namely hydrodistillation (HD), pressurized liquid extraction (PLE) and supercritical fluid extraction (SFE), for extraction of volatile compounds from C. rotundus were optimized and compared by gas chromatography-mass spectrometry. Among eight identified compounds in C. rotundus, five components including alpha-copaene, cyperene, beta-selinene, beta-cyperone and alpha-cyperone were quantitatively determined or estimated using alpha-cyperone as standard, which showed that PLE had the highest extraction efficiency, while SFE had the best selectivity for extraction of beta-cyperone and alpha-cyperone. The contents of ingredients from C. rotundus extracted with HD, PLE and SFE are significantly different, which suggest that comparison of chemical components and pharmacological activities of different extracts is helpful to elucidate the active components in C. rotundus and control its quality.     

Distribution of Volatiles in Artemisia cana.

Abstract

The chemical composition of essential oils isolated from aerial parts of wild sage, Artemisia cana. Pursh (Asteraceae), was investigated. Analyses were performed by GC and GC/MS using two columns of different polarities, polyethylene glycol (DB-Wax) and 5% phenyl 95% polydimethylsiloxane (HP-5), which enabled the separation of several co-eluting components. Up to 2.3% of oil (w/w, dry basis) was obtained by hydrodistillation of aerial parts, excluding leafless woody stalks. The stalks of Artemisia. species contained insignificant amounts of essential oils. Flowers, leaves, and stalks yielded 2.8%, 2.4%, and 0.1% of oil, respectively. A total of 34 components were identified accounting for 92.6–87.6% of the oils. The chemical composition of the oils extracted from different plant parts was very similar. High contents of 1,8-cineole (20.8–11.0%) and camphor (55.2–37.4%) were found in Artemisia cana. oils. For pilot-scale testing purposes, aerial parts were separated from leafless woody stalks and processed in a 10L DIG-Maz extractor. The chemical composition of the recovered product was similar to that of the lab-distilled oil. The oil was characterized by a light yellow to green liquid with an herbaceous, balsamic, and fresh-camphoraceous odor.