Continuous subcritical water extraction of medicinal plant essential oil: comparison with conventional techniques

A subcritical extractor equipped with a three-way inlet valve and an on/off outlet valve has been used for performing subcritical water extractions (SWE) in a continuous manner for the isolation of the essential oil of fennel, a medicinal plant. The target compounds were removed from the aqueous extract by a single extraction with 5 ml hexane, determined by gas-chromatography-flame ionization (GC-FID) and identified by mass spectrometry (MS). The proposed extraction method has been compared with both hydrodistillation and dichloromethane manual extraction. Better results have been obtained with the proposed method in terms of rapidity, efficiency, cleanliness and possibility of manipulating the composition of the extract.     

Eco-friendly and cleaner process for isolation of essential oil using microwave energy: Experimental and theoretical study

Microwave steam diffusion (MSD) was developed as a cleaner and new process design and operation for isolation of essentials oils and was compared to conventional steam diffusion (SD). The essential oils extracted by MSD for 3 min were quantitatively (yield) and qualitatively (aromatic profile) similar to those obtained by conventional steam diffusion for 20 min. In addition, an optimal operating steam flow rate of 25 g min⁻¹ and microwave power 200 W were found to ensure complete extraction yield with reduced extraction time. To confirm the efficiency of this process a mathematical model was proposed to describe the mass transfer of essential oil from lavender. Solid-steam mass transfer coefficients obtained by MSD were six times higher than obtained by SD. Scanning electronic microscopy was used to confirm the extraction mechanism of the essential oil present in the glandular trichomes of the flowers from lavender outer surface. MSD was better than SD in terms of energy saving, cleanliness and reduced waste water.     

Headspace single drop microextraction coupled with microwave extraction of essential oil from plant materials

Headspace single drop microextraction (HS-SDME) coupled with microwave extraction (ME) was developed and applied to the extraction of the essential oil from dried Syzygium aromaticum (L.) Merr. et Perry and Cuminum cyminum L. The operational parameters, such as microdrop volume, microwave absorption medium (MAM), extraction time, and microwave power were optimized. Ten microliters of decane was used as the microextraction solvent. Ionic liquid and carbonyl iron powder were used as MAM. The extraction time was less than 7 min at the microwave power of 440 W. The proposed method was compared with hydrodistillation (HD). There were no obvious differences in the constituents of essential oils obtained by the two methods.     

SPE isolation of low‐molecular oxygen compounds from essential oils

Analytical procedures of complex mixtures frequently involve their initial pre‐fractionation to make the analysis easier or possible. Recently, SPE is frequently applied for this purpose. This article discusses the possibility of essential oil's fractionation using SPE with octadecyl modified silica. The presented results show that developed SPE with C‐18 sorbent allows for easy and total isolation (100% recovery) of low‐molecular oxygen compounds from the remaining compounds, for which the recovery exceeds 95%. The obtained recoveries are satisfactory for preliminary separation of essential oils for analytical and preparative purposes.     

Ionic‐liquid‐assisted microwave distillation coupled with headspace single‐drop microextraction followed by GC–MS for the rapid analysis of essential oil in Dryopteris fragrans

A rapid, green and effective miniaturized sample preparation technique, ionic‐liquid‐assisted microwave distillation coupled with headspace single‐drop microextraction was developed for the extraction of essential oil from dried Dryopteris fragrans. 1‐Ethyl‐3‐methylimidazolium acetate was the optimal ionic liquid as the destruction agent of plant cell walls and microwave absorption was medium. n‐Heptadecane (2.0 μL) was adopted as the suspended microdrop solvent in the headspace for the extraction and concentration of essential oil. The optimal parameters of the proposed method were an irradiation power of 300 W, sample mass of 0.9 g, mass ratio of ionic liquids to sample of 2.8, extraction temperature of 79°C, and extraction time of 3.6 min. In comparison to the previous reports, the proposed technique could equally monitor all the essential oil components with no significant differences in a simple way, which was more rapid and required a much lower amount of sample.     

A surprising method for green extraction of essential oil from dry spices: Microwave dry-diffusion and gravity

Without adding any solvent or water, we proposed a novel and green approach for the extraction of secondary metabolites from dried plant materials. This "solvent, water and vapor free" approach based on a simple principle involves the application of microwave irradiation and earth gravity to extract the essential oil from dried caraway seeds. Microwave dry-diffusion and gravity (MDG) has been compared with a conventional technique, hydrodistillation (HD), for the extraction of essential oil from dried caraway seeds. Essential oils isolated by MDG were quantitatively (yield) and qualitatively (aromatic profile) similar to those obtained by HD, but MDG was better than HD in terms of rapidity (45min versus 300min), energy saving, and cleanliness. The present apparatus permits fast and efficient extraction, reduces waste, avoids water and solvent consumption, and allows substantial energy savings.     

超临界萃取川芎精油的GC-MS分析

不同压力和温度条件下超临界萃取所得川芎精油的收率不同,通过气相色谱-质谱联用对精油的挥发性成分进行分析,结果表明不同条件下超临界萃取所得川芎精油的主要挥发性成分相似,但其质量分数有一些差别.     

Optimization of microwave-assisted hydro-distillation essential oil extracted from Rumex Crispus leaves using definitive screening design

Conversion of nonfood natural products to value-added products is an important work, which is going on worldwide. In addition, to obtain a product with better quality, a sufficient separation method is helpful to improve its utilization value by using effective, rapid and environmentally friendly techniques. Thus in this work, the microwave-assisted hydrodistillation (MAHD) process of essential oils from important natural plant Rumex Crispus leaves was investigated. The experimental design and extraction conditions were optimized using a definitive screening design. The yield of essential oils of 4.67 ± 0.02 % was investigated under the optimum conditions; 534.89 W of microwave power, 23.48 min of hydrodistillation time and 4.5 mL/g of the volume of water to plant mass ratio. Under these conditions, the essential oils were analyzed using gas chromatography-mass spectrometry (GC–MS). Results revealed that the essential oil extracted by MAHD possessed high quality as proved by its higher percentage of oxygenated compounds. In addition, α-santol (29.63 %) and β-santol (25.60 %) are the primary components of oxygenated compounds in essential oils. In conclusion, the MAHD was successfully employed to obtain mainly Oxygenated compounds-rich essential oil that may be used in several industrial applications. Subsequently, a definitive screening design may be regarded as an alternative and reliable method for the prediction of experimental parameters. It was concluded that the weeds plant (Rumex Crispus) contains a reliable quantity of oils that is extremely feasible to use and recommended as good feedstock for possible use in industrial applications.     

Microwave extraction of essential oils from dried fruits of Illicium verum Hook. f. and Cuminum cyminum L. using ionic liquid as the microwave absorption medium

Ionic liquid was used as microwave absorption medium and applied to the extraction of essential oils from dried fruits of the Illicium verum Hook. f. and Cuminum cyminum L. by microwave‐assisted extraction. The extraction time is less than 15 min at the microwave power of 440 W. The constituents of essential oils obtained by the proposed method were compared with those obtained by hydrodistillation. There is no obvious difference in the constituents of essential oils obtained by the two methods.     

Rapid analysis of the essential oils from dried Illicium verum Hook. f. and Zingiber officinale Rosc. by improved solvent-free microwave extraction with three types of microwave-absorption medium

A new method of extracting essential oils from dried plant materials has been studied. By adding a microwave-absorption medium (MAM) to a reactor, solvent-free microwave extraction (SFME) was improved and can be used to extract essential oils from dried plant material without pretreatment. With a microwave irradiation power of 85 W it took only approximately 30 min to extract the essential oils completely. The whole extraction process is simple, rapid, and economical. Three types of MAM, iron carbonyl powder (ICP), graphite powder (GP), and activated carbon powder (ACP), and two types of dried plant material, Illicium verum Hook. f. and Zingiber officinale Rosc., were studied. The results were compared with those obtained by use of conventional SFME, microwave-assisted hydrodistillation (MAHD), and conventional hydrodistillation (HD), and the conclusion drawn was that improved SFME was a feasible means of extracting essential oils from dried plant materials, because there were few differences between the composition of the essential oils extracted by improved SFME and by the other methods.     

Analysis of bitter essential oils from orange and grapefruit by high-performance liquid chromatography with microbore columns

The analysis of bitter orange and grapefruit essential oils (non-volatile fraction) was carried out by HPLC in normal- and reversed-phase mode with UV detection. These oils were compared with the sweet orange and mandarin essential oils, analyzed previously. For the identification of chromatographic peaks, fractionation by RP-HPLC was carried out. The purified fractions were analyzed by GC-MS and LC-MS. Some new compounds were found, together with many others already identified in different citrus essential oils.     

Comparative study of chemical composition,antibacterial and antioxidant activity of essential oils isolated from the seeds of Amomum subulatum by using microwave extraction and hydro-distillation methods

Microwave assisted hydro-distillation (MAHD) and conventional hydro-distillation (HD) techniques were compared in the extraction of essential oils from Amomum subulatum seeds. The time required for MAHD method (70 ​min) is lesser than that for HD method (4 ​h). There is a slight increase in the yield of extracted oil in MAHD method (3.35%) compared to HD (3%). Gas chromatography–mass spectrometry GC-MS results show that MAHD extracted essential oil was wealthier in oxygenated compounds. 1, 8-Cineole was found to be a major compound in case of both the essential oil, followed by α-pinene. In MAHD the percentage of the major oxygenated monoterpene (1, 8- cineol) slightly increases from 88% to 89% as compared to hydrodistillation. Contrarily to this, the percentage of monoterpene hydrocarbon was decreased in MAHD than HD extracted oil. MAHD and HD extracted oils show good antibacterial activities against gram-negative and gram-positive bacteria. MAHD extracted oil shows better antibacterial activity than HD extracted against both gram positive and gram-negative bacteria. 2, 2-diphenyl-1-picrylhydrazyl (DPPH•) radical scavenging antioxidant activities show that MAHD extract has better inhibition percentage than HD extract, and the half-maximal inhibitory concentration IC50 value of MAHD was less than HD extracted oil.     

微波消解-水杨基荧光酮光度法测定中草药中痕量锗

在H3PO4介质中,以水杨基荧光酮为显色剂,以吐温-80为表面活性剂,研究了微波消解部分清热解毒类中草药中痕量锗的测定条件.水杨基荧光酮与锗(Ⅳ)的配合物的最大吸收峰为506 nm,表观摩尔吸光系数为ε=1.54×105 L·mol-1·cm-1,回归方程A=0.0409ρ 0.00614,相关系数 r=0.9999,检出极限为0.014 μg/mL.     

A comparison between different techniques for the isolation of rosemary essential oil

Traditional hydrodistillation (HD), supercritical fluid extraction (SFE), organic solvent extraction (SE), and water microwave assisted hydrodistillation (MAHD) techniques were compared and evaluated for their effectiveness in the isolation of rosemary essential oil. The microwave assisted hydrodistillation technique was optimized in terms of both delivered power and time duration. The extracts/distillates were analyzed by GC and GC-MS. Microwave distillation, which exploits the physical action of microwaves on plants, showed a series of advantages over the other approaches: low cost, use of water in sample pre-treatment step, greatly reduced isolation time, and attainment of high quality essential oil distillate. Moreover, the absence of environmental impact of this innovative technique was also emphasized.     

Microwave accelerated steam distillation of essential oil from lavender: A rapid, clean and environmentally friendly approach

A new process design and operation for microwave accelerated steam distillation (MASD) of essential oils was developed. A packed bed of lavender flowers (Lavandula angustifolia Mill., Lamiaceae) sits above the steam source generated by microwave heating. Only steam passes through it without the boiling water mixing with vegetable raw material, as is the case in hydro-distillation. MASD has been compared with a conventional technique, steam distillation (SD), for the extraction of essential oil from lavender flowers. Extraction of essential oils from lavender with MASD was better than SD in terms of energy saving, rapidity (10 min versus 90 min), product yield, cleanliness and product quality.     

Optimization of microwave-assisted extraction for alizarin and purpurin in Rubiaceae plants and its comparison with conventional extraction methods

A simple and rapid microwave-assisted extraction (MAE) procedure was developed and optimized for two common color pigments, alizarin and purpurin, in various samples of Rubiaceae plants. Several variables that can potentially affect the extraction efficiency, namely temperature, methanol concentration in the extractant mixture, time, and solvent volume were optimized by means of a central composite design approach. The results suggest that temperature and methanol concentration in the solvent mixture are statistically the most significant factors. The separation and quantitative determination of the pigments was carried out in less than 6 min by a developed high-performance liquid chromatographic method with UV detection at 250 nm. Under optimum operating conditions, MAE showed significantly higher recoveries than those obtained by the conventional extraction methods (ultrasonic and reflux extraction), ranging from 84 to 94%. In addition, a drastic reduction of the extraction time (20 min versus 6 h) and solvent consumption (20 versus 100 mL) was achieved with a reproducibility (RSDs < 10%) comparable with that provided by the reflux extraction as a reference method.     

萃取淫羊藿挥发油的实验与分析

报道了用正交实验法研究超临界萃取淫羊藿挥发性成分的条件;结果显示最佳萃取条件为萃取压力30 MPa,萃取温度40℃,萃取时间1 h。按对结果影响大小依次排列为:萃取压力→萃取温度→萃取时间,在最佳条件下萃取挥发油,收率为2.7%;并用气相色谱-质谱联用技术分析了淫羊藿挥发油的化学成分,从中确认出43种化学成分,用峰面积归一化法通过化学工作站数据处理系统得出各化学成分在挥发油中的质量分数;其中主要成分为薄荷醇、1,2-二甲氧基-4-(2-丙烯基)-苯、5-(1-丙烯基)-1,3-苯并间二氧杂环戊烯、3,5-二甲氧基-甲苯、冰片、十五(碳)烷、1,2,3-三甲氧基-5-甲苯、外-葑醇、2,6,6-三甲基-2,4-环庚二烯-1-酮、2-莰酮等。     

Focused microwave aqueous extraction of chlorophenols from solid matrices and their analysis by chromatographic techniques

Open-vessel focused microwave (FMW) extraction with a purely aqueous carbonate solution was used for the extraction of chlorophenols from various solid matrices. After SPE on C18-bonded silica, the analytes were determined as such by LC-UV or, as their acetyl derivatives, by GC-ECD. The FMW aqueous extraction is efficient and rapid and no organic solvents are used. PCP was detected in several solid samples, with recoveries of 101-115% (RSD, 2-4%) relative to Soxhlet extraction. Similar recoveries were obtained for the other chlorophenols for spiked samples.     

One-pot polyamidation reaction of optically active aromatic diacid containing methionine and phthalimide moieties with aromatic diamines under microwave irradiation and traditional heating

An optically active diacid containing phthalimide and l-methionine moiety was prepared in three steps, and was polymerized with several aromatic diamines to obtain a new series of optically active polyamides (PAs) through direct polyamidation using triphenyl phosphite/pyridine/N-methyl-2-pyrrolidone/CaCl₂ system as condensing agent. The polymerization reactions were carried out under both conventional heating and microwave-assisted irradiation. The data obtained by these methods indicate that, high yields and similar inherent viscosities are resulted. It is worth to mention that in the case of microwave conditions, a drastic decrease in reaction time (3 min vs. 5 h) and cleaner reaction have been achieved. These polymers are readily soluble in polar organic solvents such as N,N-dimethyacetamide, N,N-dimethyformamide, dimethyl sulfoxide. The obtained polymers were characterized by FT-IR, specific rotation measurements, elemental analysis and ¹H NMR techniques. The thermal stability of the resulting PAs were evaluated with thermogravimetric analysis and differential scanning calorimetry techniques under a nitrogen atmosphere which indicate they are moderately stable.     

Ultrasound and microwave-assisted extraction of metals from sediment: a comparison with the BCR procedure

In this paper we investigate alternatives to mechanical stirring for the extraction of the mobile fraction of metals from sediment, and analyze whether these techniques can reduce extraction time and improve reproducibility. We compare the quantities of metal extracted from BCR601 and BCR701 certified sediments using ultrasound bath, microwave-assisted extraction and the first step in the certified BCR sequential extraction procedure. Some environmentally important not-certified metals such as As, Mn, Co, Fe and Al have been included in this study. In the case of microwave-assisted extraction, we compare tests in which samples are exposed to constant, low power irradiation with tests using pulsed high power.

In the tests using the ultrasound bath, less metal was extracted than with the other extractive techniques and standard deviations were comparable to those obtained with the BCR procedure; in assays using microwaves at constant power, extraction efficiencies were different for different metals and for different reference materials and, in some cases, standard deviations were higher than those for the reference method. In contrast, tests with microwaves and constant temperature produced encouraging results: R.S.D.s lay in the 2–4% range, both for certified and not-certified metals; these values are very low compared to those for the reference method. Extraction efficiencies for certified metals were close to 100% for Cd, Zn, Cu and Ni and around 80% for Pb and Cr.