Comparison of hydrodistillation and ultrasonic solvent extraction for the isolation of volatile compounds from two unifloral honeys of Robinia pseudoacacia L. and Castanea sativa L

A comparative study of ultrasound-assisted extraction (USE) with the mixture pentane:ether (1:2) and hydrodistillation (HD) with the same trapping mixture is presented for the isolation of volatile compounds from two unifloral honeys of Robinia pseudoacacia L. and Castanea sativa L. All HD isolates contained many thermally derived artefacts (especially phenylacetaldehyde with lower percentages of furfural, cis- and trans-linalool oxides and others). USE method gave the most representative profile of all honey volatiles (without artefacts). In addition, USE enabled extraction of low molecular weight semivolatile markers (especially benzoic, vanillic and phenylacetic acids) that were not extracted by HD. In this regard, low percentage of benzoic acid (0.7–7.4%), vanillic acid (0.0–1.6%) and phenylacetic acid (0.5–4.1%) was determined in Rp USE extracts, while Cs USE extracts contained phenylacetic acid (20.2–23.5%) as the major constituent with low percentage of benzoic acid (2.5–5.5%).     

Analysis of pesticide multi-residues in leafy vegetables by ultrasonic solvent extraction and liquid chromatography-tandem mass spectrometry

Ultrasonic solvent extraction (USE) of pesticide multi-residues including monocrotophos, dimethoate, imidacloprid, carbendazim, carbaryl and simazine from leafy vegetables is presented. The extraction procedure was optimized with regard to the solvent type and amount, sonication time and number of extraction steps. The extract did not need clean-up before injected into liquid chromatography-tandem mass spectrometry (LC-MS-MS) which was employed together with electron microscope to verify the effect of USE method. The proposed procedure allows the extraction of six pesticide residues in a single step with 40 ml of ethyl acetate for 35 min sonication, providing recovery over 83% and LOQ less than 1.4 microg/kg. The optimized USE method is a simple, low cost and an effective preparation method for determination of pesticide multi-residues at trace levels in leafy vegetables in comparison with homogenized extraction method.     

Shock wave-assisted extraction of phenolic acids and flavonoids from Eysenhardtia polystachya heartwood: A novel method and its comparison with conventional methodologies

Phenolic compounds, obtained from plants are important in the food, biomaterial and pharmaceutical industries; however current extraction methods, such as Soxhlet (solid-liquid) extraction, liquid-liquid extraction, microwave-assisted extraction, and ultrasonic extraction (USE), have the disadvantages of large processing times, contamination by solvents, and degradation of analytes. This study demonstrates that shock wave-assisted extraction can be used as a more efficient, eco-friendly and rapid method. Extraction of powdered samples of Eysenhardtia polystachia heartwood, a plant with high concentration of phenolic compounds, exposed to different doses of underwater shock waves, was compared with the conventional methods. Our results revealed that shock wave-assisted extraction (1500 shock waves with a peak positive pressure of approximately 88 MPa) produced 34.54% and 31.95% higher contents than Soxhlet and USE, respectively. Extraction times using shock waves were much shorter than with all other methods tested, proving that it is an attractive method to obtain both phenolic acids and flavonoids without the need for organic solvents. Furthermore, shock waves produced a significantly higher content of total reducing sugars than Soxhlet extraction and less phenolic acids which gives the insight of a more selective extraction of components.     

顶空固相微萃取-气相色谱-质谱联用分析马蹄香中的挥发油成分

利用顶空固相微萃取-气相色谱-质谱联用技术分析马蹄香挥发油的化学成分,为马蹄香的挥发油成分分析提供新方法。以顶空固相微萃取法提取挥发油,气相色谱-质谱联用技术对挥发油成分进行分离鉴定,并采用面积归一化法确定各成分的相对质量分数。结果样品在90℃下平衡30min,顶空吸附15min的条件下,采用100μm PDMS纤维头能有效地吸附马蹄香挥发油成分。气相色谱-质谱联用技术共鉴定出57个成分,其中相对质量分数较高的有西车烯(15.93%)、1,2,3,5,6,7,8,8a-八氢-1,4-二甲基-7-(1-甲基乙烯基)甘菊蓝(13.55%)、α-广藿香烯(9.50%)等。马蹄香挥发油具有丰富的化学成分,顶空固相微萃取-气相色谱-质谱联用能全面快速地获得其组成信息,可应用于马蹄香挥发油成分的研究。     

Components of supercritical extracts of garlic and synthetic nonsymmetrical allyl disulfides as potential antimicrobial preparations

Extracts of garlic (Allium sativum L.) were obtained using supercritical carbon dioxide extraction and were separated into individual compounds using preparative high performance liquid and gas chromatography. A series of nonsymmetrical allyl disulfides with different substituents were synthesized. The compounds isolated from the supercritical garlic extract and the synthetic nonsymmetrical allyl disulfides (SNA) were tested as potential antimicrobial agents using a number of test objects: Candida utilis, Bacillus cereus, Pseudomonas aurantiaca, and Escherichia coli. It was shown that the SNA exhibit high antimicrobial activity, which was much higher that the activities of individual components of garlic and in some cases were comparable in efficiency with antibiotics of the floxacin series widely used in clinical practice. The data obtained suggest the potential for using SNA as antimicrobial agents.     

东北苍耳子挥发油化学成分分析

利用乙醚抽提东北苍耳子挥发油,GC-MS结合计算机检索对其化学成分进行分析鉴定,用色谱峰面积归一化法计算各组分的相对含量.分离出89个组分,鉴定了其中74个组分,占总挥发油量的85.63%.东北苍耳子挥发油的主要成分为3-甲基丁酸(16.421%)、3-甲基-戊酸(15.882%)、苯乙醛(11.281%)、已酸(5.051%)、糠醛(4.716%)、苯甲醇(2.358%)、苯乙醇(2.282%)等.     

气相色谱-质谱法研究香稻品种白香糯化学成分

本文采用同时蒸馏－萃取法（Ｓｉｍｕｌｔａｎｅｏｕｓ Ｄｉｔｉｌｌａｔｉｏｎｓ－Ｅｘｔｒａｃｔｉｏｎ,ＳＤＥ）提取了香稻品种－白香糯的挥发性香味成分,采用气相色谱－质谱（ＧＣ／ＭＳ）联用技术鉴定了白香糯的２３种非酸性香气成分。对其中最重要的香气成分２－乙酰基－２－吡咯啉进行了定量测定。     

New insights into the mechanisms of ultrasonic emulsification in the oil–water system and the role of gas bubbles

Ultrasonic emulsification (USE) assisted by cavitation is an effective method to produce emulsion droplets. However, the role of gas bubbles in the USE process still remains unclear. Hence, in the present paper, high-speed camera observations of bubble evolution and emulsion droplets formation in oil and water were used to capture in real-time the emulsification process, while experiments with different gas concentrations were carried out to investigate the effect of gas bubbles on droplet size. The results show that at the interface of oil and water, gas bubbles with a radius larger than the resonance radius collapse and sink into the water phase, inducing (oil–water) blended liquid jets across bubbles to generate oil-in-water-in-oil (O/W/O) and water-in-oil (W/O) droplets in the oil phase and oil-in-water (O/W) droplets in the water phase, respectively. Gas bubbles with a radius smaller than the resonance radius at the interface always move towards the oil phase, accompanied with the generation of water droplets in the oil phase. In the oil phase, gas bubbles, which can attract bubbles nearby the interface, migrate to the interface of oil and water due to acoustic streaming, and generate numerous droplets. As for the gas bubbles in the water phase, those can break neighboring droplets into numerous finer ones during bubble oscillation. With the increase in gas content, more bubbles undergo chaotic oscillation, leading to smaller and more stable emulsion droplets, which explains the beneficial role of gas bubbles in USE. Violently oscillating microbubbles are, therefore, found to be the governing cavitation regime for emulsification process. These results provide new insights to the mechanisms of gas bubbles in oil–water emulsions, which may be useful towards the optimization of USE process in industry.     

Ultrasonic-assisted extraction,fatty acids identification of the seeds oil and isolation of chemical constituent from oil residue of Belamcanda chinensis

Belamcanda chinensis is a common garden herb. The extraction technology of B. chinensis seed oil (BSO) was optimized by ultrasonic-assisted extraction (UAE) method, the composition, relative content of main fatty acids and physicochemical properties of BSO were determined, and the isolation, identification and determination of chemical constituent in BSO residue (BSOR) were also investigated. The optimum process conditions of BSO by UAE were optimized as ultrasound time 14 min, extraction temperature 42℃, the ultrasound power 413 W and the liquid–solid ratio 27:1 mL/g. Under this condition, the extraction yield was 22.32 % with the high contents of linoleic acid and oleic acid in BSO. Ten compounds were isolated and identified from BSOR, and belamcandaoid P (9) was a new compound. The contents of the determined compounds were all at high level in B. chinensis seed. The study provided a certain scientific reference for the comprehensive development and utilization of B. chinensis seeds.     

Bio-refinery of orange peels waste: A new concept based on integrated green and solvent free extraction processes using ultrasound and microwave techniques to obtain essential oil,polyphenols and pectin

In this study, extraction of essential oil, polyphenols and pectin from orange peel has been optimized using microwave and ultrasound technology without adding any solvent but only “in situ” water which was recycled and used as solvent. The essential oil extraction performed by Microwave Hydrodiffusion and Gravity (MHG) was optimized and compared to steam distillation extraction (SD). No significant changes in yield were noticed: 4.22 ± 0.03% and 4.16 ± 0.05% for MHG and SD, respectively. After extraction of essential oil, residual water of plant obtained after MHG extraction was used as solvent for polyphenols and pectin extraction from MHG residues. Polyphenols extraction was performed by ultrasound-assisted extraction (UAE) and conventional extraction (CE). Response surface methodology (RSM) using central composite designs (CCD) approach was launched to investigate the influence of process variables on the ultrasound-assisted extraction (UAE). The statistical analysis revealed that the optimized conditions of ultrasound power and temperature were 0.956 W/cm² and 59.83 °C giving a polyphenol yield of 50.02 mg GA/100 g dm. Compared with the conventional extraction (CE), the UAE gave an increase of 30% in TPC yield. Pectin was extracted by conventional and microwave assisted extraction. This technique gives a maximal yield of 24.2% for microwave power of 500 W in only 3 min whereas conventional extraction gives 18.32% in 120 min. Combination of microwave, ultrasound and the recycled “in situ” water of citrus peels allow us to obtain high added values compounds in shorter time and managed to make a closed loop using only natural resources provided by the plant which makes the whole process intensified in term of time and energy saving, cleanliness and reduced waste water.