共查询到19条相似文献,搜索用时 109 毫秒
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以姜科类植物草豆蔻中山姜素为模拟对象, 基于微波辅助萃取(MAE)过程中微波场、 温度场及浓度场等物理场之间的耦合关系, 利用Comsol软件构建了MAE多物理场耦合模型. 模拟了不同萃取时间、 微波功率下萃取体系的电磁场分布、 温度分布以及山姜素扩散分布; 通过比较萃取液温度和山姜素浓度的模拟值与实验值, 结合误差分析对模型进行了验证, 以同类植物砂仁中的异槲皮苷为萃取目标验证了模型的适用性. 结果表明, 微波功率越大, 电磁场强度越强, 萃取液温度越高, 山姜素扩散越明显, 越有利于萃取; MAE萃取山姜素和异槲皮苷的萃取液温度模拟值与实验值之间的相对均方根误差(RRMSE)分别在1.9%~4.5%和1.9%~2.8%之间, 其浓度RRMSE分别在1.7%~3.2%及1.6%~4.1%之间, 均小于5.0%, 表明建立的模型准确、 可靠, 且适用性良好. 该模型综合考虑了MAE过程中的多个物理场及其耦合关系, 可为深入研究其萃取机理提供参考. 相似文献
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密闭系统中微波辅助萃取机制探讨 总被引:11,自引:2,他引:9
通过与普通加热萃取虎杖中白藜芦醇的产率进行对比 ,对密闭系统中微波辅助萃取的机理进行了探讨。结果表明 ,微波辅助萃取与普通加热萃取二者的活化能相差不大 ,分别为30.06和30.32kJ·mol-1。但微波辅助萃取的表观速率常数约是普通加热萃取的20倍。并且还利用电子扫描显微镜对样品微结构进行了观察 ,研究表明 ,细胞内极性成分如水吸收了微波能后压力迅速增加导致细胞结构的破坏是MAE快速高效的关键 ,由于细胞的破坏 ,萃取剂和萃取目标化合物更容易通过细胞壁 ,加速了扩散速度 ,进而加速了萃取速度。 相似文献
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土壤中痕量水胺硫磷的微波辅助萃取-固相微萃取-GC-MS法测定 总被引:5,自引:2,他引:5
研究了微波辅助萃取(MAE)-固相微萃取(SPME)联合萃取、气相色谱-质谱法(GC-MS)测定土壤中水胺硫磷的分析方法;采用正交设计试验优化了微波升温程序、萃取温度、萃取时间、萃取溶剂体积等MAE条件;研究了SPME萃取涂层、萃取时间、解吸温度等对萃取效率的影响;方法的线性范围在1.O~20μg/L之间,检出限为O.49ng/g;测定25、100ng/g加标土壤样品,回收率分别为79%和107%。RSD分别为2.6%和6.5%;方法综合了MAE快速高效和SPME富集浓缩的优点,以水为萃取溶剂,特别适合于固体样品中痕量有机物的分析。 相似文献
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何首乌中磷脂类化合物的微波辅助萃取/高效液相色谱法测定 总被引:1,自引:0,他引:1
利用微波辅助萃取(MAE)技术对何首乌中磷脂类化合物的萃取条件进行研究,并通过液相色谱法分离测定.通过对MAE影响因素的考察,确定萃取溶剂为氯仿-甲醇(体积比1 : 2)的混合溶剂,固液比为1 : 20,萃取时间15 min,温度45 ℃.在HPLC中,采用Nucleosil 100-5硅胶色谱柱(250 mm×4.6 mm i.d. ,5 μm),甲醇为流动相,流速0.8 mL/min,进样量15 μL,蒸发光散射检测器. 相似文献
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微波辅助萃取-分散固相萃取-气相色谱质谱法测定茶叶中23种农药残留 总被引:1,自引:0,他引:1
建立了微波辅助萃取-分散固相萃取净化-气相色谱质谱法(GC-MS)快速测定茶叶中23种农药残留量的方法. 茶叶样品用乙腈进行微波辅助萃取(MAE),提取液经分散固相萃取(DSPE)净化处理. 采用DB-17MS毛细管色谱柱分离后,选择离子监测模式下(SIM)质谱法进行测定. 23种农药组分在0.01~0.50 mg/mL质量浓度范围内呈线性关系,相关系数r2大于0.995,方法测定低限(10S/N)为0.005~0.01 mg/kg. 以空白绿茶为基体,在4个标准添加水平0.01、0.05、0.10、0.25 mg/kg进行加标回收试验,加标平均回收率为70%~105%,相对标准偏差为3.0%~8.2%. 相似文献
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Microwave-assisted extraction (MAE) for the separation of atrazine, simazine and prometryne from synthetic soil samples, using water and some organic solvents as the extractants, was studied in detail. The effects of the soil matrix, the soil moisture and the pH of the aqueous extraction system on the MAE efficiency were also studied. It was found that the three triazines could be efficiently extracted under the conditions of 100% magnetron power output (600 W), the first grade of pressure (from 0.1 MPa to 0.5 MPa), 30 ml solvent and 4 min microwave heating with water or organic solvents, except for prometryne with dichloromethane solvent for 1-4 g sandy loam sample. This interesting result was explained by triazines' solubility in water, their sorption properties in soils and the ability of the solvent to absorb microwave energy. Finally, evaluation of the extraction efficiency, as well as the treatment and determination of MAE extracts, suggested that water, as a cheap, safe and environmentally friendly solvent, can be a good alternative to organic solvents, used as the extractants for MAE of triazines from soils. 相似文献
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A microwave assisted extraction (MAE) procedure was first developed for the simultaneous determination of isoflavonoids and astragalosides in Radix Astragali (RA). MAE showed the highest extraction efficiency when compared to Soxhlet, reflux, and ultrasonic extraction. It was found that flavonoid glycoside malonates were converted into their related glycosides during the prolonged conventional extraction, thus affecting the reproducibility. However, the conversion was inhibited when using MAE. After being optimized in terms of solvents, microwave power, and irradiation time, MAE was used for the simultaneous determination of isoflavonoids and astragalosides in RA with HPLC-UV-evaporative light scattering detection (ELSD). Our results indicated that extraction by MAE was more effective than by other conventional techniques. Moreover, the MAE method followed by HPLC-UV-ELSD determination was a simple, rapid, and reliable method for the quality assessment of RA. 相似文献
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Ionic liquids based extraction method has been applied to the effective extraction of norstictic acid, a common depsidone isolated from Pertusaria pseudocorallina, a crustose lichen. Five 1-alkyl-3-methylimidazolium ionic liquids (ILs) differing in composition of alkyl chain and anion were investigated for extraction efficiency. The extraction amount of norstictic acid was determined after recovery on HPTLC with a spectrophotodensitometer. The proposed approaches (IL-MAE and IL-heat extraction (IL-HE)) have been evaluated in comparison with usual solvents such as tetrahydrofuran in heat-reflux extraction and microwave-assisted extraction (MAE). The results indicated that both the characteristics of the alkyl chain and anion influenced the extraction of polyphenolic compounds. The sulfate-based ILs [C(1)mim][MSO(4)] and [C(2)mim][ESO(4)] presented the best extraction efficiency of norstictic acid. The reduction of the extraction times between HE and MAE (2 h-5 min) and a non-negligible ratio of norstictic acid in total extract (28%) supports the suitability of the proposed method. This approach was successfully applied to obtain additional compounds from other crustose lichens (Pertusaria amara and Ochrolechia parella). 相似文献
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《Comptes Rendus Chimie》2016,19(6):692-698
This research paper presents a quick and ecofriendly technique for the extraction of harpagoside (HS), the active marker of Harpagophytum procumbens (HP), along with a comparison with conventional methods so as to propose an efficient HPLC method. HP is widely used as an anti-inflammatory in phytotherapy. The quality control of the herbal drug and extract calls for a time consuming method of conventional extraction, which involves a high consumption of solvents. In this study, HP has been extracted using conventional ultrasound (UAE) and microwave (MAE)-assisted methods. The effects have been examined based on several parameters of HS extraction efficiencies. An HPLC method with a core-shell column was developed in order to calculate the HS in HP. The flow rate was reduced by 4. The method of validation used is specific, linear, precise and accurate. MAE and UAE saved solvent consumption, time and energy. It has, therefore, been found that the combined UAE-HPLC process is convenient and appropriate for the quality control of HP. 相似文献
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Valentin A. Semenov Dmitry O. Samultsev Leonid B. Krivdin 《Magnetic resonance in chemistry : MRC》2014,52(11):686-693
The calculation of 15N NMR chemical shifts of 27 azoles and azines in 10 different solvents each has been carried out at the gauge including atomic orbitals density functional theory level in gas phase and applying the integral equation formalism polarizable continuum model (IEF‐PCM) and supermolecule solvation models to account for solvent effects. In the calculation of 15N NMR, chemical shifts of the nitrogen‐containing heterocycles dissolved in nonpolar and polar aprotic solvents, taking into account solvent effect is sufficient within the IEF‐PCM scheme, whereas for polar protic solvents with large dielectric constants, the use of supermolecule solvation model is recommended. A good agreement between calculated 460 values of 15N NMR chemical shifts and experiment is found with the IEF‐PCM scheme characterized by MAE of 7.1 ppm in the range of more than 300 ppm (about 2%). The best result is achieved with the supermolecule solvation model performing slightly better (MAE 6.5 ppm). Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
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《Comptes Rendus Chimie》2016,19(6):699-706
Ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) are currently amongst the foremost green techniques for accelerating extraction processes. Several methods for the efficient recovery of the phenolic compounds from rosemary leaves have so far been proposed, but little data are available on the use of UAE and MAE. The aim of this work is to investigate the efficiency and selectivity of these techniques in recovering fractions of specific phenolic compounds from dried rosemary leaves using solvents that are suitable for food applications. UAE has been carried out by means of a probe system equipped with a titanium horn working at 19.5 kHz (140 W). MAE has been performed in a closed multimode reactor under N2 (20 bar) at 100 °C. All obtained extracts were dissolved in a defined solvent volume and the solutions were directly analyzed using a combination of the HPLC-DAD-MS and TOF techniques. MAE and UAE in ethanol and acetone dramatically increased phenol yield (more than three times) as compared to more traditional solid–liquid extraction processes. In terms of selectivity, remarkably high rosmarinic acid content (6.8% of the dried extract) was obtained in ethanol under ultrasound (US). Even more impressive is the selectivity of UAE in n-hexane which gave the highest carnosic acid content, up to 13% of the dried extract. In conclusion, non-conventional energy sources and, in particular, high-intensity US have proven themselves to be rapid, efficient, and selective techniques for rosemary leaf extraction and provide fractions with high rosmarinic and carnosic acid contents. 相似文献
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Lucia Sanchez-Prado Carmen Garcia-JaresMaria Llompart 《Journal of chromatography. A》2010,1217(16):2390-2414
Flame retardants, surfactants, pharmaceutical and personal care products, among other compounds, have been the object of numerous environmental studies. In this chapter, the application of microwave-assisted extraction (MAE) in the development of analytical methods for several groups of organic compounds with growing concern as emerging pollutants has been considered. Compared to other extraction techniques, optimization of MAE experimental conditions is rather easy owing to the low number of influential parameters (i.e. matrix moisture, nature of the solvent, time, power, and temperature in closed vessels). The great reduction in the extraction time and solvent consumption, as well as the possibility of performing multiple extractions, increasing the sample throughput, can also be highlighted among MAE advantages. In summary, the study of several applications of MAE to environmental problems demonstrates that this technique constitutes a good alternative for the determination of organic compounds in environmental samples. It can be used as a rapid screening tool, and also to obtain detailed information on the sources, behaviour and fate of emerging pollutants in environmental matrices. 相似文献
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Akikazu Matsumoto Ryuji Kotaki Takayuki Otsu 《Journal of polymer science. Part A, Polymer chemistry》1991,29(12):1707-1715
Bulk polymerization of alkyl N,N-dialkylfumaramates (FAE) and maleamates (MAE) was performed in the presence of a radical initiator. It has been found that FAE is more reactive than MAE when the reactivity of the two geometrical isomers was compared for their homo- and copolymerizations. From investigation on the effect of ester and N-substituents of these monomers, it has been found that the isopropyl ester shows a higher reactivity than the methyl ester and that N-ethyl and n-butyl substitution gives polymers with high molecular weight of more than several thousands. The resulting substituted polymethylenes from FAE and MAE were characterized and compared with each other. The isomerization of MAE to FAE with morpholine as an isomerization catalyst and monomer-isomerization radical polymerization were also investigated. 相似文献