加压微波辅助水解甘草酸粗品制备甘草次酸(英文)

A pressured microwave-assisted hydrolysis(PMAH) technique has been developed for hydrolyzing the crude glycyrrhizic acid(GA) extracted from licorice root to prepare glycyrrhetinic acid(GRA).In order to optimize the efficiency of PMAH,several experimental parameters were investigated,including liquid-solid ratio,hydrolysis time,sulfuric acid concentration and hydrolysis temperature.The optimized hydrolysis conditions were as follows:pressured microwave-assisted hydrolysis of crude GA for 21 min(taking 15 min to reach 150 oC,and holding it for 6 min) at 150 oC(at a radiation power of 450 W) in 3%-5% sulfuric acid solution with the liquid-solid(ml?g?1 crude GA) ratio of 25︰1.As a result of the considerable saving in time and higher product yields(up to 90%),PMAH was proved more effective than conventional methods.     

微波辅助萃取中药刺五加中有效成分的研究

Microwave-assisted extraction (MAE) for active ingredients in Ciwujia was studied by using ethanol as the extractant. Comparing MAE with conventional methods, the former can save the extracting time and increase the content of the active ingredients in product. As to the operation in MAE, the continuous radiation process is more convenient for the extraction for traditional Chinese medicine than the intermittent radiation process. Optimized by uniform design, MAE was proved to be an effective and novel process for extracting active ingredients in Ciwujia. The optimized MAE conditions are as follows: the microwave power is 510W, the radiation time 30min, the alcohol concentration at 80%, the ratio of solvent to solid material being 5:1, the soaking time 0.5h, and the herbal particle size is (520±19)μm.     

Emulsion liquid membrane for selective extraction of Bi(III)

Di(2-ethylhexyl)phosphoric acid was used as extractant of bismuth ions from nitrate medium by emulsion liquid membrane, with Triton X-100 as the biodegradable surfactant in n-pentanol bulk membrane. The novelties and innovative points of this work are the application of emulsion liquid membrane for selective and efficient extraction of bismuth ions as wel as the relevant optimization procedures. The extraction of bismuth ions was evaluated by the yield of extraction. The experimental parameters were evaluated and optimized, including the ratio of di(2-ethylhexyl)phosphoric acid mass concentration to Triton X-100 (1.0%:0.5%), nature of diluent (n-pentanol), nature and concentration of stripping solution (sulfuric acid, 0.5 mol·L?1), stirring speed (1800 r·min?1) and equilibrium time of extraction (20 min), initial feed solution of bismuth (350 mg·L?1) and the volume ratio of internal stripping phase to membrane phase (14). The experimental parameters of kinetic extraction reveal that the bismuth ions can be extracted by 100%.     

Extraction Equilibria of Trimellitic and [ 1,1′-Biphenyl]-2,2′-dicarboxylic Acid with 1-Octanol, 50%TBP,and 10%TRPO in Kerosene

To explore the feasibility of extracting aromatic acid products from oxidizing coal, two aromatic acids, trimellitic and [1,1′-biphenyl]-2,2′-dicarboxylic acid, were selected as the solutes, and the extraction equilibrium of the acids were studied with 1-octanol, 50% tributyl phosphate （TBP） in kerosene, and 10% trialkylphosphine oxide （TRPO） in kerosene. The results showed that the degree of extraction of [1,1′-biphenyl]-2,2′-dicarboxylic acid was larger than that of trimellitic acid for all of the solvent, and the extraction capacity with TRPO is more effective than the one with TBP. The extraction behavior of aromatic polyacid is different from that of carboxylic acid, and the reactive extraction function of aromatic acids with TBP and TRPO is not as effective as that of carboxylic acid. 1-octanol could be used to remove [1,1′-biphenyl]-2,2′-dicarboxylic acid from the mixture of trimellitic acid and [1,1′-biphenyl]-2,2′-dicarboxylic acid. Because the weak hydrogen bond association exists between -OH in 1-octanol and -COOH in aromatic acid, the extractive selectivity of [ 1, 1′-biphenyl]-2,2′-dicarboxylic to trimellitic acid depends on the stoichiometric ratio.     

Enhanced Recovery of Resveratrol and Emodin from Polygonum cuspidatum by a Simultaneous Extraction and Acid Hydrolysis Process

A novel and efficient extraction/hydrolysis method was developed for the recovery of resveratrol and emodin from a well-known traditional chinese medicinal herb, Polygonum cuspidatum. By using a 85% aqueous acetone solution containing 1.0 mol/L HCl as extractant, extraction of resveratrol and emodin from P. cuspidatum and conversion of resveratrol-3-O-β-glucoside and emodin-8-O-β-D-glucoside into the products could be achieved in one step. The effects of several key parameters including concentration of HCl and acetone, temperature, ratio of solvent to material, extraction duration and extraction times on the process efficiency was systematically investigated. The results showed that the optimal conditions for maximizing the recovery yield were 85% acetone containing 1.0 mol/L HCl as extractant, temperature 70 ℃, ratio of liquid to solid 50 mL /g and extraction duration 30 min. This one-pot extraction/hydrolysis process increased the yield of resveratrol and emodin to 524% and 302%, respectively, compared to a raw sample without hydrolysis. Compared with conventional method, the developed process not only achieved high yield of resveratrol and emodin, but simplified the procedures and reduced time. The results demonstrated that the simultaneous extraction/hydrolysis process is simple and efficient which could act as a useful approach for enhanced recovery of resveratrol and emodin from P. cuspidatum.     

亲和胶质气体泡沫的制备及其对胰蛋白酶的吸附分离特性

Triton X-114, an non-ionic surfactant, was modified with the affinity ligand of trypsin, paminobenzamidine (PAB) and the affinity surfactant (PAB-TX) was synthesized. Then, the affinity surfactant was used to prepare affinity-based colloidal gas aphrons (CGA). The stability of the affinity CGA was investigated at different temperatures and compared with that of the CGA prepared from Triton X-114. Compared with the CGA from Triton X-114, the affinity CGA showed high selective adsorption property for trypsin. In the separation of a protein mixture, recovery yield higher than 74% were achieved for trypsin and the separation factor reached over 1.5. The results showed that the affinity CGA possessed promising selectivity for separating trypsin from a protein mixture.     

微波协同萃取射干异黄酮的研究

Microwave-assisted extraction （MAE） of isoflavones from Belamcanda chinensis was studied using ethanol as the solvent. The single factor experiment and the orthogonal method were used to optimize the MAE condition. It was concluded that two doses of intermittent microwave power radiation, 300 W each for 4 rain, were needed for extraction. The mass ratio of solvent to material was 8：1 and the alcohol mass fraction was 80%. The extracted liquor was then concentrated under vacuum and degreased with petroleum ether. The yield of total isofiavones was about 8.8% and the contents of tectoridin and iridin were 67.6% and 16.3% respectively. Compared with direct-heating extraction （DHE）, MAE may shorten extracting duration, reduce solvent consumption, and improve yield and purity of isoflavones from Belamcanda chinensis.     

超临界 CO2萃取辣椒籽油的动力学研究简

A mathematical model for extraction of red pepper seed oil with supercritical CO2 was proposed. Some factors influencing the process were investigated, including operation pressure, temperature and extraction yield Xe （%）. The model was solved by the method of weighted residuals and used to simulate the process numerically. The kinetic equation is expressed as Xe =-16.8606exp（-t/9.98177） ＋ 16.95457 and the simulation results are in excellent agreement with the experimental data. The optimal operating parameters are 30 MPa, 318 K and 60 min.     

Investigation of Three-liquid-phase Extraction Systems for Simultaneous Separation of Emodin and Rhein

Several three-liquid-phase extraction systems comprised of organic extractant,polymer and salt aqueous solution were applied to isolate and purify simulated herbal extract containing emodin and rhein.Some influential factors on the partitioning behaviors were studied.The results revealed that extractant type and solution pH value were crucial factors for improving the separation performance.The optimal separation results were obtained at pH 8.00 with methyl isobutyl ketone as the extractant,10%（ω） polyethylene glycol with the molecular weight 4000 Da,and 10%（ω） ammonium sulphate.Under the optimized conditions,95%emodin and 97%rhein were simultaneously extracted into the organic phase and polymer-rich phase from simulated herbal solution with the initial concentration of 100×l0^-6（ω）,respectively,and their separation factor of over 10000 was achieved.By adjusting pH value,back extraction rate of both emodin and rhein could be up to about 99%.With the assistance of molecular simulation program XLOGP3 and molecular orbital package,the possible mechanism of extraction was analyzed,and hydrophobic interaction and hydrogen-bonding interaction might be the major driving forces affecting the partitioning behaviors of emodin and rhein.     

Static and dynamic studies of adsorption by four macroporous resins to enrich oridonin from Rabdosia rubescens

Oridonin, one of the active ingredients in Rabdosia rubescens(R. rubescens), has been reported to induce cell apoptosis and cell cycle arrest in many cancers. Conventional extraction methods tend to result in unsatisfied enrichment and poor quality of oridonin present in a given biomass. This paper aims to evaluate the performance and separation characteristics of four different macroporous resins to arrive at the most suitable methodology for the isolation and purification of high-quality oridonin. Static absorption kinetics, thermodynamic and dynamic adsorption were evaluated. HP-20 was selected for further study due to its high adsorption capacity of 32 mg·g~(-1) and desorption ratio with 98.5%. The pseudo-secondorder model was considered to be the most suitable for kinetic results, and Langmuir model was chosen to better describe the absorption thermodynamics. Under optimum conditions(flow rate of 4 ml·min~(-1),bed depth with 6 cm and initial concentration of 2.15 mg·min~(-1)), the effective content of oridonin increased from 33.9% to 79.1% in the dry extract with a recovery of 81% and the purity of oridonin improved from 76% to 93%. The results confirm that HP-20 provides an efficient method to purify most oridonin from R. rubescens.     

Micelle-Mediated Extraction and Cloud Point Preconcentration of Chlorophylls from Spinach

A micelle-mediated extraction and cloud point preconcentration of chlorophylls method was developed. Non-ionic surfactant (Genapol X-080) was employed as an alternative and effective extraction solvent. The optimal extraction parameters based on the micelle extraction technique were determined. Under optimal conditions, i.e., 5% Genapol X-080 (v/v), pH 9.0, liquid/solid ratio of 10:1 (mL g^?1), ultrasonic-assisted extraction for 30 min, extraction amount reached the highest value. For the preconcentration of chlorophylls by cloud point extraction (CPE), the solution was incubated at 50° for 30 min, and 0.1 g mL^?1 sodium chloride was added to the solution to facilitate the phase separation. The microstructure of coacervate phase after CPE was explored with transmitting electron microscopy. The preconcentration factor for chlorophylls was about 12.5, the extraction recovery approached 99.2%, and the loading capacity was about 1 mg mL^?1. Thus coupling of ultrasonic-assisted micelle extraction and cloud point extraction could be employed as a new and effective technique for the rapid extraction and preconcentration of chlorophylls from plants such as spinach.     

Separation of Liquiritin from Glycyrrhizic Acid in Licorice Root Extract by Nanofiltration Membrane

The aim of this work was to study the separation of liquiritin (LQ) from glycyrrhizic acid (GA), in licorice aqueous solutions using nanofiltration (NRT-7450) membrane. The LQ and GA components are the main active ingredients of licorice root extract with various pharmacological effects, The effects of transmembrane pressure, feed temperature, feed pH, and cross-flow velocity on permeate flux and recovery were determined. A lab scale cross-flow set up using flat-sheet configuration membrane was employed for all experiments. SEM micrographs showed the changes in the fouled surface during operating time. The applied transmembrane pressure, feed temperature, feed pH, and cross-flow velocity were varied from 4 to 10 bars, 30 to 40°C, 3 to 9, and 0.8 to 3.1 m s^?1 respectively. The obtained recoveries for GA and LQ varied between 0.65 to 1.86% and 16.89 to 41.65%, respectively. The optimum operating conditions for separation LQ from GA in licorice aqueous solutions using NRT-7450 nanofiltration membrane were 1.8 m s^?1cross-flow velocity, 8 bars transmembrane pressure, 40°C of feed temperature and pH 7.     

Cloud Point Extraction of Glycyrrhizic Acid from Licorice Root

Abstract

An attempt has been made to extract glycyrrhizic acid (GA) from licorice root by surfactant mediated cloud point extraction (CPE) using non‐ionic surfactant (Triton X‐100). Almost all of the GA molecules were concentrated in the surfactant‐rich phase (also called coacervate phase) after phase separation. The pH is the most critical factor regulating the distribution of GA in the micelle which related to the ionization form. The other effects of the concentration of GA and the surfactant, the temperature, and the salt concentration on the extraction efficiency of GA in the coacervate phase and aqueous phase have been studied. The mechanism of CPE of GA was explored with transmitting electron microscopy. It was deduced that aggregate GA molecules were adsorbed on micelles' outer poler mantle and inner cross‐linked micelles at high GA concentrations in coacervate phase.     

Simultaneous recovery of glycyrrhizic acid and liquiritin from Chinese licorice root (Glycyrrhiza uralensis Fisch) by aqueous two-phase system and evaluation biological activities of extracts

Aqueous two-phase system (ATPS) was used for simultaneous purification of glycyrrhizic acid (GA) and liquiritin (LQ) from crude extract of Chinese licorice root. It was revealed that 87% GA and 94% LQ were retrieved in the ATPS top phase, under the optimum conditions of 25% (w/w) ethanol, 30% (w/w) K₂HPO₄ and 4% (w/w) loading sample at 10–40°C. Compared with crude extract, the ATPS top-phase extract exhibited the highest antioxidative activity, but no tyrosinase inhibitory effect. Whereas, the ATPS bottom-phase extract was proved to be effective ABTS radical scavenger and tyrosinase inhibitor, suggesting the potency of the alcohol-salt ATPS purification for the different medicinal purposes.     

Use of micellar extraction and cloud point preconcentration for valorization of saponins from sisal (Agave sisalana) waste

Sisal (Agave sisalana) is the main hard fiber produced worldwide, with an estimated generation of 400 thousands t in 2011. From its leaves, only the hard fibers, which represent 3–5% of their weight, are removed. The remaining 95–97% is referred to as sisal waste and contains steroidal saponins that can be potentially used in foods, cosmetics and pharmaceuticals formulations, as well as for soil bioremediation. The present work aimed at to evaluate strategies for the extraction and concentration of saponins from sisal waste, focused on the use of clean solvents, such as water and ethanol. For this purpose, it was firstly performed a central composite rotatable design for the optimization of the extraction conditions followed by a comparison of this strategy with other methods (Soxhlet, ultrasound-assisted extraction and micellar extraction). Cloud point preconcentration was then tested, using several types and concentrations of salts. The use of orbital shaker extraction (200 rpm) with an ethanolic solution (30%, v/v) at 50 °C, a mass/volume ratio sisal/solvent of 0.17 (g/mL) for 4 h allowed a recovery of 38.6% of the saponins. When a micellar extraction strategy using 7.5% (v/v) of Triton X-100, under the above-mentioned conditions was performed, saponins recovery raised to 98.4%. In a subsequent step, the addition of 20% (m/v) sodium carbonate led to a preconcentration factor of 20.3. The best adsorbent for Triton removal from the preconcentrated solution was Amberlite FPX-66. The process strategy proposed in the present study showed to be efficient for saponins extraction and preconcentration from a low-cost, highly available agricultural waste.     

浊点萃取-火焰原子吸收光谱法测定水样中的微量钴

文章研究了浊点萃取-火焰原子吸收光谱法测定微量钴。以8-羟基喹啉（8-HQ）作为钴的络合剂,以Triton X-100为表面活性剂进行浊点萃取。探讨了影响浊点萃取的因素,如溶液的pH,络合剂的浓度,表面括性剂的浓度,缓冲溶液的浓度,加入表面活性剂后的平衡温度和时间。该方法具有低毒,高效,安全,简便等特点,并用于自来水、湖水、江水、雨水中微量钴的溯定,其富集率最高可达100％,回收率在90％～100％之间,方法可行。     

浊点萃取-紫外可见光谱法测定痕量钴

研究了浊点萃取(CPE)-紫外可见光谱法(UV/Vis)测定微量钴的新方法,利用表面活性剂聚乙二醇辛基苯基醚(TritonX-100)和配合剂2[(5-溴-2-吡啶)-偶氮]-5-(二乙氨基)苯酚(5Br-PADAP)对试样中的钴(Ⅱ)进行浊点萃取。探讨了影响浊点萃取及测定灵敏度的因素。在最佳条件下,钴的富集倍率为5,检出限为1.18ng/mL(n=11),RSD为2.8%(n=5,c(Co2+)=0.20μg/mL),钴含量在(0.01～0.5)μg/mL范围内服从比尔定律。本法对实际样品中的钴进行富集和测定,结果令人满意。     

浊点萃取-192紫外可见分光光度法测定痕量铝

研究了浊点萃取(CPE)-紫外可见分光光度法测定痕量铝离子的新方法,利用非离子表面活性剂Triton X-114对铝试剂与铝离子形成的络合物进行浊点萃取。探讨了影响浊点萃取及测定灵敏度的因素。在最佳条件下,铝离子的富集倍率为13.5倍,检出限为0.33μg/L,RSD为0.2%(n=6),铝离子含量在10~150μg/L范围内服从比尔定律。本法对实际样品中的铝进行富集和测定,结果令人满意。     

林檎叶防腐保鲜成分微波提取工艺的优化研究

在林檎叶天然防腐保鲜成分微波辅助浸提工艺中通过均匀试验设计构建模型,运用Excel中回归分析工具得到回归方程。试验中所选因素对微波辅助提取的影响顺序为:微波功率>液料比>浸提次数>微波时间。确定林檎叶防腐保鲜成分提取最优工艺条件为:微波时间1min,微波功率700W,液料比61.62∶1,浸提次数3.51。对林檎叶防腐保鲜成分中的活性成分进行化学定性分析,其中含有黄酮类化合物、多元酚类及皂甙等活性物质。