Effects of Ethanol Condensation Reflux Extraction and Ultrasound-assisted Extraction on the Content of Total Flavonoids of Pueraria edulis

With Pueraria edulis from different habitats in Yunnan Province,Guangdong Province and Guangxi Zhuang autonomous region as materials,the medicinal materials of P.edulis were extracted by ethanol condensation reflux extraction and ultrasound-assisted extraction,and the effects of different extraction methods the contents of total flavonoids in P.edulis from different areas were compared.The results showed that the best extraction time for P.edulis in Yunnan Province was 20 min,and that for Guangdong and Guangxi Zhuang Autonomous Region was 30 min.The yield of total flavonoids from P.edulis extracted by the condensation reflux extraction method was relatively better.The content of total flavonoids in P.edulis in Yunnan was the highest with an average content of 0.2557%,while the average content of total flavonoids in P.edulis in Guangdong was the lowest with an average content of 0.2108%.

Optimization of Ultrasound-assisted Extraction Conditions for Polysaccharides from Pinus tabulaeformis Seed Shells

[Objective] This study aimed to investigate the optimal technological condi- tions for ultrasouqd-assisted extraction of polysaccharides from Pinus tabulaeformis seed shells. [Melhod] Polysaccharides were extracted from P. tabulaeformis seed shells by ultrasound-assisted hot water extraction method and detected by phenol- concentrated sulfuric acid method. The effect of extraction temperature, extraction duration, solid-liquid ratio and extraction frequency on the extraction of polysaccha- rides was investigated using single-factor gradient experiment and the extraction conditions for polysaccharides from P. tabulaeformis seed shells were optimized us- ing L9（34） orthogonal design. [Result] The content of polysaccharides extracted twice at 60 ℃ for 25 min with solid-liquid ratio of 1：3.5 reached the maximum. The re- covery rate （n=-5） ranged from 97.71% to 100.67% and RSD was 1.56%, suggesting high stability. [Conclusion] A simple and efficient method for ultrasound-assisted ex- traction of polysaccharides from P. tabulaeformis seed shells was established in this study, which laid solid foundation for the development and utilization of abandoned pine nut shell resources.

Optimization of ultrasound-assisted extraction of camptothecin from Camptotheca acuminata seeds

Naturally occurring camptothecin（CPT） is an important source of chemotherapeutic agents.The extraction from Camptotheca acuminata is still the main approach to obtain CPT compared with total synthesis.In the present study,ultrasound-assisted extractions（UAE） of CPT from C.acuminata seeds with alkaline solutions were investigated and CPT yield were determined by High Performance Liquid Chromatography.The conditions of alkaline species and concentrations,extraction time,extraction temperature and ultrasonic power were optimized.Results show that both Na3PO4 and Na2CO3 solutions gain good extraction yields,whereas Na3PO4 solution has stronger basicity and need higher concentration than Na2CO3 solution does,thus aqueous Na2CO3 is more beneficial for the extraction.The optimal condition was ultrasonically extracted with 0.5% aqueous Na2CO3 at 50°C and ultrasonic power of 400 W for 60 min.Comparing with UAE with ethanol,the extraction with 0.5% Na2CO3 solution achieves higher yield.Moreover,aqueous Na2CO3 as a solvent has various advantages including non-toxicity,inflammable,non-corrosive and low cost,which ensure this UAE method is a superior method with high utilizing prospect.

Ultrasound-assisted Enzymatic Extraction of SDF on Passion Fruit Seeds

Ultrasound-assisted enzymatic extraction of soluble dietary fiber(SDF) from passion fruit seeds was carried out in order to shorten the extraction time and increase the yield of SDF. The effects of cellulase concentration, ultrasonic power, extraction temperature, solid-liquid ratio and water bath time on the SDF yield of passion fruit were studied by single factor analysis. And the orthogonal experiment was designed to optimize the extraction conditions. The results showed that the optimum conditions for the extraction of SDF from passion fruit by ultrasoundassisted enzymatic method were cellulase concentration 1.5%, ultrasonic power 120 W, solid-liquid ratio(g/mL) 1 ∶ 15, extraction temperature 55 ℃, and water bath time 160 min. The SDF extraction rate was determined to be 5.12%.

Ionic Liquid-Based Ultrasound-Assisted Emulsification Microextraction Coupled with HPLC for Simultaneous Determination of Glucocorticoids and Sex Hormones in Cosmetics

An effective and environmentally friendly method based on ionic liquid-based ultrasound-assisted emulsification microextraction(IL-USAEME) and high performance liquid chromatography (HPLC) has been developed for the determination of nine hormones including three glucocorticoids, one androgen and five progestogens in cosmetics. Several factors that affect the extraction efficiency, such as the kinds and volume of ionic liquid, salt concentration, ultrasonic power and time, and centrifugation time were investigated and optimized. Under the optimum extraction condition, the recoveries of analytes ranged from 85.97% to 108.84% except prednisolone (62.30%). The intraday and interday precision was below 2.51% and 3.30%, respectively.

Pectinmethylesterase extraction from orange solid wastes: Optimization and comparison between conventional and ultrasound-assisted treatments

During orange juice production, a half of fresh oranges weight is considered as production waste (peels, pulp, seeds, orange leaves and damaged orange fruits). An alternative for the management of these wastes is their treatment by addition of lime and a latter pressing, obtaining a press cake and a press liquor rich in sugars (10°Brix) and citric acid, protein, pectin and ethanol. For non-thermal concentration of press liquor to obtain citruss molasses (65°-70°Brix), the removal of pectin is necessary. Traditionally, depectinization of juices has been done by using pectinmethylesterase (PME) enzymes from external sources. In this work it performed the extraction of PME enzymes from orange peels to obtain the optimum extraction conditions. Two different methods of solventextraction were compared (conventional andultrasound-assisted methods). For the conventional extraction experiments, a central composite design with three variables ([NaCl], pH and time) and five replicates of the center point was used. For ultrasound-assisted extraction, experiments were done at pH = 5.5 and [NaCl] = 1.25M), varying extraction time (1-30 min). Response variables were PME activity, protein content and a ratio between them, named PME effectiveness (ηPME). At the same experimental conditions (pH =5.5, [NaCl] = 1.25 M, t = 15 min) it was found that conventional extractions led to slightly better results in terms of ηPME than ultrasound-assisted extraction method.

Effect of Ultrasound-Assisted Extraction of Phenolic Compounds on the Characteristics of Walnut Shells

Walnuts are one of nature’s more waste-heavy products. 67% of the nut is shell and husk, low value by-products that are rich in phenolic compounds. The phenolic compounds extracted from walnut shells are potentially good natural sources of antioxidants for the food and pharmaceutical industries. In this study, phenolic compounds were extracted using an ultrasonic bath, an ultrasonic probe and a standard shaking method. The extraction yield achieved with an ultrasonic probe was 51.2 mg GAE/g DW, two times higher than both the shaking method and the ultrasonic bath method which were 20.6 mg GAE/g DW and 25.8 mg GAE/g DW, respectively. Phenolic extraction was further improved by a size reduction of the walnut shells. The best extraction yield of 52.8 mg GAE/g DW was attained when the particle size was between 45 - 100 mesh. The ultrasonic probe treatment is the best method for extraction of phenolic compounds from walnut shells. Scanning electron microscopy (SEM) imaging indicated that the ultrasonic probe treatment could better rupture the hard structure of the cells, increasing the penetration of solvents and thus the extraction yield.

Analysis of anticancer compound,indole-3-carbinol,in broccoli using a new ultrasound-assisted dispersive-filter extraction method based on poly(deep eutectic solvent)-graphene oxide nanocomposite

Indole-3-carbinol(I3C),an important anticancer compound found in broccoli,has attracted considerable attention.The rapid extraction and accurate analysis of I3C in the pharmaceutical industry in broccoli is challenging as I3C is unstable at low pH and high temperature.In this study,a rapid,accurate,and lowcost ultrasound-assisted dispersive-filter extraction(UADFE)technique based on poly(deep eutectic solvent)-graphene oxide(PDES-GO)adsorbent was developed for the isolation and analysis of I3C in broccoli for the first time.PDES-GO with multiple adsorption interactions and a fast mass transfer rate was synthesized to accelerate adsorption and desorption.UADFE was developed by combining dispersive solid-phase extraction(DSPE)and filter solid-phase extraction(FSPE)to realize rapid extraction and separation.Based on the above two strategies,the proposed PDES-GO-UADFE method coupled with high-performance liquid chromatography(HPLC)allowed the rapid(15-16 min),accurate(84.3%-96.4%),and low-cost(adsorbent:3.00 mg)analysis of I3C in broccoli and was superior to solid-phase extraction,DSPE,and FSPE methods.The proposed method showed remarkable linearity(r=0.9998;range:0.0840-48.0 mg/g),low limit of quantification(0.0840 mg/g),and high precision(relative standard deviation<5.6%).Therefore,the PDES-GO-UADFE-HPLC method shows significant potential in the field of pharmaceutical analysis for the separation and analysis of anti-cancer compounds in complex plant samples.

Ultrasound-Assisted Emulsification Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Droplet for Separation of Trace Gold Prior to Flame Atomic Absorption Spectroscopy Determination

In the present work, a ultrasound-assisted emulsification dispersive liquid-liquid microextraction based on solidification of floating organic droplet method has been developed as a sample preparation method prior to flame atomic absorption spectrometry determination of trace amounts of gold in the standard, wastewater and river water samples. In the proposed method, 1-dodecanol and 5-(4-dimethylamino-benzylidene) were used as extraction solvent and chelating agent, respectively. Several factors that may be affected on the ex-traction process, such as type and volume of the extraction solvent, ionic strength, pH of the aqueous solu-tion, extraction temperature and extraction time were studied and optimized. Under the best experimental conditions, the calibration curve exhibited linearity over the range of 8.0 ng●mL-1- 3.0 μg●mL-1 with a correlation coefficient of 0.9978 and detection limit based on three times the standard deviation of the blank signal was 1.5 ng●mL-1. Eight replicate determinations of 0.2 and 1.0 μg●mL-1 of gold gave a mean absorbance of 0.051 and 0.253 with relative standard deviations of ±2.3% and ±1.5%, respectively. Finally, the developed method was successfully applied to the extraction and determination of gold ions in a silica ore, wastewater, river water and standard samples and satisfactory results were obtained.

超声附加绘图定位甲状腺微小结节在临床中的应用价值研究

目的：分析讨论超声附加绘图定位应用在甲状腺微小结节患者中的临床效果。方法：本组选择2014年5月～2016年5月在沧州中西医医院接受治疗的86例甲状腺微小结节患者，应用病历单双号方法分组，对照组及试验组各43例，对照组行超声检查，试验组行超声附加绘图定位检查，比较两组患者疗效。结果：试验组患者治疗总有效率为97.7%，对照组为76.7%，比较差异有统计学意义（P＜0.05）。结论：超声附加绘图定位可以准确的将甲状腺微小结节切除，降低术后肿瘤残留情况，疗效显著。

Ultrasound-assisted Low Density Solvent Based Dispersive Liquid-liquid Microextraction for Determination of Phthalate Esters in Bottled Water Samples

A technique of ultrasound-assisted low density solvent based dispersive liquid-liquid microextraction was developed for the determination of four phthalate esters, including dimethyl phthalate（DMP）, diethyl phthalate（DEP）, di-n-butyl phthalate（DnBP） and di（2-ethylhexyl） phthalate（DEHP） in bottled water samples. A low density solvent, toluene, was selected as extraction solvent. In the extraction process, a mixture of 15 μL of toluene（extraction solvent） and 100 μL of methanol（disperser solvent） was rapidly injected into 1.0 mL of water samples. A cloudy solution was formed after ultrasounded for 5 min, and then centrifuged at 5000 r/min for 5 min. The enriched analytes in the floa- ting phase were determined by means of gas chromatograph. Under the optimum conditions, the enrichment factors were found to be in a range of 29--67, and the recoveries were ranged from 81.2% to 103.9%. The limits of the detection were in a range of 3.8--5.6 μg/L. The proposed method was applied to the extraction and determination of phthalate esters in bottled water samples, and the concentrations of phthalate esters found in the water samples were below the allowable levels.

Effects of ultrasound on the desulfurization performance of hot coal gas over Zn-Mn-Cu supported on semi-coke sorbent prepared by high-pressure impregnation method

Zn-Mn-Cu/SC（U） sorbent was hydrothermally synthesized by ultrasound-assisted high-pressure impregnation method with semi-coke（SC）as support and the mixed solution of zinc nitrate,manganese nitrate and copper nitrate as active component precursors.The desulfurization performances of hot coal gas on the prepared sorbent at a mid-temperature of 500°C were tested in fixed-bed reactor.Morphology and pore structure of the prepared sorbent were also characterized by TEM,N2adsorption/desorption isotherms and XRD.For comparison,the sorbent of Zn-Mn-Cu/SC prepared by conventional high-pressure impregnation was also evaluated and characterized in order to study the effects of ultrasound treatment.Zn-Mn-Cu/SC（U） sorbent prepared by high-pressure impregnation under ultrasound-assisted condition showed a better desulfurization performance than Zn-Mn-Cu/SC.It could remove H2 S from 1000×10-6m3/m3 to 0.1×10-6m3/m3 at 500°C and maintained for 12.5 h with the sulfur capacity of 7.74%,in which both the breakthrough time and sulfur capacity were about 32% and 51% higher than those of Zn-Mn-Cu/SC sorbent.The introduction of ultrasound during high-pressure impregnation process greatly improved the morphology and pore structure of the sorbent.The ultrasonic treatment made particle size of active components smaller and made them more evenly disperse on semi-coke support,which provided more opportunities to contact with H2S in coal-based gases.However,there were no any difference in compositions and existing forms of active components on the Zn-Mn-Cu/SC and Zn-Mn-Cu/SC（U） sorbents.

Determination of contents of eight alkaloids in fruits of Macleaya cordata (Willd) R. Br. from different habitats and antioxidant activities of extracts

A reliable ultrasound-assisted extraction （UAE） method combined with HPLC-UV for quantification of eight active alkaloids in fruits of Macleaya cordata （Willd） R. Br. was developed. The optimization conditions of UAE were obtained by using Box-Behnken design of response surface methodology. Chromatography was carried out using a Kromasil C18 column by gradient elution with 0.1% phosphoric acid aqueous solution for HPLC-UV. All calibration curves showed good linear correlation coefficients （R^2〉0.999 6） and recoveries （from 97.3% to 104.9%） were acceptable. 1,1-diphenyl-2-picrylhydrazyl （DPPH） method was employed to test the antioxidant activity of the extract from the samples. The proposed method was successfully applied to quantifying eight components in nine samples of M.cordata, and significant variations of alkaloid contents and antioxidant aetivity of the samples from different habitats were demonstrated. It presents a powerful proof for the selection of the best sources to extract eight kinds of alkaloids.

Extraction and Purification Process Optimization and Antioxidant Activity in vitro of Flavonoids in Amaranthus caudatus L.

[Objectives]To explore the optimal extraction and purification process of the flavonoids in Amaranthus caudatus L.and to study the antioxidant activity in vitro of the flavonoids in A.caudatus.[Methods]Taking A.caudatus as the raw material,flavonoids were extracted by alcohol extraction method,and AB-8 macroporous adsorption resin was selected for purification.The hydroxyl radical scavenging ability,DPPH radical scavenging ability,and O^2-radical scavenging ability were used as evaluation indicators,to explore the antioxidant activity in vitro of the flavonoids in A.caudatus.[Results]The optimal extraction process conditions of flavonoids in A.caudatus are:liquid-to-material ratio 40:1,extraction temperature 60℃,ethanol concentration 60%,ultrasonic power 320 W,extraction time 50 min.Under these conditions,the extraction yield of flavonoids in A.caudatus is(1.35±0.01)%.The optimal purification process conditions of flavonoids in A.caudatus are 2.5 g AB-8 macroporous adsorption resin,sample volume 5 mL,mass concentration of adsorption solution 1.60 mg/mL,pH value of adsorption solution 3.0,sample flow rate 3 BV/h,ethanol concentration in desorption process is 70%and the desorption flow rate is 3 BV/h.Under these conditions,the recovery rate reaches 88.35%±0.68%.[Conclusions]A.caudatus has a high content of flavonoids and has excellent free radical scavenging ability in vitro.This study is intended to provide important technical support for the research of flavonoid activity of A.caudatus and the development of functional products.

Optimization of a continuous ultrasound assisted oxidative desulfurization(UAOD) process of diesel using response surface methodology(RSM) considering operating cost

A continuous-flow ultrasound-assisted oxidative desulfurization(UAOD)of partially hydro-treated diesel has been investigated using hydrogen peroxide-formic acid as simple and easy to apply oxidation system.The effects of different operating parameters of oxidation stage including residence time(2–24 min),formic acid to sulfur molar ratio(10–150),and oxidant to sulfur molar ratio(5–35)on the sulfur removal have been studied using response surface methodology(RSM)based on Box–Behnken design.Considering the operating costs of the continuous-flow oxidation stage including chemical and electrical energy consumption,the appropriate values of operating parameters were selected as follows:residence time of 16 min,the formic acid to sulfur molar ratio of 54.47,and the oxidant to sulfur molar ratio of 8.24.In these conditions,the sulfur removal and the volume ratio of the hydrocarbon phase to the aqueous phase were 86.90%and 4.34,respectively.By drastic reduction in the chemical consumption in the oxidation stage,the volume ratio of the hydrocarbon phase to the aqueous phase was increased up to 10.Therefore,the formic acid to sulfur molar ratio and the oxidant to sulfur molar ratio were obtained 23.64 and 3.58,respectively,which lead to sulfur removal of 84.38%with considerable improvements on the operating cost of oxidation stage in comparison with the previous works.

Evaluation of Oil Yield of Oil Shale by Infrared Spectrometry Coupled with Ultrasound-assisted Extraction

The oil yield of oil shale was evaluated by Fourier transform infrared（FTIR） spectrometry coupled with ultrasound-assisted extraction. The extraction conditions, including the amount of sample, extraction time and extrac- tion temperature, were examined and optimized. Twenty-four oil shale samples were collected and divided into calibration set and prediction set randomly with a ratio of 2：1. The oil yields of all the samples were determined by the routine method（low-temperature retorting） for reference. The linear regression（LR） equations of oil yield vs. the total area of the spectrum peaks in a wavenumber range of 3100--2800 cm-1 as well as the sum of absorbance of three absorption peaks（2855, 2927 and 2955 cm-l）, and the multiple linear regression（MLR） model of oil yield vs. the absorbances of the three absorption peaks were constructed with the samples in calibration set and applied to the evaluation of the oil yields of the samples in prediction set, respectively. The results show that the MLR model provides more accurate predictions than the other LR two equations. The determination coefficient（P2p ）, the root- mean-square error of prediction（RMSEP） and the residual prediction deviation（RPD） of the MLR model are 0.9616, 0.6458 and 3.6, respectively. The present method is a rapid and effective alternative to the routine low-temperature retorting method.

The ultra-sonication of minerals in swine feed

A sample preparation method based on ultrasound assisted-extraction （UAE） of Ca, Mg and P from swine feed has been described. The experiment was performed to cover the variables influencing the sonication process and, the method validation using standard reference material. Final solutions obtained upon sonication were analyzed by flame atomic absorption spectrometry （for Ca and Mg） and by UV-vis spectrophotometry （for P）. The best conditions for metal extraction were as follows： sample mass： 100 mg in 20 mL 0.10 mol/L HCI, a particle size： 〈60 lam, sonication time： 5 cycles of 10 s and ultrasound power： 102 W. The UAE method was applied in digestibility assays in different piglet feeds and their results showed that it is highly comparable （P 〉 0.05） to the other methods used for such purposes, as block digestion, and offered a Ca, Mg and P method of quantification limit of 10.6, 12.4 and 14 mg/kg, respectively. The major advantages of the UAE method compared to other methods are the high treatment rate, low reagent usage in the extracts and, it does not generate toxic residues that might negatively affect human health and the environment, accompanied by good precision and accuracy.

Ultrasound-assisted extraction of bound phenolic compounds from the residue of Apocynum venetum tea and their antioxidant activities

Bound phenolic compounds from the residue of Apocynum venetum(A.venetum)tea were released by alkaline digestion with sonication,followed by extraction using ethyl acetate(EtOAc).The fragment ions of compounds in free and bound forms were identified by liquid chromatography electrospray ionization tandem mass spectrometry(LC-ESI-MS/MS)in both positive and negative modes.Further investigation of chemical constituents in the EtOAc extract led to the isolation of eleven individual compounds,and their chemical structures were identified as(−)-epicatechin(1),(−)-loliolide(2),(−)-syringaresinol-4-O-β-D-glucopyranoside(3),alloside of benzyl alcohol(4),3-[(6-O-hexopyranosylhexopyranosyl)oxy]-2-(palmitoyloxy)propyl(9Z,12Z,15Z)-9,12,15-octadecatrienoate(5),apocynoside I(6),quercetin-3-O-β-D-glucopyranoside(7),kaempferol-3-O-β-D-glucopyranoside(8),[1-acetyloxy-3-[3,4,5-trihydroxy-6-[[3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxymethyl]oxan-2-yl]oxypropan-2-yl]hexadecanoate(9),1-stearoyl-2-palmitoyl-sn-glycerol(10),and 3-hexene-l-O-β-D-glucoside(11)using a series of spectroscopic methods.Compounds 2–5 and 9–11 were isolated for the first time from A.venetum,while antioxidant experiments showed that compounds 1,7,and 8 displayed strong DPPH and ABTS+radical scavenging activities.This study represents the first investigation of bound phenolic compounds with potential health benefits in the residue of A.venetum tea.

Determination of Five (5) Possible Contaminants in Recycled Cardboard Packages and Food Simulants Using Ultrasound Assisted Extraction Coupled to GC-MS

A modified analytical procedure has been developed to test for 5 organic pollutants [benzophenone, 2 diisopropylnaphthalenes (DIPNs) {2,6- and 2,7-diisopropylnapthalene} and 2 hydrogenated terphenyls (HTPs) {m-terphenyl and o-terphenyl}] that can be found as residues in recycled cardboards intended for use as food packaging materials and to test for migration levels of these compounds in a food simulant (Tenax). A main objective was to develop a modified rapid and reliable method for the identification and quantification of these compounds at low concentrations. The method was based on ultrasound-assisted solvent extraction (UAE) followed by gas chromatography-mass spectrometry (GC-MS) analysis. The developed method was applied to analyze 3 commercially available recycled carton board food-packaging materials and also to study the potential migration of the 5 organic pollutants from these materials into Tenax to check if these recycled cardboards can be considered as suitable for use in direct contact with foodstuffs. The limits of detection (LODs) of standard solutions of the 5 compounds were determined at a signal-to-noise ratio of 3. The LODs and the limits of quantification (LOQs) of examined pollutants ranged between 0.005 to 0.5 mg/kg, and 0.1 to 1 mg/kg, respectively. The extremely low amounts of most contaminants that migrate from packaging materials to Tenax indicate that the recycled cardboards tested can be safely used for direct food contact applications.

Ultrasound-assisted intensified aqueous extraction of phenolics from waste Syzygium cumini leaves:Kinetic studies and evaluation of antioxidant,antidiabetic and anticancer potential

This is the first report illustrating the extraction of total phenolic compounds(TPC)using the ultrasound-assisted aqueous extraction(USAE)technique from waste Syzygium cumini leaves(WSCL).A kinetic study indicated that Peleg’s model was appropriately fitted to the experimental data when the effect of different parameters was checked on extraction with respect to time.Extraction yields of total phenolic contents(TPC)and total flavonoid contents(TFC)were 78.38 mg GAE/g,and 10.15 mg CE/g,respectively,at optimized parameters of 1:25 WSCL:water,35℃ temperature,134 W power,50%duty cycle and in 9 min of sonication time.Cumulative yields of TPC and TFC obtained by 5 sequential stirred batch extraction were 79.36 mg GAE/g and 10 mg CE/g,respectively.The cost and energy requirement of the USAE process was around 3000 times less than that of the Soxhlet technique.SEM images showed the changes in the morphology of the WSCL surface area before and after ultrasonic extraction.FTIR analysis showed the presence of O-H,N-H,C-H,C=C,and halogenated functional groups.The obtained WSCL extract showed antioxidant potential with an IC_(50) value of 15.64μg/mL.IC_(50) values of extract forα-amylase andα-glucosidase inhibitions were 8.3 and 6.64μg/mL.Antiproliferation activity against breast,cervical,and lung cancer showed the potential with GI50 values 252.8,112.5,and 97.8μg/mL,respectively.Aqueous extract of Syzygium cumini leaves can be used to treat oxidative stress,diabetes,and cancer.