响应面法优化超声辅助提取-原子荧光法快速测定茶叶痕量汞

研究了一种使用超声波辅助提取(UAE)-原子荧光法测定茶叶痕量汞的快速方法.采用Plackett-Burman设计从6个影响汞提取率的因素中筛选出3个显著因素—超声时间St,超声温度T和HNO3:H2O2(1:1,δ)体积A2,并采用中心组合设计和响应面法优化参数.结果表明,最优提取条件为,浸泡时间6 min,St 8...     

Optimization of the ultrasound-assisted synthesis of allyl 1-naphthyl ether using response surface methodology

Allyl 1-naphthyl ethers are useful compounds for different purposes, but reported methods to synthesize them require long reaction times. In this work, we have obtained allyl 1-naphthyl ether in good yield using ultrasonic-assisted methodology in a 1-h reaction. A central composite design was used to obtain a statistical model and a response surface (p<0.05; R(2)=0.970; R(2)(adj)=0.949; R(2)(pred)=0.818) that can predict the optimal conditions to maximize the yield, validated experimentally.     

Inhibitory effect of Saccharomyces cerevisiae extract obtained through ultrasound-assisted extraction on melanoma cells

Although the immune enhancing effect of yeast has been widely reported, studies specifically investigating its effects on skin cancer are lacking. Therefore, this study aimed to develop a yeast extract capable of inhibiting melanoma cells using ultrasound technology, which can lyse the cell walls allowing subsequent rapid yeast extraction. To compare the extraction efficiency across different extraction methods, the total yield, as well as total glucan, α-glucan, and β-glucan yields were measured. Ultrasound-assisted extract of yeast (UAEY) was found to effectively inhibit melanoma cell growth and proliferation as well as the expression of cyclin D1 and c-myc, in vitro. Additionally, the extract reduced melanoma tumor volume and cyclin D1 levels in BALB/c nu/nu mice. The optimal extraction conditions were 0.2 M NaOH, 3 h, 70 °C, 20 kHz, and 800 W, resulting in an increased total extraction and β-glucan yields of 73.6% and 7.1%, respectively, compared with that achieved using a conventional chemical (0.5 M NaOH) extraction method. Taken together, the results of this study suggest that UAEY may represent an effective anti-skin cancer agent.     

Optimization of the ultrasound-assisted extraction of melatonin from red rice (Oryza sativa) grains through a response surface methodology

An analytical ultrasound-assisted extraction (UAE) technique has been optimized and validated for the extraction of melatonin from rice grains. A Box–Behnken design in conjunction with a response surface methodology based on six factors and three levels was used to evaluate the effects of the studied factors prior to optimizing the UAE conditions. The significant (p < 0.05) response surface models with high coefficients of determination were fitted to the experimental data. Solvent composition and extraction temperature were found to have very significant effects on the response value (p < 0.005). The optimal UAE conditions were as follows: extraction time of 10 min, ultrasound amplitude of 30%, cycle of 0.2 s⁻¹, extraction temperature of 40 °C, 50% methanol in water as the extraction solvent at pH 3.5 and a solvent/solid ratio 2.5:1. The method validation ensured right values for linearity, LOD, LOQ, precision and recovery. Furthermore, the method was successfully applied in the analysis of a number of rice samples throughout the rice production process. Hence, it was demonstrated that this particular UAE method is an interesting tool for the determination of melatonin in rice grain samples.     

Optimization of ultrasound extraction of functional compound from makiang seed by response surface methodology and antimicrobial activity of optimized extract with its application in orange juice

An ultrasound-assisted extraction (UAE) was optimized for the extraction of bioactive compound (total phenolic compound and total flavonoid content) with antioxidant activity (DPPH and FRAP assays) using response surface methodology based on Box-Behnken design (BBD). The effect of extraction temperature (X₁: 30–70 °C), extraction time (X₂: 25–45 min) and amplitude (X₃: 30–50%) were determined. In addition, antimicrobial activity and application of optimized makiang seed extract (MSE) were also evaluated. Results showed that the optimum condition of UAE were X₁: 51.82 °C, X₂: 31.87 min and X₃: 40.51%. It was also found that gallic acid was the major phenolic compound of optimized MSE and its minimum inhibitiory concentration (MIC) and minimum bactericidal concentration (MBC) was between 1.56 - 6.25 and 25–100 mg/mL respectively. The addition of MSE could enhance the stability of orange juice and shelf life extension was also obtained. This research finding suggests the beneficial opportunities for ultrasound-assisted extraction for the production of bioactive compound from makiang seed with antioxidant activity leading to an application in medicinal and functional food industry.     

Optimization of ultrasonic cell grinder extraction of anthocyanins from blueberry using response surface methodology

Ultrasonic cell grinder extraction (UCGE), using water as the solvent, was firstly applied to extract anthocyanins from blueberry. Extraction yield was related with four variables, including ratio of solution to solid, extraction power, buffer time, and extraction time. On the basis of response surface methodology (RSM), the optimal conditions were determined to be the ratio of solution to solid as 25:1 (mL/g), the extraction power as 1500 W, the buffer time as 3.0 s, and the extraction time as 40 min. The experimental yield of anthocyanins using UCGE was 2.89 mg/g higher than that of conventional ultrasound-assisted extraction (CUAE). This study indicated that UCGE was an innovative, efficient, and environment friendly method in ultrasonic extraction fields, and had a potential to effectively extract other bioactive constituents.     

Optimization of ultrasonic-assisted extraction of natural antioxidants from rice bran using response surface methodology

Ultrasonic technology was applied for extraction of polyphenols and antioxidants from the rice bran using ethanol as a food grade solvent. Response surface methodology (RSM) was used to optimize experimental conditions for extraction of polyphenols and antioxidants. Three independent variables such as solvent percentage (%), temperature (°C) and time (min) were studied. Effect of ethanol concentration was found to be significant on all responses. Total phenolic content (TPC) varied from 2.37 to 6.35mg gallic acid equivalent/g of dry sample. Antioxidant activity of the extracts was determined by the ferric reducing antioxidant power (FRAP) assay and scavenging activity of 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical. FRAP and DPPH values varied from 31.74 to 57.23μmol Fe(2+)/g of dry sample and 16.88% to 55.61% inhibition, respectively. Extraction yields ranged from 11 to 20.2%. Optimal ultrasonic-assisted extraction (UAE) conditions were identified as 65-67% ethanol, 51-54°C, 40-45min. The experimental values agreed with those predicted by SRM models, thus indicating suitability of the model employed and the success of RSM in optimizing the extraction conditions.     

Ultrasound-assisted extraction of functional compound from mulberry (Morus alba L.) leaf using response surface methodology and effect of microencapsulation by spray drying on quality of optimized extract

This study aimed to optimize the ultrasound-assisted extraction (UAE) condition of mulberry leaf extract (MLE) using response surface methodology and to microencapsulate MLE by spray drying using different coating materials and ratios of coating material and MLE. The extraction results showed that MLE from condition of 60 °C (X₁, temperature), 30 min (X₂, time) and 60% v/v (X₃, ethanol concentration) exhibited the highest bioactive compound and antioxidant activity (DPPH and FRAP assay). Based on this optimal condition, MLE was further encapsulated by spray drying. It was found that MLE encapsulated with resistant maltodextrin at ratio of MLE and resistant maltodextrin 1:1 (w/w) showed the highest encapsulation yield (%) and encapsulation efficiency (%). Water solubility, moisture content and water activity were non-significant (p > 0.05) among the microcapsules. The scanning electron microscope (SEM) revealed that the types of coating material affected their microstructures and microcapsules prepared by resistant maltodextrin as coating material had a spherical shape, smooth surface and less shrinkage than microcapsules prepared by maltodextrin and gum arabic which had rough surfaces. The highest antioxidant activity was obtained from microcapsule prepared by gum arabic at ratio of MLE and gam arabic 1:2 (w/w). In conclusion, optimal condition from UAE and encapsulation by spray drying suggest the critical potential for production of functional food with improved bioactive compound stability and maximized antioxidant activity.     

Optimization of ultrasound extraction of phenolic compounds from coconut (Cocos nucifera) shell powder by response surface methodology

Coconut is a tropical fruit largely consumed in many countries. In some areas of the Brazilian coast, coconut shell represents more than 60% of the domestic waste volume. The coconut shell is composed mainly of lignin and cellulose, having a chemical composition very similar to wood and suitable for phenolic extraction. In this work, the use of ultrasound to extract phenolic compounds from coconut shell was evaluated. The effect of temperature, solution to solid ratio, pH and extraction time were evaluated through a 2(4) experimental planning. The extraction process was also optimized using surface response methodology. At the optimum operating condition (30 degrees C, solution to solid ratio of 50, 15 min of extraction and pH 6.5) the process yielded 22.44 mg of phenolic compounds per gram of coconut shell.     

Optimization of ultrasonic-assisted extraction (UAE) of betulin from white birch bark using response surface methodology

Betulin is an abundant naturally occurring triterpene, which makes it a potentially important raw material for a precursor of biologically active compounds. The objective of the current study was to determine the optimum UAE conditions for betulin from B. papyfera bark. The optimum conditions were evaluated with fractional factorial design and optimized using response surface methodology. High yields of betulin were observed from white birch bark by UAE technology. The solvent concentration and the ratio of material to solvent were the most significant parameters on betulin extraction as evaluated through FFD. The extraction conditions were further investigated with central composite design. The fitted second-order model revealed that the optimal conditions consisted of 98% ethonal concentration, 1:42 the ratio of white birch bark to solvent, extraction temperature 50 °C, ultrasonic frequency 5 kHz and extraction time 3 h. Under the optimized condition, the maximum productivity of betulin predicted is 23.17%. The extraction productivity and purity of betulin under the optimized extraction conditions were great higher than that of the non-optimized condition. The present study demonstrates that ultrasound is a great efficiency tool for the fast extraction of betulin from white birch bark.     

Ultrasound-assisted extraction and purification of schisandrin B from Schisandra chinensis (Turcz.) Baill seeds: Optimization by response surface methodology

The objective of this study is to develop a process consisting of ultrasonic-assisted extraction, silica-gel column chromatography and crystallization to optimize pilot scale recovery of schisandrin B (SAB) from Schisandra chinensis seeds. The effects of five independent variables including liquid–solid ratio, ethanol concentration, ultrasonic power, extraction time, and temperature on the SAB yield were evaluated with fractional factorial design (FFD). The FFD results showed that the ethanol concentration was the only significant factor for the yield of SAB. Then, with the liquid–solid ratio 5 (mL/g) and ultrasonic power 600 W, the other three parameters were further optimized by means of response surface methodology (RSM). The RSM results revealed that the optimal conditions consisted of 95% ethanol, 60 °C and 70 min. The average experimental SAB yield under the optimum conditions was found to be 5.80 mg/g, which was consistent with the predicted value of 5.83 mg/g. Subsequently, a silica gel chromatographic process was used to prepare the SAB-enriched extract with petroleum ether/acetone (95:5, v/v) as eluents. After final crystallization, 1.46 g of SAB with the purity of 99.4% and the overall recovery of 57.1% was obtained from 400 g seeds powder. This method provides an efficient and low-cost way for SAB purification for pharmaceutical industrial applications.     

Optimisation of ultrasound assisted extraction of phenolic compounds from Sparganii rhizoma with response surface methodology

The present study reports on the extraction of phenolic compounds from sparganii rhizome. Box–Behnken Design (BBD), a widely used form of response surface methodology (RSM), was used to investigate the effect of process variables on the ultrasound-assisted extraction (UAE). Three independent variables including ethanol concentration (%), extraction time (min) and solvent-to-material ratio (mL/g) were studied. The results showed that the optimal UAE condition was obtained with an ethanol concentration of 75.3%, an extraction time of 40 min and a solvent-to-material ratio of 19.21 mL/g for total phenols, and an ethanol concentration of 80%, an extraction time of 33.54 min and solvent-to-material ratio of 22.72 mL/g for combination of ρ-hydroxybenzaldehyde, ρ-coumaric acid, vanillic acid, ferulic acid, rutin and kaempferol. The experimental values under optimal conditions were in good consistent with the predicted values, which suggested UAE is more efficient process as compared to solvent extraction.     

Optimization of ultrasound assisted extraction of antioxidant compounds from marjoram (Origanum majorana L.) using response surface methodology

The present study optimized the ultrasound assisted extraction (UAE) conditions to maximize the antioxidant activity [Ferric ion Reducing Antioxidant Power (FRAP)], total phenol content (TP) and content of individual polyphenols of extracts from marjoram. Optimal conditions with regard to amplitude of sonication (24.4-61.0 μm) and extraction temperature (15-35 °C) and extraction time (5-15 min) were identified using response surface methodology (RSM). The results showed that the combined treatment conditions of 61 μm, 35 °C and 15 min were optimal for maximizing TP, FRAP, rosmarinic acid, luteolin-7-O-glucoside, apigenin-7-O-glucoside, caffeic acid, carnosic acid and carnosol values of the extracts. The predicted values from the developed quadratic polynomial equation were in close agreement with the actual experimental values with low average mean deviations (E%) ranging from 0.45% to 1.55%. The extraction yields of the optimal UAE were significantly (p < 0.05) higher than solid/liquid extracts. Predicted models were highly significant (p < 0.05) for all the parameters studied with high regression coefficients (R²) ranging from 0.58 to 0.989.     

Optimization of ultrasound-assisted extraction of anthocyanins in red raspberries and identification of anthocyanins in extract using high-performance liquid chromatography-mass spectrometry

Anthocyanins (Acys) are naturally occurring compounds that impart color to fruit, vegetables and plants. The extraction of Acys from red raspberry (Rubus idaeus L. var. Heritage) by ultrasound-assisted process (UAP) was studied. A central composite rotate design (CCRD) was used to obtain the optimal conditions of ultrasound-assisted extraction (UAE), and the effects of operating conditions, such as the ratio of solvents to materials, ultrasonic power and extraction time, on the extraction yield of Acys were studied through response surface methodology (RSM). The optimized conditions of UAE were as follows: ratio of solvents to materials was 4:1 (ml/g), extraction time was 200 s, and ultrasonic power was 400 W. Under these conditions 34.5 mg of Acys from 100 g of fresh fruits (T_Acy, expressed as cyanidin-3-glucoside), approximately 78.13% of the total red pigments, could be obtained by UAE. The Acys compositions of extracts were identified by high-performance liquid chromatography–mass spectrometry (HPLC–MS), 12 kinds of Acys had been detected and eight kinds of Acys were characterized. Result indicated that cyanidin-3-sophoroside, cyanidin-3-(2^G-glucosylrutinoside), cyanidin-3-sambubioside, cyanidin-3-rutinoside, cyanidin-3-xylosylrutinoside, cyanidin-3-(2^G-glucosylrutinoside), and cyanidin-3-rutinoside were main components in extracts. In addition, in comparison with the conventional solvent extraction, UAE is more efficient and rapid to extract Acys from red raspberry, due to the strong disruption of fruit tissue structure under ultrasonic acoustic cavitation, which had been observed with the scanning electron microscopy (SEM). However, the Acys compositions in extracts by both methods were similar, which were investigated using HPLC profile.     

Electrospun precursor carbon nanofibers optimization by using response surface methodology

Ultrafine fibers were electrospun from Polyacrylonitrile and N,N-dimethylformamide solution to be used as a precursor for carbon nanofibers. An electrospinning set-up was used to collect fibers with diameter ranging from 104 nm to 434 nm. Morphology of fibers and its distribution were investigated by varying Berry's number, charge density, spinning angle, spinneret diameter and collector area. A more systematic understanding of process parameters was obtained and a quantitative relationship between electrospinning parameters and average fiber diameter was established by using response surface methodology. It was concluded that; Berry's number, charge density and spinneret diameters played an important role to the diameter of nanofibers and its standard deviation. Spinning angle and collector area had no significant impact. Based on response surface methodology the optimum Polyacrylonitrile average fiber diameter of 280 nm and 28 nm standard deviation, were collected at 1.6 kV/cm charge density, 8 Berry's number and 0.9 mm spinneret diameter.     

Optimization of process parameters of titanium dioxide films by response surfaces methodology

An efficient approach for determination of the optimum process parameters for titanium dioxide coatings by using second-order response surface model is presented and investigated experimentally. Thin films were prepared by electron-beam evaporation associated with ion-beam assisted deposition by using different control factors, including starting materials, working pressure, substrate temperature, deposition rate and annealing temperature. The factorial design of the experiment was established to meet the equipment conditions and to avoid affecting the results. The main effect between various factors and interactions are independent. The significant level of both the main effects and the interaction are observed by analysis of variance (ANOVA) approach. Based on the statistical analysis, the results have provided much valuable information on the relationship between various control factors and thin film properties. Besides the optimum optical constants and surface roughness of TiO₂ thin films were obtained in the range of each parameter level. The factorial prediction model for preparation parameters of thin film was also established.     

Enzymatic inactivation and antioxidant properties of blackberry juice after thermoultrasound: Optimization using response surface methodology

The purpose of this research was to optimize the thermoultrasound conditions for blackberry juice using the response surface methodology and considering juice quality parameters and antioxidant capacity. With the exception of microbial growth, the response variables showed high correlation coefficients with the mathematical model (R²adj > 0.91). Thermoultrasound treatment inactivated all the evaluated microorganisms, and at the optimum conditions (50 ± 1 °C at 17 ± 1 min) it increased enzyme inactivation and antioxidant activity in comparison to pasteurized juice. The results demonstrated that thermoultrasound can be an alternative to pasteurization for the production of safe and high-quality juices with the added value of higher concentration of bioactive compounds and antioxidant capacity.     

Optimization of ultrasonic-assisted ultrafiltration process for removing bacterial endotoxin from diammonium glycyrrhizinate using response surface methodology

Ultrasonic-assisted ultrafiltration (UAU) removing bacterial endotoxin from diammonium glycyrrhizinate, was firstly applied to surfactant separation. Separation efficiency was related with four variables, including ultrafiltration molecular weight cut off (MWCO), ultrasonic power, concentration and pH. The SCQ-9200E ultrasonic system was provided for the study with adjustable ultrasonic power 80 W to 800 W, and the ultrasonic frequency was 40 KHz. On the basis of response surface methodology (RSM), the optimal separation conditions were determined to be the ultrafiltration MWCO as 10 kDa, the ultrasonic power as 570 W, diammonium glycyrrhizinate concentration as 150.00 μg/mL and the pH as 4.70. The experimental rejection of bacterial endotoxin was 94.08%, meanwhile the transmittance of diammonium glycyrrhizinate was 93.65%. Based on the ultrasonic power, solution volume, and ultrasonic container size, the experiments with UAU at different power intensities showed that ultrasonic at a power intensity of 57 W/L and the power density of 0.32 W/cm² could solve the separation contradiction between diammonium glycyrrhizinate and bacterial endotoxin. This study indicated that UAU could be an innovation in ultrasonic separation fields, and had a vast range of prospects for making use in pharmaceutical preparation area.     

Improved adsorption performance of nanostructured composite by ultrasonic wave: Optimization through response surface methodology,isotherm and kinetic studies

In this work, ultrasound-assisted adsorption of an anionic dye, sunset yellow (SY) and cationic dyes, malachite green (MG), methylene blue (MB) and their ternary dye solutions onto Cu@ Mn-ZnS-NPs-AC from water aqueous was optimized by response surface methodology (RSM) using the central composite design (CCD). The adsorbent was characterized using Field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), Energy-dispersive X-ray spectroscopy (EDX) and EDX mapping images. The effects of various parameters such as pH, sonication time, adsorbent mass and initial concentrations of SY, MG and MB were examined. A total 33 experiments were conducted to establish a quadratic model. Cu@ Mn-ZnS-NPs-AC has the maximum adsorption efficiency (>99.5%) when the pH, sonication time, adsorbent mass and initial concentrations of SY, MG and MB were optimally set as 6.0, 5 min, 0.02 g, 9, 12 and 12 mg L⁻¹, respectively. Sonication time has a statistically significant effect on the selected responses. Langmuir isotherm model was found to be best fitted to adsorption and adsorption capacities were 67.5 mg g⁻¹ for SY, 74.6 mg g⁻¹ for MG and 72.9 mg g⁻¹ for MB. Four kinetic models (pseudo-first order, pseudo-second order, Weber–Morris intraparticle diffusion rate and Elovich) were tested to correlate the experimental data and the sorption was fitted well with the pseudo-second order kinetic model.