Impact of ultrasound on solid–liquid extraction of phenolic compounds from maritime pine sawdust waste. Kinetics,optimization and large scale experiments

Maritime pine sawdust, a by-product from industry of wood transformation, has been investigated as a potential source of polyphenols which were extracted by ultrasound-assisted maceration (UAM). UAM was optimized for enhancing extraction efficiency of polyphenols and reducing time-consuming. In a first time, a preliminary study was carried out to optimize the solid/liquid ratio (6 g of dry material per mL) and the particle size (0.26 cm²) by conventional maceration (CVM). Under these conditions, the optimum conditions for polyphenols extraction by UAM, obtained by response surface methodology, were 0.67 W/cm² for the ultrasonic intensity (UI), 40 °C for the processing temperature (T) and 43 min for the sonication time (t). UAM was compared with CVM, the results showed that the quantity of polyphenols was improved by 40% (342.4 and 233.5 mg of catechin equivalent per 100 g of dry basis, respectively for UAM and CVM). A multistage cross-current extraction procedure allowed evaluating the real impact of UAM on the solid–liquid extraction enhancement. The potential industrialization of this procedure was implemented through a transition from a lab sonicated reactor (3 L) to a large scale one with 30 L volume.     

Continuous and pulsed ultrasound-assisted extraction of carob’s antioxidants: Processing parameters optimization and identification of polyphenolic composition

Polyphenols in carobs have recently attracted great attention due to their wide range of biological and health promoting effects. A comprehensive study was conducted to find an optimum method for the extraction, purification and characterization of these valuable bioactive substances. Under this framework, the ultrasound-assisted extraction (UAE) of polyphenols from carob pulp was optimized by the maximization of the yield in total phenolics using response surface methodology. In particular, the effects of solid-solvent ratio, solvent concentration, extraction time, sonication amplitude, and sonication mode were investigated and optimized using a complete experimental design. In comparison to conventional extraction techniques, UAE offered a higher yield of antioxidants and a shorter processing time. Solid-phase extraction was evaluated as a clean-up strategy prior to the electrophoretic analysis of extracts. The results from the analysis of real samples revealed the predominance of gallic acid and highlighted the great influence of the ripening stage on carobs composition.     

Optimization of the synthesis parameters of high surface area ceria nanopowder prepared by surfactant assisted precipitation method

Response surface methodology (RSM) has been used to optimize the critical parameters responsible for higher surface area of ceria nanopowder prepared by surfactant assisted precipitation method. A three-level central composite design (CCD) was used to optimize pH, CTAB/metal molar ratio and calcination temperature. A quadratic model between response and the independent parameters was developed and the response surface model was tested with analysis of variance (ANOVA). The optimum operating conditions determined were a pH value of 9.4, CTAB/metal molar ratio of 0.5 and calcination temperature of 266 °C. Under these optimal conditions maximum surface area of 158 m²/g has been achieved.     

Box-Behnken设计优化浊点萃取-原子荧光光谱法测定中药材中的汞

建立了浊点萃取分离原子荧光光谱法测定中药材中痕量汞的方法。Hg2+可与双硫腙生成疏水性螯合物,水浴加热15 min,鳌合物被萃取到Triton X-114表面活性剂相,经离心与水相分开。在单因素基础上,筛选出对萃取效率有较为显著影响的四因素—溶液pH、Triton X-114浓度、双硫腙浓度和平衡温度,并首次采用Box-Behnken设计和响应面法优化实验参数。结果表明,响应值与因素之间可采用二项式拟合,四个因素的一次项和二次项,以及pH和Trion X-114、双硫腙交互项对萃取率影响显著,p＜0.05;浊点萃取的最佳条件为： pH值为5.1,Trion X-114浓度1.16 g·L-1,双硫腙浓度为4.87 mol·L-1,平衡温度为35.6 ℃,理论荧光值4 528.74,实测值与其较接近,仅有2.1%的差别。汞在1~5 μg·L-1与荧光值有良好的线性关系,方法检出限为0.012 47 μg·L-1,RSD为1.30%。该方法成功用于巴戟天、穿心莲和陈皮中汞含量的测定,加标回收率为95.0%~100.0%。Box-Behnken设计结合响应面分析法可以很好的用于浊点萃取条件的优化。     

Novel modified ultrasonication technique for the extraction of lycopene from tomatoes

Lycopene extraction was carried out via the ultrasonic assisted extraction (UAE) with response surface methodology (RSM). Sonication enhanced the efficiency of relative lycopene yield (enhancement of 26% extraction yield of lycopene in 6 replications at 40.0 min, 40.0 °C and 70.0% v/w in the presence of ultrasound), lowered the extraction temperature and shortened the total extraction time. The extraction was applied with the addition of oxygen-free nitrogen flow and change of water route during water bath sonication. The highest relative yield of lycopene obtained was 100% at 45.0 °C with total extraction time of 50.0 min (30:10:10) and ratio of solvent to freeze-dried tomato sample (v/w) of 80.0:1. Optimisation of the lycopene extraction had been performed, giving the average relative lycopene yield of 99% at 45.6 min, 47.6 °C and ratio of solvent to freeze-dried tomato sample (v/w) of 74.4:1. From the optimised model, the average yield of all-trans lycopene obtained was 5.11 ± 0.27 mg/g dry weight. The all-trans lycopene obtained from the high-performance liquid chromatography (HPLC) chromatograms was 96.81 ± 0.81% with 3.19 ± 0.81% of cis-lycopenes. The purity of total-lycopene obtained was 98.27 ± 0.52% with β-carotene constituted 1.73 ± 0.52% of the extract. The current improved, UAE of lycopene from tomatoes with the aid of RSM also enhanced the extraction yield of trans-lycopene by 75.93% compared to optimised conventional method of extraction. Hence, the current, improved UAE of lycopene promotes the extraction yield of lycopene and at the same time, minimises the degradation and isomerisation of lycopene.     

Ultrasonication--a complementary 'green chemistry' tool to biocatalysis: a laboratory-scale study of lycopene extraction

Lycopene is bequeathed with multiple bio-protective roles, primarily attributed to its unique molecular structure. The concomitant exploitation of two of the green chemistry tools viz., sonication and biocatalysis is reported here for the laboratory scale extraction of lycopene from tomato peel. The coupled system improved the extraction by 662%, 225% and 150% times over the unaided, only cellulase ‘Onozuka R-10’ treated and only sonication treated samples respectively. The sonication parameters (duration, cycle and amplitude) during the coupled operation were optimized using response surface methodology (RSM). Derivative UV-visible spectra (i.e., dA/dλ and d²A/dλ² against λ), FTIR analysis, and DPPH scavenging test suggested that the reported extraction protocol did not affect the molecular structure and bioactivity of the extracted lycopene. The influence of sonication on the probable structural modulation (through UV-visible spectral analysis) and activity of the enzyme were also analyzed. A plausible mechanism is proposed for the enhanced extraction achieved via the coupled system.     

Brewing coffee? – Ultra-sonication has clear beneficial effects on the extraction of key volatile aroma components and triglycerides

Ultrasound has been investigated as a new technique for brewing coffee. A two-level factorial experimental design was conducted to identify the effects of ultra-sonication on the extraction of coffee components during ultrasonically-assisted coffee brewing. Different brews were produced by aqueous extraction from roasted ground coffee beans with sonication, and without it as a control, by varying coffee concentration (5% and 10% w/w), temperature (25 and 50 °C) and sonication time (1 and 5 min). These brews were tested for antioxidant capacity (using the ABTS assay), caffeine and triglycerides (using quantitative NMR spectroscopy) and specific aroma/flavour volatiles (using headspace SPME-GC-MS). Additional observations of colour, foaming, body and flavour were also reported. Ultrasound was found to significantly increase the extraction of caffeine, triglycerides and several of the key volatile compounds from coffee, although it did appear to decrease the concentration of antioxidants over the controls, especially with longer time and higher temperature. Furthermore, all the sonicated samples exhibited a lighter caramel colour and lower foam formation which were attributed to their higher triglyceride content. The increased concentration of triglycerides and volatiles were by far the most outstanding responses.     

Optimization of high pressure bioactive compounds extraction from pansies (Viola × wittrockiana) by response surface methodology

Response surface methodology (RSM) was employed for the first time to optimize high pressure extraction (HPE) conditions of bioactive compounds from pansies, namely: pressure (X₁: 0–500?MPa), time (X₂: 5–15?min) and ethanol concentration (X₃: 0–100%). Consistent fittings using second-order polynomial models were obtained for flavonoids, tannins, anthocyanins, total reducing capacity (TRC) and DPPH (2,2-diphenyl-1-picrylhydrazyl) radical scavenging activity. The optimum extraction conditions based on combination responses for TRC, tannins and anthocyanins were: X₁?=?384?MPa, X₂?=?15?min and X₃?=?35% (v/v) ethanol, shortening the extraction time when compared to the classic method of stirring (approx. 24?h). When the optimum extraction conditions were applied, 65.1?mg of TRC, 42.8?mg of tannins and 56.15?mg of anthocyanins/g dried flower were obtained. Thus, HPE has shown to be a promising technique to extract bioactive compounds from pansies, by reducing the extraction time and by using green solvents (ethanol and water), for application in diverse industrial fields.     

油菜秸秆对水溶液中Pb(Ⅱ)吸附条件优化与机理的研究

探究油菜秸秆髓芯、外壳、籽荚对水溶液中Pb(Ⅱ)的吸附能力及其吸附机理。以水溶液中Pb(Ⅱ)最大去除率为评价指标,采用响应面法Box-Behnken Design实验来分析溶液pH、Pb(Ⅱ)初始浓度、粒径大小、油菜秸秆各部位投加量和时间因素对油菜秸秆吸附Pb(Ⅱ)的影响程度并建立多元回归模型,优化出最佳吸附条件参数组合;应用吸附动力学、等温吸附线模型来拟合油菜秸秆各部位对Pb(Ⅱ)吸附过程,评价其吸附行为;用红外光谱对吸附水溶液中Pb(Ⅱ)前后的油菜秸秆髓芯、外壳、籽荚进行表征,探讨其基团变化情况。结果表明： 水溶液pH与油菜秸秆髓芯、外壳、籽荚的投加量两个因素是影响油菜秸秆对水溶液中Pb(Ⅱ)去除的关键因素。模型回归决定系数分别是R2_髓芯=0.9664,R2_外壳=0.970 1,R2_籽荚=0.964 9,方程拟合较好,模型可用。油菜秸秆髓芯、外壳、籽荚对Pb(Ⅱ)的吸附行为符合二阶动力学方程与Langmuir等温线模型,对水溶液中Pb(Ⅱ)最大吸附量分别为135.14,78.74和90.09 mg·g-1。通过比较油菜秸秆髓芯、外壳、籽荚吸附水溶液中Pb(Ⅱ)前后红外光谱图发现,油菜秸秆各部位基团(羟基、羧基、酰胺等基团)发生了峰波数位移、强度降低的变化,提示这些基团在吸附水溶液Pb(Ⅱ)过程中发挥重要作用。     

Ultrasonic extraction of steroidal alkaloids from potato peel waste

Potato processors produce large volumes of waste in the form of potato peel which is either discarded or sold at a low price. Potato peel waste is a potential source of steroidal alkaloids which are biologically active secondary metabolites which could serve as precursors to agents with apoptotic, chemopreventive and anti-inflammatory properties. The present study investigated the relative efficacy of ultrasound assisted extraction (UAE) and solid liquid extraction (SLE) both using methanol, to extract steroidal alkaloids from potato peel waste and identified optimal conditions for UAE of α-solanine, α-chaconine, solanidine and demissidine. Using response surface methodology optimal UAE conditions were identified as an amplitude of 61 μm and an extraction time of 17 min which resulted the recovery of 1102 μg steroidal alkaloids/g dried potato peel (DPP). In contrast, SLE yielded 710.51 glycoalkaloid μg/g DPP. Recoveries of individual glycoalkoids using UAE yielded 273, 542.7, 231 and 55.3 μg/g DPP for α-solanine, α-chaconine, solanidine and demissidine respectively. Whereas for SLE yields were 180.3, 337.6, 160.2 and 32.4 μg/g DPP for α-solanine, α-chaconine, solanidine and demissidine respectively. The predicted values from the developed second order quadratic polynomial equation were in close agreement with the experimental values with low average mean deviation (E < 5%) values. Predicted models were highly significant (p < 0.05) for all parameters studied. This study indicates that UAE has strong potential as an extraction method for steroidal alkaloids from potato peel waste.     

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...