微波浸取测定土壤中总溶解固体

微波溶样技术是近年来分析化学领域中应用很广泛的一种样品预处理的新技术 ,它具有对样品的分析快速、安全、无污染、无损失、省试剂等特点[1,2 ] 。由于水溶性无机盐是吸附在土壤颗粒表面 ,而土壤颗粒是一种蜂窝状结构 ,渗透在蜂窝内的盐分较难溶解 ,所以传统的测定土壤中总溶解固体的方法是采用振荡法[3 ,4 ] ,此法在测定大量样品时费时、操作繁琐。本文研究了用微波溶样方法浸取土壤中的总溶解固体。试验表明 ,本法简单、快速 ,且浸取完全 ,测定结果准确可靠。1　试验部分1.1　仪器与试剂ＷＲ 1Ｃ型微波样品处理系统双层密封微波消化罐Ｃ…     

Optimization of Ultrasound-Assisted Extraction of Yields and Total Methoxyflavone Contents from Kaempferia parviflora Rhizomes

The major bioactive components of Kaempferia parviflora (KP) rhizomes, 3,5,7,3′,4′-pentamethoxyflavone (PMF), 5,7-dimethoxyflavone (DMF), and 5,7,4′-trimethoxyflavone (TMF), were chosen as the quantitative and qualitative markers for this plant material. In order to extract bioactive components (total methoxyflavones) from KP rhizomes, ultrasound-assisted extraction (UAE) was proposed as part of this study. Plackett–Burman design (PBD) and Box–Behnken design (BBD) were utilized to optimize the effects of UAE on extraction yields and total methoxyflavone contents in KP rhizomes. First, PBD was utilized to determine the effect of five independent variables on total yields and total methoxyflavone contents. The results indicated that the concentration of the extracting solvent (ethanol), the extraction time, and the ratio of solvent to solid were significant independent terms. Subsequently, BBD with three-level factorial experiments was used to optimize the crucial variables. It was discovered that the concentration of ethanol was the most influential variable on yields and total methoxyflavone contents. Optimum conditions for extraction yield were ethanol concentration (54.24% v/v), extraction time (25.25 min), and solvent-to-solid ratio (49.63 mL/g), while optimum conditions for total methoxyflavone content were ethanol concentration (95.00% v/v), extraction time (15.99 min), and solvent-to-solid ratio (50.00 mL/g). The relationship between the experimental and theoretical values was perfect, which proved that the regression models used were correct and that PBD and BBD were used to optimize the conditions in the UAE to obtain the highest yield and total methoxyflavone content in the KP rhizomes.     

Optimization of Ultrasonic-Assisted Extraction of Total Flavonoids from Abrus Cantoniensis (Abriherba) by Response Surface Methodology and Evaluation of Its Anti-Inflammatory Effect

Abrus cantoniensis is a Chinese herbal medicine with efficacy in clearing heat and detoxification, as well as relieving liver pain. The whole plant, except the seeds, can be used and consumed. Flavonoids have been found in modern pharmacological studies to have important biological activities, such as anti-inflammatory, antibacterial and antioxidant properties. The antibacterial and antioxidant bioactivities of the total flavonoids of Abrus cantoniensis (ATF) have been widely reported in national and international journals, but there are fewer studies on their anti-inflammatory effects. The present study focused on the optimization of the ultrasonic extraction process of ATF by response surface methodology and the study of its anti-inflammatory effects in vitro and in vivo. The results showed that the factors that had a great impact on the ATF extraction were the material-to-liquid ratio, ultrasonic extraction cycles and ethanol concentration. The best extraction process used a material-to-liquid ratio of 1:47, ultrasonic extraction cycles of 4 times, an ethanol concentration of 50%, an ultrasonic extraction time of 40 min and an ultrasonic power of 125 W. Under these conditions, the actual extraction rate of total flavonoids was 3.68%, which was not significantly different from the predicted value of 3.71%. In an in vitro anti-inflammatory assay, ATF was found to be effective in alleviating LPS (lipopolysaccharide)-induced inflammation in mouse peritoneal macrophages. In an in vivo anti-inflammatory assay, ATF was found to have a significant inhibitory effect on xylene-induced ear swelling in mice and cotton ball granuloma in mice, and the inhibitory effect was close to that of the positive control drug dexamethasone. This may provide a theoretical basis for the further development of the medicinal value of Abrus cantoniensis.     

Banana as Adjunct in Beer Production: Applicability and Performance of Fermentative Parameters

Traditionally, the raw materials for beer production are barley, hops, water, and yeast, but most brewers use also different adjuncts. During the alcoholic fermentation, the contribution of aroma compounds from other ingredients to the final beer flavor depends on the wort composition, on the yeast strain, and mainly on the process conditions. In this context, banana can also be a raw material favorable to alcoholic fermentation being rich in carbohydrates and minerals and providing low acidity. In this work, the objective was to evaluate the performance of wort adjusted with banana juice in different concentrations. For this, static fermentations were conducted at 15 °C at pilot scale (140 L of medium). The addition of banana that changed the concentration of all-malt wort from 10 °P to 12 and 15 °P were evaluated (°P is the weight of the extract or the sugar equivalent in 100 g solution, at 20 °C). The results showed an increase in ethanol production, with approximately 0.4 g/g ethanol yield and 0.6 g/L h volumetric productivity after 84 h of processing when concentrated wort was used. Thus, it was concluded that banana can be used as an adjunct in brewing methods, helping in the development of new products as well as in obtaining concentrated worts.     

Flavonoids in Selected Mediterranean Fruits: Extraction,Electrochemical Detection and Total Antioxidant Capacity Evaluation

Flavonoids are natural phenolic derivatives that, in low concentration, can provide health benefits by preventing biomolecules (proteins, nucleic acids, lipids, sugars) oxidative damage through free radical mediated reactions. The flavonoids, in selected Mediterranean seasonal fruits: apricot, sour cherry, plum, pomegranate, date, prickly pear (cactus fruit), and nectarine, by RP‐HPLC, coupled with photodiode array and electrochemical detectors, after microwave‐ultrasound assisted extraction, using flavonoid standards, were detected. The total antioxidant capacity in the lyophilized fruit extracts, by differential pulse voltammetry, (electrochemical index‐EI), integrated peak area, and chronoamperometry, was evaluated. In the lyophilized fruit extracts, and the catechin standard, the free radical scavenger efficient concentration (EC₅₀), using DPPH^. assay, was determined.     

Determination of Interfacial Reaction Parameters in Ion-Association Extraction by Total Reflection Induced Thermal Lens

Studies on adsorption kinetics and reaction mechanism at liquid-liquid interfaces are very important for not only classical solvent extraction analysis but also modern nano-science. For this purpose, we should develop versatile techniques that have in-situ, real time and highly sensitive feature. An interfacial thermal lens (TL) technique has been developed for monitoring the formation of Fe(Ⅱ)-4,7-diphenyl-1,10-phenanthroline (DPP) complex at a benzene-acetate buffer interface.     

Isolation and Extraction of Total Flavonoids from Epimedium Koreanum Nakai by Supercritical Fluid Extraction

In the present paper is reported the metnocl for the isolation and extraction of total flavonoids of Epimedium Koreanum Nateai by means of supercritical fluid extraction(SFE). By examining pressure, temperature, amounts of modifier and extraction time, the optimized condition of SFE is confirmed as 30 MPa and 60℃, with 70% ethanol as the modifier. The samples were statically extracted for 30 min, followed bydynamic extraction for 120 min at a flow rate of 6 mL/min. The quantitative analysis of total flavonoids was performed by UV-Vis spectrophotometry. Compared with the conventional method, the SFE method is more efficient, more rapid and more friendly environmentally.     

Optimization of Enzyme-Assisted Extraction and Purification of Flavonoids from Pinus koraiensis Nut-Coated Film and Antioxidant Activity Evaluation

Pinus koraiensis nut-coated film is a kind of by-product of nut processing, which has been shown to contain flavonoids, polyphenols, and other substances that can be used to produce natural antioxidant extracts. In this study, response surface methodology (RSM) was used to optimize the extraction process of flavonoids of P. koraiensis nut-coated film (PNF), and macroporous resin HPD600 was used to purify PNF (P-PNF). Its antioxidant activity was examined by DPPH (1,1-diphenyl-2-picrylhydrazyl) radical scavenging capacity, oxygen free radical absorption capacity (ORAC), total oxygen radical capture (TRAP), and iron ion reduction capacity. Under the ideal extraction conditions comprising a cellulase dosage of 90 U/g, a material/liquid ratio of 1:20 (g/mL), and an extraction time of 2 h, the PNF yield was 3.37%. Purification conditions were sample concentration of 2.0 mg/mL, pH of 5, water washing volume of 3 bed volume (BV), eluent ethanol concentration of 50%, and volume of 2 BV. The P-PNF recovery was 84.32%, and purity increased from 33.80% to 61.70%. Additionally, P-PNF showed increased antioxidant activity compared to PNF. Cumulatively, this study obtained the optimal values for the process parameters in order to achieve the maximum rates of extraction of PNF for economically optimal production at an industrial scale.     

荒漠植物中总脱氧核糖核酸分子的提取方法

建立了荒漠植物总脱氧核糖核酸分子（DNA）的提取方法.荒漠植物叶片加少量交联聚乙烯吡咯烷酮（PVPP粉末）研磨三次以上,得到样品超细粉末.样品粉末迅速加入前处理缓冲液,混匀后低速离心,弃上清留下沉淀物,在沉淀物中加入等体积预热的提取裂解液,混匀后60~70℃温浴1 h.高速离心提取上清液加入纯化液混匀、抽提、离心.再次提取混合液上清,加入预冷的异丙醇,-18℃沉淀DNA 0.5 h以上,异丙醇溶液高速离心,取沉淀用75%乙醇清洗两遍,晾干,加入超纯水溶解.方法具有操作简单和耗时少等优点,操作过程大约2~3 h.DNA损失少,产量高于500 ng/μL.方法提取主要荒漠植物叶片DNA纯度高、完整性好,具有广泛适用性.     

微波法提取水蓼中总黄酮的工艺研究

研究了水蓼中总黄酮的微波提取最佳工艺。采用单因素试验和正交试验考察微波功率、乙醇浓度、微波辐射时间、料液比对水蓼中总黄酮提取率的影响,优选提取工艺。最佳工艺条件为:微波功率为520W,乙醇浓度为60%,微波辐射60s,间歇辐射3次,料液比为1g∶20mL。结果表明,微波提取具有提取率高、提取速度快等特点,用于中草药的提取应用前景广阔。     

Estimation of Sorption Parameters of Solids by Means of Derivatograph Q

Derivatograph Q-1500D was completed with a partial vapour pressure control unit in order to study the sorption phenomena. The proposed arrangement allows to perform time consuming experiments at ambient atmospheric pressure in the temperature range 10–200°C.This revised version was published online in November 2005 with corrections to the Cover Date.     

Unconventional Extraction of Total Non-Polar Carotenoids from Pumpkin Pulp and Their Nanoencapsulation

Pumpkin is considered a functional food with beneficial effects on human health due to the presence of interesting bioactives. In this research, the impact of unconventional ultrasound-assisted extraction (UAE) and microwave-assisted extraction techniques on the recovery of total non-polar carotenoids from Cucurbita moschata pulp was investigated. A binary (hexane:isopropanol, 60:40 v/v) and a ternary (hexane:acetone:ethanol, 50:25:25 v/v/v) mixture were tested. The extracts were characterized for their antioxidant properties by in vitro assays, while the carotenoid profiling was determined by high-performance liquid chromatography coupled with a diode array detector. UAE with the binary mixture (30 min, 45 °C) was the most successful extracting technique, taking into consideration all analytical data and their correlations. In parallel, solid lipid nanoparticles (SLN) were optimized for the encapsulation of the extract, using β-carotene as a reference compound. SLN, loaded with up to 1% β-carotene, had dimensions (~350 nm) compatible with increased intestinal absorption. Additionally, the ABTS ((2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) assay showed that the technological process did not change the antioxidant capacity of β-carotene. These SLN will be used to load an even higher percentage of the extract without affecting their dimensions due to its liquid nature and higher miscibility with the lipid with respect to the solid β-carotene.     

Optimization of Ultrasound-Assisted Extraction of Polyphenols from Ilex latifolia Using Response Surface Methodology and Evaluation of Their Antioxidant Activity

The polyphenolic extract of Ilex latifolia (PEIL) exhibits a variety of biological activities. An evaluation of the parameters influencing the ultrasonic extraction process and the assessment of PEIL antioxidant activity are presented herein. Response surface methodology (RSM) was used to optimize the experimental conditions for the polyphenols ultrasonic-assisted extraction (UAE) from the leaves of Ilex latifolia. We identified the following optimal conditions of PEIL: ethanol concentration of 53%, extraction temperature of 60 °C, extraction time of 26 min and liquid–solid ratio of 60 mL/g. Using these parameters, the UAE had a yield of 35.77 ± 0.26 mg GAE/g, similar to the value we predicted using RSM (35.864 mg GAE/g). The antioxidant activity of PEIL was assessed in vitro, using various assays, as well as in vivo. We tested the effects of various doses of PEIL on D-galactose induced aging. Vitamin C (Vc) was used as positive control. After 21 days of administration, we measured superoxide dismutase (SOD) and glutathione peroxidase (GSH-Px) activities, malondialdehyde (MDA) levels in mouse serum and liver tissue. The results demonstrated that the PEIL exhibits potent radical scavenging activity against 1,1-diphenyl-2-picrythydrazyl (DPPH∙), 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid (ABTS⁺), and hydroxyl (∙OH) radicals. The serum concentrations of SOD and GSH-Px were higher, and MDA levels were lower, in the medium- and high-dose PEIL-treated groups than those in the aging group (p < 0.01), and the activity of MDA was lower than those of the model group (p < 0.01). The liver concentrations of SOD and GSH-Px were higher (p < 0.05), and MDA levels were lower, in the medium- and high-dose PEIL-treated groups than those in the aging control group (p < 0.01). These results suggest that optimizing the conditions of UAE using RSM could significantly increase the yield of PEIL extraction. PEIL possesses strong antioxidant activity and use as a medicine or functional food could be further investigated.     

Towards Accurate Predictions of Proton NMR Spectroscopic Parameters in Molecular Solids

The factors contributing to the accuracy of quantum-chemical calculations for the prediction of proton NMR chemical shifts in molecular solids are systematically investigated. Proton chemical shifts of six solid amino acids with hydrogen atoms in various bonding environments (CH, CH₂, CH₃, OH, SH and NH₃) were determined experimentally using ultra-fast magic-angle spinning and proton-detected 2D NMR experiments. The standard DFT method commonly used for the calculations of NMR parameters of solids is shown to provide chemical shifts that deviate from experiment by up to 1.5 ppm. The effects of the computational level (hybrid DFT functional, coupled-cluster calculation, inclusion of relativistic spin-orbit coupling) are thoroughly discussed. The effect of molecular dynamics and nuclear quantum effects are investigated using path-integral molecular dynamics (PIMD) simulations. It is demonstrated that the accuracy of the calculated proton chemical shifts is significantly better when these effects are included in the calculations.     

Porous Solids from Rigid Colloidal Templates: Morphogenesis

Modern research is increasingly focusing on structuring matter on a nanometer length scale rather than producing molecularly new species. This article describes a method for synthesizing porous solids from rigid colloidal templates in three steps (see scheme): a) assembly of colloidal particles into a regular array, b) impregnation of the template with monomer(s) and polymerization, and c) removal of the template. For the materials prepared there is a vast number of potential applications ranging from robust catalysts and supports over size- and shape-selective membranes to photovoltaic devices.     

Optimization of Microwave-Assisted Pectin Extraction from Cocoa Pod Husk

Optimization of pectin extraction from cocoa pod husk was carried out to examine independent variables that affect the quality of pectin obtained and determine the best conditions for the extraction process. In this study, three independent variables thought to contribute to microwave-assisted pectin extraction were used, namely, extraction time (20, 25, and 30 min), microwave power (180, 300, and 450 W), and citric acid concentration (2.5%, 5%, and 10%). Response surface methodology was applied using central composite design (CCD) to examine the effect of independent variables on the parameter measured. Among the seven parameters measured, namely, yield, temperature, moisture content, ash content, equivalent weight, methoxyl content, and galacturonic acid content, the statistical analysis test showed that the model equations that were suitable for predicting response values were temperature, moisture content, and ash content. Therefore, the optimization of conditions was only reviewed for these three parameters. Optimization results concluded that the factors that had the most significant effect on temperature, moisture content, and ash content were extraction time and microwave power. Optimal conditions for pectin extraction were at 30 min extraction time, 450 W microwave power, and 10% solvent concentration, resulting in a temperature of 104 °C, moisture content of 6%, and ash content of 8%. Other parameter values measured under these conditions were a yield of 21.10%, equivalent weight of 602.40 mg/mol, methoxyl content of 6.07%, and galacturonic acid content of 72.86%. Pectin extracted from cocoa pod husk using this method has the potential to be further applied, especially in the food and pharmaceutical industries.     

Natural Deep Eutectic Solvent-Based Microwave-Assisted Extraction of Total Flavonoid Compounds from Spent Sweet Potato (Ipomoea batatas L.) Leaves: Optimization and Antioxidant and Bacteriostatic Activity

Natural deep eutectic solvents (NADESs) coupled with microwave-assisted extraction (MAE) were applied to extract total flavonoid compounds from spent sweet potato (Ipomoea batatas L.) leaves. In this study, ten different NADESs were successfully synthesized for the MAE. Based on single-factor experiments, the response surface methodology (RSM) was applied, and the microwave power, extraction temperature, extraction time, and solid–liquid ratio were further evaluated in order to optimize the yields of total flavonoid compounds. Besides, the extracts were recovered by macroporous resin for the biological activity detection of flavonoid compounds. As a result, NADES-2, synthesized by choline chloride and malic acid (molar ratio 1:2), exhibited the highest extraction yield. After that, the NADES-2-based MAE process was optimized and the optimal conditions were as follows: microwave power of 470 W, extraction temperature of 54 °C, extraction time of 21 min, and solid–liquid ratio of 70 mg/mL. The extraction yield (40.21 ± 0.23 mg rutin equivalents/g sweet potato leaves) of the model validation experiment was demonstrated to be in accordance with the predicted value (40.49 mg rutin equivalents/g sweet potato leaves). In addition, flavonoid compounds were efficiently recovered from NADES-extracts with a high recovery yield (>85%) using AB-8 macroporous resin. The bioactivity experiments in vitro confirmed that total flavonoid compounds had good DPPH and O₂⁻· radical-scavenging activity, as well as inhibitory effects on E. coli, S. aureus, E. carotovora, and B. subtilis. In conclusion, this study provides a green and efficient method to extract flavonoid compounds from spent sweet potato leaves, providing technical support for the development and utilization of sweet potato leaves’ waste.     

Efficient Extraction of Total Polyphenols from Apple and Investigation of Its SPF Properties

The purpose of this study was to evaluate the sun protection factor (SPF) of cosmetic emulsions with the addition of hydroalcoholic apple extract. First, the total polyphenolic content, the antioxidant activity and SPF properties of the extracts obtained by sonication and refluxing were evaluated. The two extraction methods were improved using the central composite design. For cosmetic emulsion that contained a different concentration of apple extract (10–40%), a SPF value between 0.51 and 0.90 was obtained. The most efficient apple extract was obtained by reflux using 50% ethanol and a 60 min extraction time. The concentrated extract was incorporated in a cosmetic emulsion whose SPF maximum was 0.90. Accordingly, due to photoprotective properties, the apple extract can be a candidate for use in cosmetic formulations.     

Artificial Intelligence Assisted Ultrasonic Extraction of Total Flavonoids from Rosa sterilis

Flavonoids in Rosa sterilis were studied. The flavonoids in Rosa sterilis were extracted by ultrasonic method, and the extraction conditions were modeled and optimized by response the surface methodology and the artificial intelligence method. The results show that the ultrasonic method can effectively extract total flavonoids, and the extraction rate is close to the prediction value of ANN-GA algorithm, which proves the rationality of the model. The order of the effects of the parameters on the experiment was material liquid ratio > extraction power > extraction time > ethanol concentration. In addition, the scavenging effects of flavonoids on DPPH, O²⁻· and ·OH were also determined, and these indicated that flavonoids have strong antioxidant activities. The kinetics of the extraction process was studied by using the data of the extraction process, and it was found that the extraction process conformed to Fick’s first law.     

Optimization of the Extraction of Proanthocyanidins from Grape Seeds Using Ultrasonication-Assisted Aqueous Ethanol and Evaluation of Anti-Steatosis Activity In Vitro

Conventional extraction methods of proanthocyanidins (PAC) are based on toxic organic solvents, which can raise concerns about the use of extracts in supplemented food and nutraceuticals. Thus, a PAC extraction method was developed for grape seeds (GS) and grape seed powder using food-grade ethanol by optimizing the extraction conditions to generate the maximum yield of PAC. Extraction parameters, % ethanol, solvent: solid (s:s) ratio, sonication time, and temperature were optimized by the central composite design of the response surface method. The yields of PAC under different extraction conditions were quantified by the methylcellulose precipitable tannin assay. The final optimum conditions were 47% ethanol, 10:1 s:s ratio (v:w), 53 min sonication time, and 60 °C extraction temperature. High-performance liquid chromatography analysis revealed the presence of catechin, procyanidin B2, oligomeric and polymeric PAC in the grape seed-proanthocyanidin extracts (GS-PAC). GS-PAC significantly reduced reactive oxygen species and lipid accumulation in the palmitic-acid-induced mouse hepatocytes (AML12) model of steatosis. About 50% of the PAC of the GS was found to be retained in the by-product of wine fermentation. Therefore, the developed ethanol-based extraction method is suitable to produce PAC-rich functional ingredients from grape by-products to be used in supplemented food and nutraceuticals.