乙酸脱除天然竹纤维木质素的研究

以慈竹为研究对象,对常压下乙酸脱除天然竹纤维中的木质素进行了探讨。以反应温度、乙酸体积分数、催化剂硫酸体积分数和反应时间为单因子,考察这些因素对天然竹纤维木质素脱除率的影响。结果表明:影响因素从大到小依次为反应温度、催化剂硫酸体积分数、乙酸体积分数和反应时间。正交试验结果表明,乙酸在脱除天然竹纤维木质素的过程中也脱除了部分半纤维素和纤维素。结合木质素脱除率、半纤维脱除率和纤维素脱除率,得到了最佳工艺条件,即90℃,乙酸体积分数88%,硫酸体积分数0.3%,反应时间3 h,在该条件下木质素的脱除率达到55.84%。     

Microwave-assisted extraction of phenolics with maximal antioxidant activities in tomatoes

Microwave-assisted extraction (MAE) was investigated for extraction of phenolic compounds from tomato with maximised antioxidant activities using response surface methodology (RSM) coupled with a central composite design, and in vitro antioxidant assays (FRAP and ORAC). MAE was more efficient for greater antioxidant activities and higher total phenolic contents than solvent extraction. The optimal MAE processing parameters were 96.5 °C, 2.06 min, 66.2% ethanol for FRAP, and 96.5 °C, 1.66 min, 61.1% ethanol for ORAC. The models were successfully applied to 20 tomato cultivars, whose total phenolic contents (TPC) and indexes (TPI) were 489.30–997.45 mg gallic acid equivalent/100 g dry weight (DW) and 281.34–468.52 mg/100 g DW, respectively. Eight phenolic compounds were identified. Individual phenolics were 6.10–42.73 mg/100 g DW. The FRAP, but not the ORAC value showed good correlation with the TPC or TPI. The methodologies developed and the knowledge acquired in this study will provide useful information to tomato breeders and food processors.     

Optimization of microwave-assisted extraction of triterpene saponins from defatted residue of yellow horn (Xanthoceras sorbifolia Bunge.) kernel and evaluation of its antioxidant activity

Microwave-assisted extraction (MAE) of triterpene saponins from defatted residue of yellow horn (Xanthoceras sorbifolia Bunge.) kernel was optimized in this study. Compared with the conventional extraction methods ultrasonic-assisted extraction (UAE) and heat reflux extraction (HRE), MAE possessed higher efficiency for the extraction of triterpene saponins. The MAE conditions including extraction temperature, extraction duration, irradiation power, ethanol concentration, ratio of solvent to material and extraction cycles were studied and optimized. The optimum extraction parameters were as follows: 51 °C, 7 min, 900 W, 32 ml/g, 42% (v/v) ethanol and 3 cycles. Under the above conditions, the highest extraction yield of triterpene saponins reached 11.62 ± 0.37% of defatted kernel, which was much higher than those of conventional extraction methods. In addition, MAE extract of triterpene saponins exhibited substantial free radical-scavenging activity with an IC₅₀ value of 0.782 mg/ml.

Industrial relevance

Large amounts of defatted kernels of yellow horn are discarded after oil extraction in biodiesel production. It is not only an environmental pollution but also a waste of bioresource. In fact, the residue still has potential for bioactive and medicinal use. Therefore, this study focused on the utilization of defatted kernels of yellow horn by optimizing MAE and evaluation of the antioxidant activity of the resulting extract. MAE provided a better way to deal with defatted kernels of yellow horn as a utilization of waste material of the bioactive resource in food and pharmaceutical industry.     

Microwave-assisted extraction of phenolic antioxidant compounds from peanut skins

A microwave-assisted extraction system was used to extract phenolic antioxidants from peanut skins. The effects of microwave power (10%, 50%, 90% nominal), irradiation time (30, 90, 150 s) and sample mass (1.5, 2.5, 3.5 g) on total phenolic content (TPC), ORAC (oxygen radical absorbance capacity) level and resveratrol content of peanut skin extracts (PSE) were investigated. Peanut skins were extracted with 37.5 ml of 30% ethanol (EtOH) in water. A response surface method was used to estimate optimum extraction conditions, based on TPC, ORAC level and resveratrol content. The maximum predicted TPC, under the optimised conditions (90% microwave power, 30 s irradiation time and 1.5 g skins), was 143.6 mg gallic acid equivalent (GAE)/g skins. The highest ORAC value was 2789 μmol trolox equivalents (TE)/g skins, which occurred at 90% power, 150 s and 1.5 g of skins. Resveratrol was identified in PSE by LC–MS–MS analysis.     

苦参中黄酮类组分的提取及抗氧化性的研究

用正交试验探索超临界萃取苦参中黄酮类组分的最佳工艺条件,最佳参数为:温度40℃,压力30 MPa,乙醇流速0.4 mL/min,时间60 min,最高得率为5.82%.在此基础上对苦参中黄酮类组分进行分离提取,用分光光度法测定其抗氧化性.结果显示苦参中黄酮类组分对自由基有消除作用.     

Comparative antioxidant activity of nanoscale lignin prepared by a supercritical antisolvent (SAS) process with non-nanoscale lignin

Nowadays, lignin antioxidant study is a hot spot. But some properties of lignin make it hard for a wide range of application. To improve lignin antioxidant activity, we employed supercritical antisolvent (SAS) method for preparation of nanoscale lignin (0.144 ± 0.03 μm) using acetone as a solvent and supercritical carbon dioxide as an antisolvent. The nanoscale lignin was characterised by Scanning Electron Microscopy (SEM), Fourier-Transform Infrared Spectroscopy (FTIR) and X-ray Diffraction (XRD). The results showed that SAS process did not result in lignin degradation or chemical structure change. Due to solubility increase, many antioxidant parameters of the nanoscale lignin were obviously enhanced, including DPPH radical scavenging activity, superoxide radical scavenging activity and reducing power. As an antioxidant, the nanoscale lignin was a better material than the non-nanoscale lignin. Our study was to promote the lignin application in animal husbandry, pharmaceutical and food processing industries.     

Effects of supercritical fluid extraction parameters on lycopene yield and antioxidant activity

The effects of various parameters of supercritical carbon dioxide (SC-CO₂) fluid extractions of tomato skins on the extraction yields and antioxidant activities of lycopene-rich extracts were investigated. A Box–Behnken design was applied to study the effects of three independent variables (temperature ranging from 40 to 100 °C, pressure ranging from 20 to 40 MPa, and flow rate ranging from 1.0 to 2.0 mL/min) on lycopene yield. The model showed good agreement with the experimental results, by the coefficient of determination (r² = 0.9834). Temperature, pressure, and the quadratic term for the temperature of SC-CO₂ extraction were large significantly positive factors affecting lycopene yield (P < 0.05). The maximum total lycopene content of 31.25 μg/g of raw tomato was extracted at the highest temperature of 100 °C, 40 MPa and 1.5 mL/min. TEAC assay was applied to assess the antioxidant activity of lycopene-rich extracts from SC-CO₂ fluid extraction. The effects of SC-CO₂ fluid extraction parameters on the antioxidant activities of the extracts differed with the yield. For each unit of lycopene extract, the antioxidant activity level was constant below 70 °C, but then gradually decreased above 70 °C due to isomerization occurring as a result of the higher temperature. The ratio of all-trans-lycopene to the cis-isomers changed from 1.70 to 1.32 when the operating temperature was adjusted from 40 to 100 °C, indicating an increased bioavailability due to the generation of the cis-isomers. No significant effects of pressure or flow rate of SC-CO₂ fluid extraction on the antioxidant activity were observed.     

Optimized microwave-assisted extraction of total phenolics (TP) from Ipomoea batatas leaves and its antioxidant activity

An efficient microwave-assisted extraction (MAE) technique was employed to extract total phenolics (TP) from sweetpotato [Ipomoea batatas (L.) Lam.] leaves (TPSL). The optimal conditions for microwave-assisted extraction of TPSL were determined by response surface methodology. A face-centered cubic design (FCD) was applied to evaluate the effects of three independent variables (microwave power, extraction time and ethanol proportion) on the recovery of TPSL. The correlation analysis of the mathematical-regression model indicated that quadratic polynomial model could be employed to optimize the microwave extraction of TPSL. From response surface plots, microwave power, extraction time and ethanol proportion exhibited independent and interactive effects on the extraction of TPSL. The optimal conditions to obtain the highest recovery of TPSL were as follows: microwave power, 302 W; extraction time, 123 s; ethanol proportion, 53% (v/v). Under these optimal conditions, the experimental values agreed with the predicted ones by analysis of variance. It indicated high fitness of the model used and the success of response surface methodology for optimizing TPSL extraction. After method development, the antioxidant activity of the MAE extract was preliminarily evaluated. MAE showed obvious advantages in terms of high extraction efficiency and antioxidant activity of extract with in shortest extraction time.Industrial Relevance: Sweet potato leaves have been neglected except for a partial use as livestock feed in China. This study describes the response surface optimization of microwave-assisted extraction (MAE) process for the enhanced recovery of total phenolics from sweetpotato leaves (TPSL). MAE showed obvious advantages in terms of high extraction efficiency and antioxidant activity of extract within shortest extraction time. TPSL obtained using MAE showed potential for use in health-care food and pharmaceutical industry.     

Ethanol modified supercritical fluid extraction and antioxidant activity of cajaninstilbene acid and pinostrobin from pigeonpea [Cajanus cajan (L.) Millsp.] leaves

Supercritical fluid carbon dioxide (SF-CO₂) extraction (SFE) of cajaninstilbene acid (CSA) and pinostrobin (PI) from pigeonpea leaves and antioxidant activity were investigated for the first time. SFE gave higher extraction yields than conventional heat-refluxing extraction (HRE) because of the severe breakage of cell morphology caused by SF-CO₂, which was observed by scanning electron microscopy (SEM). CO₂ flow rate, modifier composition and liquid to solid ratio were firstly optimised, 12 kg/h, and 80% EtOH with a liquid to solid ratio of 10 ml/g raw material exhibited better extraction performance. Then a central composite design (CCD) combined with response surface methodology was used to study the effects of extraction pressure, temperature and time on the extraction yields of CSA and PI, the optimal parameters were 30 MPa, 60 °C and 2 h. An antioxidant activity investigation showed SFE extracts exhibited better free radical-scavenging activity than HRE extracts with an IC₅₀ value of 0.2259 mg/ml.     

Microwave-assisted extraction of betalains from red beet (Beta vulgaris)

The use of microwave assisted extraction (MAE) was investigated in this work for the extraction of betalains from diced red beets. Several treatments with different combinations of time, power and duty cycle applied to the samples were studied. The combination of 400 W and 100% duty cycle for 90–120 s resulted in the highest amount of recovered betanines; whereas at 140–150 s the highest amount of betaxanthins was obtained. The addition of ascorbic acid (0.040 mol/L) to the extracting solvent and the development of a two-step MAE process with a cooling period in-between and after processing steps led to an enhancement in the amount of pigments obtained. The effect of extraction time at each extraction step on betalains yield was determined by applying a factorial design and surface plots were constructed. The duration of the second step significantly affected the yield of betanines and betaxanthins obtained (p < 0.05). A prediction model was proposed and validated to meet the optimal extraction times. Betalain yields obtained by MAE were twice as high as those obtained during conventional extraction and conventional extraction at 80 °C.     

Microwave-assisted extraction of free amino acids from foods

 A microwave-assisted solvent extraction technique was developed for the extraction of free amino acids from foods. Four different samples were subjected to microwave extraction with varying amounts of extractant at several temperature values, for varying times to determine optimum extraction conditions. The extractions were performed with or without shaking the vessels in order to investigate the effects of mixing on the extraction efficiency and reproducibility. A comparison was made between this method and the traditional 1 h shaking extraction. The experiments indicated that the microwave-assisted extraction is an effective technique for the extraction of free amino acids from samples of plant or animal origin. The extraction yields obtained by the microwave method were about 10% better than by the conventional shaking technique. The times needed for the complete sample preparations were reduced by 66% with the application of microwaves. Received: 10 October 1997 / Revised version: 23 January 1998     

Subcritical water extraction of antioxidant compounds from Seabuckthorn (Hippophae rhamnoides) leaves for the comparative evaluation of antioxidant activity

A novel environmentally friendly technique, subcritical water extraction (SWE) was employed for the extraction of antioxidant compounds from Seabuckthorn leaves (SBT). Antioxidant activity of the extracts was evaluated using commonly accepted chemical assays. Also, present study reports the cytoprotective and antioxidant properties of SBT against tertiary-butyl hydroperoxide (tert-BOOH) induced oxidative stress in murine macrophages (Raw 264.7). Exposure of cells to tert-BOOH resulted, increase in cytotoxicity, reactive oxygen species (ROS) production and decrease in mitochondrial membrane potential, which is responsible for fall in intracellular antioxidant levels. Pretreatment of cells with SBT extracts inhibited cytotoxicity, ROS production and maintained antioxidants levels similar to that of control cells.     

The antioxidant capacity of polysaccharide from Laminaria japonica by citric acid extraction

An optimal citric acid extraction condition (pH 2.0; extraction temperature: 120 °C; extraction time: 3 h) was developed to obtain polysaccharide from Laminaria japonica. The yield of polysaccharide was 13.31 ± 0.08%, with IC₅₀ value of DPPH radical scavenging activity of 0.98 ± 0.01 mg mL^?1. The viscosity of polysaccharide extracted by citric acid (LJPA) was eight times lower than that of polysaccharide extracted by hot water (LJPW), which may be attributed to the low average molecular weight of LJPA (17.12 kDa). Gas chromatography analysis indicated that LJPA was composed of rhamnose, fucose, xylose, manose, glucose and galactose with relative molar percentages of 4.51%, 20.27%, 12.43%, 12.81%, 10.29% and 39.69% respectively. Furthermore, LJPA exhibited significantly higher antioxidant capacities including oxygen radical absorbance capacity (ORAC), ABTS radical scavenging activity and reducing power than LJPW. Citric acid extraction showed a positive influence on the polysaccharide degradation and antioxidant capacities of L. japonica.     

A remarkable influence of microwave extraction: Enhancement of antioxidant activity of extracted onion varieties

Four (red, yellow, white and grelot onion) varieties of Allium cepa, a rich source of quercetin (flavonol) glycosides, were studied for their total content of reducing compounds (TCRC), flavonol content and antioxidant activity evaluation. Extracts obtained by solvent free microwave hydrodiffusion and gravity (MHG) technique and conventional solvent extraction (CSE) were analysed with high performance liquid chromatography (HPLC) for quantification of flavonoids. Three different methods were selected for evaluating the antioxidant capacity of the different onion varieties (after the determination of their phenolic content by the Folin–Ciocalteu method): the reduction of the stable DPPH (2,2-diphenyl-1-picrylhydrazyl) radical, the ORAC (oxygen radical absorbance capacity) method, and the inhibition of the AAPH-induced peroxidation of linoleic acid in SDS micelles. The highest antioxidant capacity was observed for red onion, followed by yellow, white and grelot onion. In spite of the low recovery of extractable flavonoids (quercetin 3,4′-diglucoside, 4′-glucoside and 3-glucoside), MHG remained the preferred extraction method in comparison to the conventional method, as all the samples obtained under microwave-assisted extraction (MAE) exhibited the highest antioxidant activities in all the tests. Also the microscopic observations of extracted tissues showed that at cellular level, microwaves induced disruptions of vacuoles and cell walls thus promoting the effectiveness of this method.     

Mechanochemical‐assisted extraction and antioxidant activity of polysaccharides from Ganoderma lucidum spores

Mechanochemical‐assisted extraction (MCAE) method was developed to an effective method for polysaccharides extraction from Ganoderma lucidum spores. The MCAE parameters and the antioxidant activity of polysaccharides were investigated. Through response surface methodology design experiments, the processing conditions were optimised as follows: material/solid reagent (Na₂CO₃) 5 g·g^?1, milling time 20 min, solution/material ratio twenty (mL·g^?1) and extraction time 130 min. Under these conditions, the yield of polysaccharides was (5.92 ± 0.13)%, which was in close agreement with the predicted value. Compared with the heat‐reflux extraction method, the MCAE method had higher extraction yield, shorter extraction time and lower extraction temperature. In addition, the polysaccharides obtained from MCAE exhibit significant antioxidant activity.     

The antioxidant, angiotensin converting enzyme inhibition activity, and phenolic compounds of bamboo shoot extracts

This study was undertaken to evaluate the functional properties of two of the most popular species of edible bamboo shoots in Korea (Phyllostachys pubescens and Phyllostachys nigra). Powdered bamboo shoots were extracted with methanol and an aqueous suspension of the obtained methanol extract was partitioned successively with chloroform, ethyl acetate, and butanol, leaving a residual water extract. All obtained extracts were evaluated for their antioxidant capacity and antimicrobial activity, angiotensin converting enzyme (ACE) inhibition activity, and ascorbic acid and phenolic compound content. Methanol and water fractions showed a particularly high ascorbic acid contents. The ethyl acetate fraction contained a high concentration of phenolic compounds. Among all extracts, the ethyl acetate and butanol fractions showed particularly high antioxidant activity. Methanol extract had a significantly higher ACE inhibitory activity than other extracts. None of the extracts inhibited the tested bacteria.     

Microwave-assisted extraction of phenolic compounds from tea residues under autohydrolytic conditions

Phenolic compounds were extracted from three kinds of tea residues (green, oolong and black tea residues) by microwave-assisted extraction in water under autohydrolytic conditions without using any catalyst or organic solvent. Productions of phenolic compounds were enhanced by microwave heating at 230 °C. The main phenolic constituent in the extract from green tea residue was pyrogallol (24.6%) which was estimated to be originated from degradations of catechins. Derivatives of guaiacyl units of lignin such as dihydroconiferyl alcohol (10.3%) and vanillin (8.1%) were, however, the main constituents in oolong tea residue. In the case of black tea residue, derivatives of both catechins and lignin were comparably extracted. These phenolic compounds are interesting as a bio-based chemical feedstock such as phenolic precursors and antioxidants.     

Investigation of the effects of different organosolv pulping methods on antioxidant capacity and extraction efficiency of lignin

Different organosolv pulping methods delignified raw materials (Acanthopanax senticosus remainder) were investigated, including acetone-acetic acid-water method (8/1/1, v/v/v), 1,4-butanediol-acetic acid-water method (8/1/1, v/v/v), ethanol-acetic acid-water method (8/1/1, v/v/v) and acetic acid-water method (4/1, v/v). Lignin extraction efficiency and antioxidant capacity from different organosolv methods were compared.The results showed that the lignin extraction efficiency of the 1,4-butanediol-acetic acid-water method was the highest (39%) among methods of this paper. The lignin from acetic acid-water method was the most effective free radical scavengers, whose 1,1-di-phenyl-2-picrylhydrazyl (DPPH) radical scavenging capacity (IC₅₀) was about 0.6587 mg/ml.Acanthopanax senticosus remainder (raw materials) and pulps were characterised by scanning electron microscopy (SEM) and pulps strength properties. All lignin samples were analysed by Fourier-transform Infrared Spectroscopy (FTIR). The results showed that organosolv pulping process had large influence on pulps morphology, pulps strength properties and lignin structure.     

Optimisation of microwave‐assisted extraction of phenolic compounds from broccoli and its antioxidant activity

The effect of independent variables of microwave‐assisted extraction (MAE), extraction temperature (50–90 °C), microwave power (100–200 W), solvent concentration (methanol/water, 50–90%, v/v) and extraction time (1–27 min) on total phenolics and flavonoids contents as well as antioxidant activity of broccoli extracts was investigated. Response surface methodology was successfully applied for optimisation and the high correlation of the mathematical model indicated that a quadratic polynomial model could be used for optimisation of investigated responses. Considering the maximum amount of extracted total phenolics, total flavonoids and antioxidant activity expressed as ORAC value, the optimal conditions for all three investigated responses were obtained (temperature ?71.11 °C; microwave power ?167.03 W; solvent concentration ?75.95%; and extraction time 16.34 min), which is in agreement with optimal conditions obtained for each investigated responses. The development of simultaneously MAE methods for total phenolics, total flavonoids and antioxidant activity of broccoli extracts might simplify assessment of broccoli as valuables source of antioxidants.     

Influence of solvent and temperature on extraction of phenolic compounds from grape seed,antioxidant activity and colour of extract

This study was aimed to investigate the influence of solvent (water and ethanol in concentration: 50%, 70% and 96%) and extraction temperature (25–80) °C on polyphenols extraction of grape seed (Vitis vinifera L. cv. “Frankovka”) cultivated in Eastern Croatia. The best results were reached using 50% ethanol at 80 °C. The most abundant individual polyphenolic compound was catechin which makes the average of 45.11% of the total phenolic content followed by epicatechin (34.45%), procyanidin B₂ (12.90%), gallic acid (5.34%), gallocatechin (1.58%), epicatechin gallate (1.01%). The antioxidant activity of extracts was determined by DPPH‐method and it was highly dependent on extraction solvent and temperature. The total extractable proanthocyanidins content of extract had the highest positive correlation (r = 0.994) with antioxidant activity, which indicated that these compounds might be the most important antioxidant in examined grape seed extracts. Relationship between phenolic content and colour of extracts was observed.