Optimisation of accelerated solvent extraction of antioxidant compounds from rosemary (Rosmarinus officinalis L.), marjoram (Origanum majorana L.) and oregano (Origanum vulgare L.) using response surface methodology

The present study optimised the accelerated solvent extraction (ASE) conditions (Dionex ASE® 200, USA) to maximise the antioxidant capacity of the extracts from three spices of Lamiaceae family; rosemary, oregano and marjoram. Optimised conditions with regard to extraction temperature (66–129 °C) and solvent concentration (32–88% methanol) were identified using response surface methodology (RSM). For all three spices results showed that 129 °C was the optimum temperature in order to obtain extracts with high antioxidant activity. Optimal methanol concentrations with respect to the antioxidant activity of rosemary and marjoram extracts were 56% and 57% respectively. Oregano showed a different response to the effect of methanol concentration and was optimally extracted at 33%. The antioxidant activity yields of the optimal ASE extracts were significantly (p < 0.05) higher than solid/liquid extracts. The predicted models were highly significant (p < 0.05) for both total phenol (TP) and ferric reducing antioxidant property (FRAP) values in all the spices with high regression coefficients (R²) ranging from 0.952 to 0.999.     

Antimicrobial, antioxidant and phytochemical investigations of sea buckthorn (Hippophaë rhamnoides L.) leaf, stem, root and seed

The antimicrobial and antioxidant activities of crude ethanolic extract from Hippophaë rhamnoides L. (Elaeagnaceae) leaf, stem, root and seed, and their respective fractions, obtained by liquid-liquid extraction (LLE) using hexane (HF), ethyl acetate (EAF) and water (WF), were investigated. The crude extract was obtained by Pressurised Liquid Extraction (PLE), using ethanol at 100 bar and 60 °C. Antimicrobial activity was tested against food-borne and clinical microorganisms. Antioxidant activity was measured using the DPPH-radical scavenging and the ferric reducing antioxidant power (FRAP) assays. The phytochemical contents were examined by colorimetric methods. The results showed that crude extracts were active against Gram − and + strains, and that seed and root extracts were better radical scavengers than leaf and stem extracts. For all organs, the two activities tested were found to be higher in WF. These activities were correlated with the presence of phenolic compounds in active fractions. High Performance Thin Layer Chromatography (HPTLC) fingerprints confirmed presence of phenolic compounds in active extracts and fractions.     

The antioxidative properties of Holy basil and Galangal in cooked ground pork

The ethanolic extracts from Holy basil and Galangal were examined for their extraction yield, total phenolic content, antioxidant activity against a β-carotene-linoleic acid emulsion system, DPPH scavenging activity and reducing power. Ethanolic extracts of Holy basil exhibited higher extraction yield, total phenolic content, antioxidant activity, DPPH scavenging activity and reducing power than ethanolic extracts of Galangal. Antioxidative efficiency to inhibit lipid oxidation of dried Holy basil and dried Galangal powder, ethanolic extracts of Galangal and Holy basil and commercial antioxidant mixture in cooked ground pork was investigated during refrigerated storage at 5°C for 14 days. The quantitative measurements of thiobarbituric acid reactive substances (TBARS), conjugated diene, peroxide value (POV) and hexanal content were used as indicators of lipid oxidation. Increased levels of TBARS value, POV and hexanal content were noticed in all meat samples during storage, however most marked in cooked ground pork without antioxidants, whereas conjugated diene tended to decrease with increasing storage time. Ranking of the treatment in order of their antioxidant effectiveness showed that commercial antioxidant mixture (0.3% citric acid+0.5% ascorbic acid+0.02% α-tocopherol)>dried Galangal powder>dried Holy basil powder>ethanolic extracts of Galangal>ethanolic extracts of Holy basil>control. Furthermore, in cooked ground pork samples a high correlation between TBARS value and hexanal contents was obtained.     

Antioxidant activity and phenolic content of pressurised liquid and solid–liquid extracts from four Irish origin macroalgae

The efficiency of solid–liquid extraction (SLE) and pressurised liquid extraction (PLE) for the recovery of antioxidant and polyphenols from the Irish macroalgae, Fucus serratus, Laminaria digitata, Gracilaria gracilis and Codium fragile, was assessed using the 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH) and ferric reducing antioxidant power (FRAP) assays and the Folin–Ciocalteu total phenol content (TPC) assay. Fucus serratus had TPC and antioxidant activities thirty times higher than the other species. Solid–liquid extraction cold water (CW_SLE) had the highest TPC (81.17 μg GAE mg^?1 sample) derived from F. serratus, compared with the TPC of 61.12 μg GAE mg^?1 sample for the corresponding PLE extract. For both SLE and PLE extracts, low TPC levels were observed in L. digitata, G. gracilis and C. fragile. The majority of SLE extracts possessed higher FRAP and DPPH activities compared with their PLE counterparts. This study indicates that the high temperatures and pressures in PLE did not enhance the antioxidant activities relative to conventional SLE extraction.     

Effect of milling time on antioxidant compounds and activities of methanol extracts of sorghum [Sorghum bicolor (L.) Moench]

Antioxidant compounds and activities of methanol extracts of sorghum for different milling times were investigated. Total polyphenol, flavonoid, and tannin contents were measured using spectrophotometric methods. Methanol extracts were also evaluated for antioxidant activities based on DPPH and ABTS radical-scavenging activities. As milling rates increased, milling recovery and a value decreased, while L and b values increased. The extraction yield, antioxidant compound contents, and antioxidant activities of sorghum grain decreased with increasing milling rates. Methanol extracts from sorghum bran generally showed higher antioxidant activities than extracts from sorghum grain. The antioxidant content was higher in sorghum bran extracts than in grain extracts. A significant (p<0.05) correlation was observed between free radical-scavenging activity and the content of polyphenolic compounds. Sorghum bran exhibited antioxidant activities that may have important health benefits.     

紫皮豇豆(Vigna unguiculata L.)花色苷的研究

首次应用高效液相色谱-二极管阵列检测器-质谱联用技术(HPLC-DAD-MS)鉴定出紫皮豇豆主要含有三种花色苷,分别为飞燕草色素、矢车菊色素、天竺葵色素的葡萄糖苷,其中矢车菊葡萄糖苷相对百分含量达到93.4%;应用pH示差法测定出其单体花色苷的含量为57.15mg/100g鲜重;应用DPPH法测定结果显示,花色苷粗提液有较强的抗氧化能力。     

Effect of an acid treatment on the phytochemical and antioxidant characteristics of extracts from selected Lamiaceae species

Aqueous-methanol extracts were prepared from basil (Ocimum basilicum L.), bay (Laurus nobilis L.), oregano (Origanum vulgare L.), rosemary (Rosmarinus officinalis L.), sage (Salvia officinalis L.), savory (Satureja hortensis L.) and thyme (Thymus vulgaris L.) by maceration and their phytochemical and antioxidant characteristics were assessed. Each extract was submitted to an acid treatment (1.2 N HCl in 50% methanol) to determine whether such a process had an effect upon their chemistry and antioxidative efficacy. The treatment appeared to have improved the antioxidant potency of the extracts in general; however, there were some exceptions. The treatment did not increase the Fe(III) reductive activity of the extracts from basil or bay samples nor the ability of the oregano and sage extracts to scavenge 1,1-diphenyl-2-picrylhydrazyl radicals at pH 7.4. The Folin-Ciocalteu phenol content of the basil extract was not increased with acid treatment.     

Rapid screening of antioxidant activity of sage (Salvia officinalis L.) extracts obtained by supercritical carbon dioxide at different extraction conditions.

Sage herb (Salvia officinalis L.) was extracted at supercritical fluid extraction (SFE) conditions with carbon dioxide at different parameters and the extracts tested on their antioxidant activity (AA). SFE of sage herb at 35 MPa pressure was found to be an effective method to obtain pure extracts. The yields of the extracts were substantially increased by using 1% of entrainer solvent ethanol. The fractionation of sage extract was a complex procedure in terms of extract distribution between separators operating at various pressure and temperature conditions. It was also proved by testing the AA of the extracts in rapeseed oil. The effect of the extracts on the rapeseed oil weight gain varied in a wide range (from 'very low' to 'high') depending on the fractionation conditions. Preliminary results showed that to obtain more effective antioxidant fractions separation steps should be started at 10 MPa lower pressure than that used for the extraction.     

Influence of the phenophase on the phenolic profile and antioxidant properties of Dalmatian sage

This study aimed to research the influence of phenophase on the phenolic profile (phenolic acids, flavonoids and stilbenes) and related antioxidant properties of sage, one of the most characteristic plants of Dalmatian karst. The total phenol and flavonoid contents in sage leaves were determined spectrophotometrically, while the principal phenolics were determined using HPLC-RP-DAD. Antioxidant properties of this well known medicinal plant were determined as free radical scavenging activity (DPPH), ferric reducing/antioxidant power (FRAP) and by Briggs-Rauscher oscillating reaction (BR). The results strongly indicate that Dalmatian sage leaves are rich source of valuable phenolics, mainly phenolic acids, with extremely good antioxidant properties. The presence of resveratrol or its derivatives was confirmed in all extracts. The best results for total phenols and flavonoids, as well as the best antioxidant properties were obtained for May sage, while the highest amounts of catechin monomers and compounds from group of stilbenes were found in February extract.     

Rapid screening of antioxidant activity of sage (Salvia officinalis L.) extracts obtained by supercritical carbon dioxide at different extraction conditions

Sage herb (Salvia officinalis L.) was extracted at supercritical fluid extraction (SFE) conditions with carbon dioxide at different parameters and the extracts tested on their antioxidant activity (AA). SFE of sage herb at 35 MPa pressure was found to be an effective method to obtain pure extracts. The yields of the extracts were substantially increased by using 1% of entrainer solvent ethanol. The fractionation of sage extract was a complex procedure in terms of extract distribution between separators operating at various pressure and temperature conditions. It was also proved by testing the AA of the extracts in rapeseed oil. The effect of the extracts on the rapeseed oil weight gain varied in a wide range (from ‘very low’ to ‘high’) depending on the fractionation conditions. Preliminary results showed that to obtain more effective antioxidant fractions separation steps should be started at 10 MPa lower pressure than that used for the extraction.     

纤维素酶水解处理提高燕麦全粉中总多酚含量与抗氧化活性

采用Folin-酚法和高效液相色谱法考察了纤维素酶水解处理对燕麦粉中总多酚及多酚组分含量的影响,并利用2,2’-联氮双-（3-乙基苯并噻唑啉-6-磺酸）二铵盐（2,2’-azinobis (3-ethylbenzothiazoline-6-sulfonic acid)diammonium salt,ABTS）自由基、1,1-二苯基-2-三硝基苯肼（1,1-diphenyl-2-picrylhydrazyl,DPPH）自由基清除能力、铁离子还原能力（ferric reducing antioxidant power,FRAP）和蛋白损伤修复等方法测定酶解前后提取液的体外抗氧化活性。结果表明：酶解处理以后可显著增加燕麦粉中总多酚含量,尤其是阿魏酸含量提高了11～24 倍;酶解处理后燕麦粉多酚提取物的ABTS＋·、DPPH自由基清除能力和FRAP值等体外抗氧化活性和蛋白氧化损伤修复能力得到显著增强。总体而言,纤维素酶水解处理能够有效提高燕麦粉中总多酚含量及其功能活性,主要原因可能是阿魏酸等酚酸物质含量的提高。     

红薯叶不同溶剂提取物抗氧化性及活性成分鉴定

研究不同极性溶剂对红薯叶中酚类化合物的提取以及提取物抗氧化性的影响,并鉴定提取物中的主要抗氧化成分组成。分别采用极性不同的7 种溶剂（蒸馏水、甲醇、无水乙醇、丙酮、正丁醇、乙酸乙酯和氯仿）从红薯叶中提取多酚,并评价提取物中总酚、总黄酮和花青素的含量,以及对1,1-二苯基-2-三硝基苯肼（1,1-diphenyl-2-picrylhydrazyl,DPPH）自由基清除能力和还原能力,最后运用高效液相色谱-串联质谱（high performance liquidchromatography tandem mass spectroscopy,HPLC-MS/MS）技术分析抗氧化活性最好的提取物中多酚的主要组成成分。结果表明：提取溶剂的极性对红薯叶中多酚类化合物的提取效率和提取物抗氧化活性有很大的影响,水提物具有最高的粗提物得率（（37.13±1.60）%）,而甲醇提取物中总酚含量（13.80 mg GAE/g）和总黄酮含量（（5.68±0.35）mg QE/g）最高,且具有最好的DPPH自由基清除能力（IC50为0.32 mg/mL）与还原能力（ρ0.5为0.95 mg/mL）。采用HPLC-MS/MS从红薯叶甲醇提取物中鉴定9 种、初步鉴定3 种酚类化合物,鉴定的化合物为咖啡酸、对羟基苯甲酸、1-咖啡酸奎宁酸、3-咖啡酸奎宁酸、异绿原酸A、异绿原酸B、异绿原酸C、3,4,5-三咖啡酰奎尼酸和金丝桃苷。     

马齿苋不同溶剂提取物的抗氧化活性

研究马齿苋不同溶剂提取物的抗氧化能力。以水、70%甲醇、70%乙醇和70%丙酮为提取溶剂,通过清除DPPH·、ABTS^+、·OH及FRAP法评价马齿苋不同溶剂提取物的抗氧化作用,并测定提取物的总多酚、总黄酮含量。结果表明,马齿苋不同溶剂提取物在4种抗氧化评价体系中均表现出一定的抗氧化活性, 70%丙酮提取物抗氧化活性最强,总多酚含量最高。70%丙酮可作为马齿苋抗氧化活性成分提取的优选溶剂,而总多酚含量可作为马齿苋抗氧化提取物的质量评价指标。     

Neuroprotective potential of some terebinth coffee brands and the unprocessed fruits of Pistacia terebinthus L. and their fatty and essential oil analyses

In the current study, neuroprotective effects of the ethyl acetate and methanol extracts of four terebinth coffee brands and the fruits of Pistacia terebinthus L. were investigated through enzyme inhibition tests against acetylcholinesterase, butyrylcholinesterase, and tyrosinase as well as antioxidant test systems. Antioxidant activity was measured using radical scavenging activity tests and metal-related tests including metal-chelation capacity, ferric-reducing antioxidant power (FRAP), and phosphomolybdenum reducing power (PRAP). The fatty oils of the coffee brands and the fruits and the fruit essential oil were examined by GC–MS. Total phenol and flavonoid contents were calculated spectrophotometrically. The extracts had moderate inhibition against butyrylcholinesterase (9.78–45.74% at 200 μg mL⁻¹) and potent scavenging activity against DPPH. They exerted strong activity in FRAP and metal-chelation tests and modest activity in PRAP test. Oleic acid was identified as the major fatty acid in the fatty oils, while α-pinene (26.31%) was dominant in the essential oil.     

Valorization of sage extracts (Salvia officinalis L.) obtained by high voltage electrical discharges: Process control and antioxidant properties

Study explored high voltage electrical discharge (HVED) for recovery of bioactive compounds from Dalmatian sage. HVED parameters were: treatment time (3, 9 min), ethanol content (0, 25, 50%, v/v), voltage for argon (15, 20 kV) and nitrogen (20, 25 kV). Findings were compared to conventional extraction (CE) with assessment of total phenolic content (TPC), antioxidant activity (EPR), NIR spectroscopy, colorimetric parameters, Fourier-transform infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). Raw sage was analyzed for pesticide residues and heavy metals. The optimal HVED extraction expressed as TPC 57.21 mg GAE/g was obtained with nitrogen/9 min/25 kV/33% of ethanol. Sage is safe for extraction in terms of pesticide residues and heavy metals. HVED electroporation facilitated the extraction of bioactive compounds and produced extracts with high antioxidant potential, thus confirmed HVED as “green” extraction for sustainable functional food production.     

Influence of pressurised liquid extraction and solid–liquid extraction methods on the phenolic content and antioxidant activities of Irish macroalgae

The efficiencies of pressurised liquid extraction (PLE) and a traditional solid–liquid extraction (SLE) at extracting antioxidant polyphenols from Irish macroalgae Ascophyllum nodosum, Pelvetia canaliculata, Fucus spiralis and Ulva intestinalis were compared. PLE was more effective for extracting polyphenols with acetone/water (80:20); however, when food‐friendly solvents of ethanol/water (80:20) and water were employed, SLE resulted in higher phenolic content in brown macroalgal extracts. For example, the Fucus spiralis SLE water and ethanol/water extracts displayed total phenolic contents (TPCs) of 130.58 ± 2.78 and 142.81 ± 1.77 μg phloroglucinol equivalents (PGE) mg^?1 sample, respectively, compared with TPCs of 90.79 ± 1.16 and 124 ± 6.54 μg PGE mg^?1 sample for the corresponding PLE extracts. All SLE aqueous ethanolic macroalgal extracts possessed higher DPPH radical scavenging abilities (RSA) and ferric reducing antioxidant power (FRAP) than their PLE equivalents . This study indicates that the application of high extraction temperatures (50–200 °C) and pressures (500–3000 psi) used in PLE does not enhance the antioxidant activities of macroalgal extracts relative to SLE extraction. The ability to produce antioxidant food‐friendly macroalgal extracts using SLE could represent significant cost reductions on an industrial scale further enhancing the potential of macroalgal polyphenols to be used in functional food preparations.     

Radiation-induced enhancement of antioxidant activity in extracts of rosemary (Rosmarinus officinalis L.)

Dry rosemary leaf powder was subjected to 30 kGy of gamma ray irradiation, followed by solvent extraction with methanol, ethanol or water. The antioxidant activity of the extracts was assessed using the DPPH radical-scavenging method and the reducing power test. EC₅₀ values, using the radical-scavenging method, indicate a 22% increase in the antioxidant activity of ethanol and water extracts as a result of irradiation treatment. EC₅₀ values in the reducing power test show an increase of 45% and 28% for the ethanol and water extracts, respectively. The antioxidant activity of methanol extracts of irradiated rosemary remained the same as in the controls in both types of test. A high correlation was found between the EC₅₀ values obtained in the DPPH radical test and those from the reducing power test. Total phenolic content (Folin–Denis test) increased by 35% in the water extracts as a result of irradiation but remained the same in the methanol and ethanol extracts. The methanol extract showed the highest antioxidant activity and the highest amount of total phenolic compounds. Radiation reduced the good correlation between antioxidant activity and total phenolic content.     

Antioxidant activity and phenolic composition of sumac (Rhus coriaria L.) extracts

Antioxidant activity and phenolic compounds of sumac extracts were investigated. Sumac was extracted in methanol and subjected to solvent–solvent partitioning to yield two fractions as ethyl acetate and aqueous. Methanol extract was further fractioned over Sephadex LH-20 column. Antioxidant activity of extracts and fractions were screened using ferric thiocyanate and DPPH radical scavenging methods. Phenolic composition of active fraction(s) was determined by HPLC–MS systems. Those fractions which exhibited strong antioxidant activity were rich in anthocyanins and hydrolysable tannins. While gallic acid was the main phenolic acid in the extracts, anthocyanin fraction contained cyanidin, peonidin, pelargonidin, petunidin, and delphinidin glucosides and coumarates. Pentagalloyl glucose was abundant in the hydrolysable tannin fraction. Effective scavenging concentration (EC₅₀) on DPPH radical was 0.70 μg/mL both in ethyl acetate and tannin fractions, and 5.33 μg/mL in anthocyanin rich fraction. Same extracts and fractions showed moderate lipid peroxidation inhibition effect compared with the synthetic antioxidants. The findings demonstrate that sumac can be used as a natural antioxidant.     

Culinary herbs inhibit lipid oxidation in raw and cooked minced meat patties during storage

The effect of dried spices and the ethanol extract of those spices was studied on the stability of fresh chicken minced meat, and fresh and cooked pork patties pretreated with NaCl during refrigerated and frozen storage. The antioxidant activities of the spices were measured by thiobarbituric acid reactive substances (TBARS) and peroxide value (POV) in meat samples. The lipid oxidation was effectively inhibited in the chicken meat treated with several dry spices diminishing the TBARS to a range of 32% and 83% of those found in the control samples in frozen stored meat for 6 months. Marjoram, wild marjoram and caraway were the most effective dry spices. Ethanolic extracts of the same spices were more potent as antioxidants by lowering the concentration of the TBARS to a range of 20–27% of those found in the control samples. Addition of sodium salt to the minced pork resulted very high concentrations of the oxidation products originated from the polyunsaturated fatty acids. The treatment with ethanolic extract of spices (sage, basil, thyme and ginger) significantly inhibited the lipid peroxidation in refrigerated and chilled pork patties pretreated with NaCl by reducing both POV and TBARS. Heat treatment with microwaves produced significantly elevated levels of both lipid peroxides and TBARS, but the amount of these oxidation products was less than 10% in spice‐treated salted meat samples compared to that in untreated ones. Lipid peroxidation also grew continuously during the storage period at −18°C in raw and cooked samples. Ethanolic extracts of spices had a very strong antioxidative effect inhibiting lipid peroxidation in heat‐treated meat products during frozen storage. The highest antioxidant activity was observed in the case of ginger. High correlation coefficients were found between TBARS and POV both in raw and cooked pork patties (0.86, 0.91, respectively) during frozen storage. It is supposed that these compounds originated from the polyunsaturated fatty acids during oxidation processes but at different stages. Utilization of spices, spice mixtures or spice extracts in semi‐prepared meat products intended to be frozen for up to 6 months or more before consumption is proved to be advantageous in regard of shelf life of the food, as well as of human health, because of the beneficial effect of spices in inhibition of lipid peroxidation during heat treatment and chilling storage. © 1999 Society of Chemical Industry     

两种方法测定香辛料提取物抗氧化活性的比较

本实验分别采用TBARS(硫代巴比妥酸反应物)法和FRAP(还原能力)法研究七种香辛料95%乙醇提取物的抗氧化作用。结果表明,七种香辛料提取物均有较好的抗氧化和还原能力。TBARS法测定抗氧化能力大小依次为:甘草>迷迭香>肉豆蔻>姜黄>丁香>白豆蔻>桂皮;FRAP法测定还原能力大小为:丁香>桂皮>肉豆蔻>迷迭香>姜黄>甘草>白豆蔻。两种方法得到的活性顺序存在很大差异,表明活性大小与其体系密切相关。