黑果腺肋花楸花色苷提取工艺优化及其抗氧化活性和组成鉴定

目的：优化超声波辅助提取黑果腺肋花楸花色苷的条件,测定花色苷的抗氧化能力,鉴定黑果腺肋花楸花色苷提取物的组成成分。方法：采用响应面法优化花色苷提取条件,通过1,1-二苯基-2-三硝基苯肼自由基清除能力、2,2’-联氨-双（3-乙基苯并噻唑啉-6-磺酸）二铵盐自由基清除能力及Fe3＋还原能力方法评价其抗氧化能力,高效液相色谱-质谱联用法进行成分分析。结果表明：提取温度60?℃、超声功率100?W、料液比1∶30（g/mL）、超声时间31?min、乙醇体积分数64%和pH?2.0时为最优提取条件,此时黑果腺肋花楸花色苷含量可达（3.61±0.01）mg/g。体外抗氧化实验表明,在相同质量浓度条件下,黑果腺肋花楸花色苷提取物的抗氧化活性明显高于VC。组分鉴定表明黑果腺肋花楸花色苷提取物中共有6?种花色苷,其中矢车菊-己糖苷二聚体和矢车菊-3,5-二己糖苷为新检测出的2?种花色苷。     

Polyphenols, Anthocyanins, Ascorbic Acid, and Radical Scavenging Activity of Rubus, Ribes, and Aronia

ABSTRACT: Total polyphenols, total anthocyanins, and reduced ascorbic acid were evaluated in berries belonging to the genera Rubus, Ribes, and Aronia by means of spectrophotometric and high-performance liquid chromatography (HPLC) techniques. The 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activity of the fruit extracts was tested. Total polyphenols ranged from 140.6 to 888.5 mg/100 g fresh weight (FW), total anthocyanins ranged from 22.0 to 460.5 mg/100 g FW, and reduced ascorbic acid ranged from 12.4 to 153.8 mg/ 100 g FW. The average EC50 values for Aronia melanocarpa, Ribes nigrum, Ribes rubrum, Rubus fruticosus, and Rubus idaeus were 1.8, 2.8, 5.3, 6.4, and 8.2 mg FW, respectively. The results indicate that the fruits tested are good sources of natural antioxidants.     

Radical Scavenging Activity and LC-MS Metabolic Profiling of Petals, Stamens, and Flowers of Crocus sativus L

Radical scavenging activities of Crocus sativus petals, stamens and entire flowers, which are waste products in the production of the spice saffron, by employing ABTS radical scavenging method, were determined. At the same time, the metabolic profiles of different extract (obtained by petals, stamens and flowers) were obtained by LC-ESI-IT MS (liquid chromatography coupled with electrospray mass spectrometry equipped with Ion Trap analyser). LC-ESI-MS is a techniques largely used nowadays for qualitative fingerprint of herbal extracts and particularly for phenolic compounds. To compare the different extracts under an analytical point of view a specific method for qualitative LC-MS analysis was developed. The high variety of glycosylated flavonoids found in the metabolic profiles could give value to C. sativus petals, stamens and entire flowers. Practical Application: Waste products obtained during saffron production, could represent an interesting source of phenolic compounds, with respect to the high variety of compounds and their free radical scavenging activity.     

Peel Effects on Phenolic Composition,Antioxidant Activity,and Making of Pomegranate Juice and Wine

Pomegranate peel was used in juicing to find out its effects on the juice products’ (storable juice and wine) sensory property, polyphenols composition, and antioxidant ability. Macroporous resin was used to purify the polyphenols, and 6 different in vitro assays were used to comprehensively determine the antioxidant activity of each. The results showed that juicing with peel made the juice bitter and astringent, but contributed better sensory quality to wine. Peel contributed higher total polyphenols and flavonoids, but lower anthocyanins to the juice products, and caused the phenolics content to fluctuate more dramatically during making wine than the storable juice. Polyphenols purified from the juice products containing peel showed higher total reducing ability and 2,2‐diphenyl‐1‐picrylhydrazyl and 2,2′‐azino‐bis(3‐ethylbenzothiazoline‐6‐sulfonic acid radical elimination abilities, but their clearance activity of hydroxyl radicals was not positive, and their superoxide anion radical elimination ability showed no significant difference when compared to polyphenols purified from juice products without peel.     

Total Phenolic Compounds, Flavonoids, and Radical Scavenging Activity of 21 Selected Tropical Plants

ABSTRACT:  Free radical scavenging activity of 21 tropical plant extracts was evaluated using 1,1-diphenyl-2-picrylhydrazyl assay (DPPH). Total phenolic compounds and flavonoids were determined using Folin–Ciocalteu and HPLC, respectively. Results of the study revealed that all the plants tested exhibited excellent antioxidant activity with IC₅₀ in the range of 21.3 to 89.6 μg/mL. The most potent activity was demonstrated by  Cosmos caudatus  (21.3 μg/mL) and  Piper betle  (23.0 μg/mL) that are not significantly different than that of     -tocopherol or BHA.  L. inermis  extract was found to consist of the highest concentration of phenolics, catechin, epicatechin, and naringenin. High content of quercetin, myricetin, and kaempferol were identified in  Vitex negundo ,  Centella asiatica , and  Sesbania grandiflora  extracts, respectively. Luteolin and apigenin, on the other hand, were found in  Premna cordifolia  and  Kaempferia galanga  extracts. Strong correlation ( R  = 0.8613) between total phenolic compounds and total flavonoids ( R  = 0.8430) and that of antioxidant activity of the extracts were observed. The study revealed that phenolic, in particular flavonoids, may be the main contributors to the antioxidant activity exhibited by the plants.
Practical Application: Potent antioxidant from natural sources is of great interest to replace the use of synthetic antioxidants. In addition, some of the plants have great potential to be used in the development of functional ingredients/foods that are currently in demand for the health benefits associated with their use.     

Correlation of In Vivo and In Vitro Assay Results for Assessment of Free Radical Scavenging Activity of Green Tea Nutraceuticals

Green tea (GT)‐derived catechins; epigallocatechin gallate (EGCG) in particular are commonly used nutraceuticals for their free‐radical scavenging activity (FRSA). The influence of photodegradation on the protective power of GT nutracenticals against oxidative stress was thoroughly explored. Photodegradation of GT extracts was carried out and monitored using orthogonal stability‐indicating testing protocol; in vitro and in vivo assays. Total polyphenol content (TPC) and FRSA were determined spectrophotometrically while EGCG was selectively monitored using SPE‐HPLC. In vivo assessment of photodegraded samples was investigated via measuring a number of biomarkers for hepatic oxidative stress and apoptosis (caspase‐3, inducible nitric oxide synthase, nitric oxide, mitogen‐activated protein kinase, glutathione, thiobarbituric acid reactive substances, nuclear factor kappa beta, and nuclear factor erythroid 2‐related factor) as well as liver damage (alanine transaminase and aspartate transaminase) in serum of rats previously subjected to oxidative stress. Results showed complete degradation of EGCG in photodegraded green tea samples with no correlation with either TPC or FRSA. On the other hand, in vivo assay results revealed not only loss of activity but formation of harmful pro‐oxidants. Photostability was found crucial for the protective effect of GT extract against lead acetate insult. Results confirmed that careful design of quality control protocols requires correlation of chemical assays to bioassays to verify efficacy, stability, and most importantly safety of nutraceuticals.     

Extraction, Identification, and Quantification of Flavonoids and Phenolic Acids in Electron Beam-Irradiated Almond Skin Powder

ABSTRACT:  The effect of electron beam irradiation doses from 0 to 30 kGy on extraction yield and phenolic compounds was evaluated in almond skin phenolic extracts (ASPE). Total soluble phenols and distribution of phenolic compounds from acidified methanol ASPE and 52% methanol ASPE were quantified using Folin–Ciocalteau method, liquid chromatography with diode array and fluorescence detection, and negative ion electrospray-mass spectrometry. Electron beam irradiation increased extraction yield by as much as 23%, with the greatest increase observed in the acidified methanol ASPE. Irradiated samples extracted with acidified methanol also exhibited an increase in extractable phenols (Folin–Ciocalteau) and total HPLC-resolved phenolics at all irradiation doses. Samples extracted with 52% methanol exhibited an increase at 10 and 20 kGy, but a 31% decrease at 30 kGy. An increase in aglycones respective to their glycosides was not observed with irradiation. Therefore, the increase in phenolics was attributed to release of phenolics from their cellular matrix.     

芒果皮渣多酚的提取分离及抗氧化活性分析

以芒果皮渣为原料,通过单因素实验优选粗多酚的提取方法和工艺参数;采用不同极性有机溶剂萃取粗多酚,筛选多酚含量最高的组分,并通过HPD100型大孔树脂分离纯化;进一步,采用LC-Q-TOF-MS法对纯化组分初步定性并比较了不同溶剂萃取相和纯化组分的体外抗氧化活性。结果表明,超声辅助法对芒果皮渣多酚的提取效果较好,最佳提取条件为:乙醇浓度80%、浸提时间1.5 h、浸提温度60℃、超声功率250 W、液料比30:1 mL/g,在此条件下,多酚得率为9.68%;乙酸乙酯相所得多酚含量最高,达到254.41 mg/g;从树脂纯化组分中共鉴定出17种化合物,主要包括黄酮、黄酮醇、酚酸和鞣质等,具有优异的抗氧化活性,其清除DPPH自由基、ABTS+自由基、羟自由基和超氧阴离子自由基的IC50值分别为0.191×10-3 mg/m L、0.081 mg/mL、0.43 mg/mL和0.63mg/m L。表明乙酸乙酯相中的纯化组分是深入挖掘芒果皮渣抗氧化功效的物质基础。     

Analysis of Phenolic Composition of Noble Muscadine (Vitis rotundifolia) by HPLC‐MS and the Relationship to Its Antioxidant Capacity

Abstract: Phenolic compounds and anthocyanins in muscadines have attracted much attention due to their diverse biological activities. With bioassays of antioxidant activities in terms of total phenolic content (TPC), total anthocyanin content (TAC), total procyanidin content (TPA), oxygen radical absorbance capacity (ORAC), and ferric reducing antioxidant power (FRAP) of different parts of the Noble muscadine, the butanol (BuOH) extract of the muscadine skin showed the highest TPC (317.91 ± 1.83 mg GAE/100 g FW), which might be ascribed to its high TAC of 227.06 ± 1.29 mg/100 g fresh weight (FW). The ethyl acetate (EtOAc) extract of the muscadine seed contained the highest TPA (55.30 ± 0.63 mg CE/100 g FW). Correlation analyses demonstrated a significant linear relationship of TPC and TAC compared to their ORAC and FRAP values within the range of R² from 0.9283 to 0.9936, which suggested that phenolics and anthocyanins in the extracts contributed significantly to their antioxidant potential. Nineteen individual phenolics and 5 anthocyanins were identified by HPLC‐MS, which indicated different chemical profiles of anthocyanins and other phenolics in the muscadine extracts. Practical Application: The paper has provided rich information of bioactive phytochemical profiles in different solvent extracts and their correlation with the antioxidant activity in the muscadine that is a very special regional fruit in U.S. Its high content of phenolic compounds demonstrates that muscadine could be beneficial to human health.     

Separation, identification, and quantitation of phenolic acids in Chinese waxberry (Myrica Rubra) juice by HPLC-PDA-ESI-MS

A high-performance liquid chromatography coupled with photodiode-array spectrophotometry and electrospray ionization-mass spectrometry (HPLC-PDA-ESI-MS) method for separation and determination of phenolic acids in ethyl acetate extracts from Chinese waxberry (Myrica Rubra) juice was developed. Total of 4 phenolic acids (ferulic, caffeic, sinapic, and salicylic acids) were identified by comparing their HPLC retention times, UV-Vis absorption spectra, and simultaneously recorded mass spectra with authentic standards. Quantitation was carried out by the peak area method. The calibration curves are linear over the concentration range studied with the correlation coefficients, R(2), greater than 0.99. The contents of ferulic, caffeic, sinapic, and salicylic acids in waxberry juice samples studied were 2.76, 3.58, 2.89, and 1.92 mg/L, respectively, and they occur mainly in bound forms. All relative standard deviations were less than 4%. The recoveries range from 83.6% to 95.8% for the 4 analytes. To the authors' best knowledge, this is the first report for the identification of the sinapic and salicylic acids in Chinese waxberry products.     

Phenolic Composition,Essential Oil,and Antioxidant Activity in the Aerial Part of Artemisia Herba-Alba from Several Provenances: A Comparative Study

This study characterized the phenolic, aroma compositions, and antioxidant capacities of four Artemisia herba alba accessions collected from north and center regions in Tunisia in order to select valuable origin with optimal bioactive compounds production. The total polyphenol and flavonoid contents varied between accessions with maxima contents observed in center regions. Kaempherol, apigenin, naringenin, p-coumaric, trans-cinnamic, and caffeic acids were the most abundant compounds with percentage varying depending on the considered accession. Significant changes on essential oil yields (0.4–1.2%) were found between accessions and three different oil chemotypes were distinguished: camphor, fenchol/α-thujone, and α-thujone/camphor. Cluster analysis of volatile and phenolic compositions grouped the accessions on different groups. Antioxidant activities of extracts were found to be higher than essential oils for the four provenances. The results suggested that the center regions have high potential for selecting varieties rich on essential oil, antioxidant phenolic acids, and flavonoids.     

羊栖菜多糖提取分离及其清除自由基的活性研究

为研究羊栖菜中多糖的提取分离及其对羟自由基(·OH)的清除活性,以及超声波时间、温度、时间、固液比对羊栖菜多糖提取的影响。采用L16(45)正交试验,得到超声波辅助水浴提取法提取羊栖菜多糖的最佳工艺条件为固液比1:40(m/V)、超声波时间20min、温度100℃、水浴时间150min,在此条件下,羊栖菜多糖提取率为6.60%。采用Fenton 体系研究羊栖菜多糖对·OH 的清除作用,得到其清除能力随其质量浓度的增大而增大,在多糖质量浓度为0.05～0.50mg/ml 范围内线性关系良好,脱蛋白多糖对·OH 清除率的线性相关系数R=0.9959,0.50g/L 脱蛋白多糖对·OH 清除率为42.2%。     

蒙古绣线菊六个化合物及其挥发油化学成分和清除DPPH自由基活性、抗菌活性的测定分析

通过GC/MS对水蒸气蒸馏法提取的蒙古绣线菊枝、叶挥发油化学成分进行分析。挥发油的主要成分为脂肪酸及其衍生物,其中棕榈酸乙酯占挥发油总含量38.631%、反亚油酸乙酯23.576%、亚麻酸乙酯14.634%。通过硅胶柱色谱法分离和核磁鉴定,白桦脂醇(1)、羽扇豆醇-3,20-二醇(2)、1β-羟基-6,9-二烯-8-羰基-11-降-11-二酮(3)、3-(4-甲氧基苯基)丙醛(4)、豆甾醇(5)、β-谷甾醇(6)六个化合物从蒙古绣线菊枝、叶中分离出来。对它们清除DPPH自由基活性、抗菌活性也分别进行了测定。试验结果表明挥发油有良好的清除DPPH自由基活性(IC50=900 μg/mL),对所选菌株没有明显的抗菌活性。化合物(4)显示出较强的清除DPPH自由基活性(IC50=13 μg/mL),对黄曲霉、枯草芽孢杆菌和白色念珠菌均有明显的抑菌活性。化合物(3)清除DPPH自由基活性微弱,对黄曲霉和枯草芽孢杆菌显示明显的抑菌活性,这些研究结果对传统中草药的研究和新药物的研制具有一定的意义。     

Phenolics,Aroma Profile,and In Vitro Antioxidant Activity of Italian Dessert Passito Wine from Saracena (Italy)

A traditional sweet dessert wine from Saracena (Italy), made with nonmacerated local white grapes (Guarnaccia, Malvasia and Moscato), was analyzed for phenolics and aroma profile and antioxidant activities. The most abundant classes of phenols identified by high‐performance liquid chromatography were hydroxybenzoic acids and flavan‐3‐ols, where gallic acid showed the highest content (376.5 mg/L). The analysis by solid phase microextraction‐gas chromatography‐mass spectrometry revealed the presence of superior alcohols (from iso‐butanol and iso‐amyl alcohol up to 2‐phenylethanol) and their ethyl esters, terpenes (such as linalool), furfuryl compounds, and free fatty acids (up to palmitic acid) as the key odorants of this wine. The antioxidant activity, evaluated by different in vitro assays 2,2‐diphenyl‐1‐picrylhydrazyl (DPPH), 2,2′‐azino‐bis(3‐ethylbenzothiazoline‐6‐sulphonic acid (ABTS), and β‐carotene bleaching test), showed that passito wine had a radical scavenging activity (IC₅₀ value of 0.03 v/v against DPPH·) and inhibited linoleic acid oxidation with an IC₅₀ value of 0.4 v/v after 30 min of incubation.     

不同热风干燥方式对香菇多酚组成及其抗氧化活性的影响

研究了六种不同热风干燥方式对香菇多酚含量、组成及抗氧化活性的影响。采用福林-酚法和HPLC法对香菇多酚定量定性分析,并用化学法评价其抗氧化活性。结果显示:恒温干燥(ID)游离酚含量最高(2.69 mg GAE/g DW),结合酚含量最低(0.19mg GAE/g DW);均匀间歇干燥(UID)游离酚含量最低,结合酚含量相对较高。游离酚主要成分为没食子酸、绿原酸、咖啡酸、槲皮素,结合酚主要成分为没食子酸、槲皮素。六种干燥方式多酚均具有一定的抗氧化能力,其中ID组游离酚和结合酚的DPPH·清除能力最强,IC50值分别为0.53μg/m L、0.06μg/m L;ID组游离酚的ABTS+·清除能力最强,IC50值为3.32μg/m L,各干燥组间结合酚ABTS+·清除能力无显著差异;不同干燥组间的还原力无显著差异。结论:不同处理香菇多酚的含量、组成、抗氧化性有所差异,恒温干燥(ID)是香菇干燥比较理想的方式。     

Drying Sage (Salvia officinalis L.) Plants and Its Effects on Content, Chemical Composition, and Radical Scavenging Activity of the Essential Oil

Chemical composition and antioxidant activity of Salvia officinalis essential oil (EO) were studied under different drying methods of plant material. Results obtained showed that dried plant material yielded more essential oils than did the fresh one. The highest EO yields were obtained by infrared drying at 45?°C (0.39%) followed by air drying (0.30%) and oven drying at 45?°C (0.26%). The analysis of EOs by gas chromatography?Cmass spectrometry, showed in each of 55 identified compounds belonging mostly to oxygenated monoterpenes. This class of compounds was significantly affected by following drying methods: oven at 65?°C, microwave (500?W), and infrared at 45?°C. The main components of sage EO, 1,8-cineole, ?? and ??-thujone, camphor, viridiflorol, and manool showed significant variation (p?<?0.05) with drying methods. Their concentrations increased significantly, particularly when drying sage at ambient air. Finally, the screening of antioxidant activity of the different sage EOs using the di(phenyl)-(2,4,6-trinitrophenyl)iminoazanium radical (DPPH) assay showed an appreciable reduction of the stable radical DPPH, although microwave drying was the most efficient method with an IC50 of 1.60% as compared with fresh plant (IC50?=?5.32).     

Comparison between Supercritical CO2 Extraction and Hydrodistillation for Two Species of Eucalyptus: Yield,Chemical Composition,and Antioxidant Activity

In this work, 2 Eucalyptus species extracts (Eucalyptus cinerea and Eucalyptus camaldulensis) were prepared by hydrodistillation (HD) and supercritical carbon dioxide extraction (SCE) techniques. The best yields of E. cinerea and E. camaldulensis (27.5 and 8.8 g/kg, respectively) were obtained using SCE at 90 bar, 40 °C compared to HD (23 and 6.2 g/kg, respectively). Extracts were quantified by gas chromatography‐flame ionization detection and identified by gas chromatography‐mass spectrometry. 1,8‐cineole and p‐menth‐1‐en‐8‐ol were the major compounds of E. cinerea essential oil obtained by HD (64.89% and 8.15%, respectively) or by SCE (16.1% and 31.87%, respectively). Whereas, in case of E. camaldulensis, 1,8‐cineole (45.71%) and p‐cymene (17.14%) were the major compounds obtained by HD, and 8,14‐cedranoxide (43.79%) and elemol (6.3%) by SCE. Their antioxidant activity was assessed using 2 methods: 2,2‐azino‐di‐3‐ethylbenzothialozine‐sulphonic acid radical cation (ABTS^?+) and 2,2‐diphenyl‐1‐picrylhydrazyl radical (DPPH^?). In the SCE extracts from both E. cinerea and E. camaldulensis, a promising radical scavenging activity was observed with ABTS^?+, (65 and 128 mg/L, respectively). The total phenolics composition of the extracts was measured and the range was 2 to 60 mg of gallic acid equivalent/g dry plant material. The SCE method was superior to HD, regarding shorter extraction times (30 min for SCE compared with 4 h for HD), a low environmental impact, allows production of nondegraded compounds and being part of green chemistry.