HPLC-DAD-Q-TOF-MS在线筛选鉴定牛蒡中的抗氧化成分

建立高效液相色谱-飞行时间质谱联用在线筛选并鉴定牛蒡提取物中抗氧化活性成分的方法。样品经在线色谱柱分离后进行分流,一路与稳定的1,1-二苯基-2-三硝基苯肼-甲醇溶液混合,实现在线筛选自由基清除剂;另一路进入二极管阵列检测器-串联三重四极杆飞行时间质谱,用于化合物的快速鉴别。负离子模式下,通过高分辨率质谱获得的相对分子质量结合化合物的紫外吸收特征,参考相关文献和部分对照品验证,从牛蒡乙酸乙酯相中筛选并鉴定出咖啡酸及衍生物19 种。本方法可实现快速定向筛选和鉴定食品及中药等复杂体系中的抗氧化活性成分。     

白簕叶不同极性部位的体外抗氧化活性分析

利用不同溶剂对白簕叶各极性部位进行提取、显色鉴定和薄层色谱分析,并考察其中乙酸乙酯、正丁醇和水3个不同极性部位提取液的体外抗氧化活性,通过测定其铁还原力、对DPPH·的清除率、总抗氧化力,筛选出主要的抗氧化活性部位。结果表明,白簕叶3个不同极性部位的成分的种类和含量差别均较大,体外抗氧化结果显示各部分体外抗氧化活性也存在较大差异,其中正丁醇部位抗氧化活性最高。     

快速分析彝药桃树寄生抗氧化成分

目的：快速分离、鉴定彝药桃树寄生的抗氧化成分。方法：通过1,1- 二苯基-2- 三硝基苯肼(DPPH) 自由基清除实验,评价彝药桃树寄生的甲醇提取物及其二氯甲烷、正丁醇及水萃取物的抗氧化作用,利用生物活性-高效液相跟踪方法,快速分离、鉴定其有效成分。结果：从彝药桃树寄生的二氯甲烷萃取物中分离、鉴定出有效成分为松脂酚(pinoresinol)。结论：利用生物活性- 高效液相跟踪方法可以快速分离、鉴定彝药桃树寄生中的抗氧化成分,可应用于其他天然植物活性成分的快速筛选。     

野地瓜茎正丁醇萃取物中主要抗氧化活性成分的筛选

探清野地瓜茎不同极性萃取物的抗氧化活性,筛选并鉴定抗氧化活性较高萃取物的主要化学成分。通过系统溶剂法对野地瓜茎提取物进行萃取,获得石油醚、二氯甲烷、乙酸乙酯、正丁醇相提取物及剩余上层被萃取水相提取物;采用1,1-二苯基-2-三硝基苯肼(DPPH)自由基清除能力、2,2’-联氮基-双-(3-乙基苯并噻唑-6-磺酸)二铵盐(ABTS)自由基清除能力和总还原力(TRPA)试验综合评价其不同极性萃取物的抗氧化活性;结合在线高效液相色谱—质谱—二苯基三硝基苯肼(HPLC-DAD-ESI/MSn-DPPH)快速筛选并鉴定活性较高萃取物中的抗氧化活性成分。结果表明:正丁醇萃取物具有较强的抗氧化活性(P0.05),随着质量浓度的增大呈明显的剂量依赖效应,正丁醇萃取物对DPPH自由基、ABTS自由基清除能力的半数抑制浓度(IC_(50))分别为(23.28±0.21),(76.30±1.13)μg/mL。经液相色谱、质谱、文献报道和对照品的综合分析,从野地瓜茎正丁醇萃取物中筛选的3种抗氧化活性化合物为5-O-咖啡酰奎宁酸、3-O-咖啡酰奎宁酸和4-O-咖啡酰奎宁酸。     

发酵肉制品中高抗氧化肉品发酵剂的筛选鉴定

为获得高抗氧化活性的天然肉品发酵剂,通过清除自由基、还原能力和抗脂质过氧化实验对来源于5种发酵肉制品中30株乳酸菌的发酵上清液、菌体细胞和胞内提取物的抗氧化活性进行研究,并按照肉品发酵剂的筛选标准对高抗氧化性的菌株进行筛选,鉴定出符合要求的菌株。结果表明:这30株乳酸菌具有不同的抗氧化能力且不同组分的抗氧化活性之间存在很大差异,发现菌株L23、L26和L28具有较高的抗氧化活性,其中L23符合肉品发酵剂的筛选标准,可作为天然高抗氧化性肉品发酵剂用于生产。经鉴定L23为希腊魏斯氏菌。     

贵州顶坛花椒抗氧化活性成分研究

目的:研究顶坛花椒的抗氧化活性成分。方法:采用1,1-二苯基-2-三硝基苯肼(DPPH)自由基清除法筛选测定顶坛花椒果皮的甲醇提取物及其不同极性溶剂萃取部位抗氧化活性,筛选出抗氧化活性部位,然后采用柱层析法及高效液相色谱法分离活性部位,通过13C-NMR、1H-NMR和质谱法,结合文献数据鉴定化合物结构。结果:顶坛花椒的甲醇提取物具有显著DPPH自由基清除能力,其乙酸乙酯萃取部位为活性部位,从中分离得到的5个主要成分分别被鉴定为:2’-羟基-β-山椒素(1),异鼠李素-3-O-β-半乳糖苷(2),槲皮素-3-O-β-半乳糖苷(3),槲皮素-3-O-β-葡萄糖苷(4),槲皮素-3-O-β-(4’’-O-硬脂酰基)葡萄糖苷(5),其中(5)为首次从花椒属植物分离得到。结论:顶坛花椒果皮具有显著的抗氧化作用,主要活性成分为其中的酰胺类和黄酮类组分。     

UPLC-PDA-MS-ABTS阳离子自由基在线分析藤茶的抗氧化活性成分

采用超高效液相色谱-二极管阵列检测器-质谱-2,2’-联氮双(3-乙基苯并噻唑啉-6-磺酸)二铵盐阳离子自由基在线法对藤茶中的抗氧化活性成分进行定性鉴别;以Trolox为对照品,采用标准曲线法,对藤茶中的主要成分二氢杨梅素的抗氧化活性进行定量分析。结果表明,从藤茶中共鉴定出4个化合物,其中主要抗氧化活性成分为二氢杨梅素;对市售12批藤茶样本进行抗氧化活性分析,其中产于湖北恩施和福建武夷山的样本抗氧化活性最高。所建定量分析方法快捷、稳定、可靠,可用于藤茶样本的在线抗氧化分析。     

高抗氧化活性双歧杆菌的筛选及鉴定

目的:筛选高抗氧化活性双歧杆菌优良菌株,为双歧杆菌抗氧化剂的开发与应用提供参考。方法:以新疆吐鲁番地区长寿老人源的16株双歧杆菌为出发菌株,以超氧阴离子清除率、DPPH清除率、羟自由基清除率、抗脂质过氧化率和还原能力为考察指标,比较不同菌株及部位的抗氧化能力,筛选优良菌株。采用形态学观察、API 20A生化鉴定系统和16S r DNA序列分析对菌株进行分类学鉴定。结果 :菌株不同部位抗氧化能力差异较大,无细胞提取物清除超氧阴离子、DPPH能力和抗脂质过氧化反应能力最强,菌体细胞清除羟自由基的活性最高,发酵上清液的还原能力强于其他部位。综合比较不同待测菌株的各项抗氧化指标,发现菌株BF-10的抗氧化能力较强且全面,为筛选到的高抗氧化优良菌株。分类学鉴定结果表明该菌株为动物双歧杆菌。结论:获得高抗氧化活性动物双歧杆菌BF-10。     

蜂巢提取液的成分鉴定及抗氧化功效测定

对蜂巢乙醇提取液和水提取液进行了成分鉴定和抗氧化活性的研究。通过对这两种提取液进行GC-MS气质分析,各鉴定出其中17种成分,对两种提取液的总还原力、DPPH·清除率、ABTS+·清除率、超氧阴离子清除率、羟自由基清除率以及油脂抗氧化进行测定,结果表明蜂巢水提液和蜂巢乙醇提取液与化学合成抗氧剂BHT相比均具有较强的抗氧化活性,随着各自浓度的增加,抗氧化活性随之增强,当浓度增加到一定值,清除率趋于稳定,而且蜂巢水提取液的抗氧化效果比乙醇提取液的好,表明蜂巢提取液是一种优良的天然抗氧化剂和自由基清除剂。     

桑黄营养成分、活性成分及多糖性质分析

为探寻不同桑黄子实体中营养、活性成分及抗氧化活性差异，本研究比较分析了5种桑黄的营养、活性成分含量及其多糖的抗氧化活性，以此为评价指标筛选优质桑黄子实体，采用rDNA ITS序列分析对目标桑黄进行鉴定，并对其多糖的抗氧化活性进行测定，通过紫外光谱、傅里叶变换红外光谱和高效液相色谱分析多糖性质。结果表明，供试桑黄在营养、活性成分含量及多糖抗氧化活性方面均存在较大差异；其中，桑黄S-4中粗纤维、粗蛋白、多糖、总酚、总黄酮、总三萜含量相对较高，粗脂肪和灰分含量相对较低，且S-4多糖对DPPH自由基、ABTS⁺自由基和O₂^-自由基的清除能力均较好，半抑制浓度(IC₅₀)分别为35.07、12.87、91.34μg/mL，对ABTS⁺自由基的清除能力与抗坏血酸相当；将S-4作为目标桑黄，经鉴定，为杨树桑黄；紫外、红外光谱和单糖组成分析表明S-4多糖具有典型的多糖类特征吸收峰，是含有β-糖苷键和呋喃环的多糖，主要由葡萄糖、半乳糖、岩藻糖、葡萄糖醛酸、核糖和甘露糖组成。S-4的营养、活性成分...     

Reliable identification of grapevine rootstock varieties using RAPD PCR on woody samples

Since grapevine ( Vitis spp .) rootstock material is being traded increasingly as disbudded woody material a lack of distinctive morphological features on such material necessitates an alternative and reliable means of identification. Methods described here were developed for rapid and efficient extraction of DNA from woody samples rich in phenolic compounds and polysaccharides, and for subsequent identification of varieties by RAPD PCR. Using these methods, and with the application of only one selected RAPD primer, we were able to differentiate sixteen rootstock varieties, including the seven varieties most commonly used in Germany. Problems commonly encountered with reproducibility of RAPD patterns were avoided by choosing primers with a dinucleotide sequence and a high G/C content that allowed a rather high annealing temperature of 45°C. Methods described here should also be useful for other horticultural crops, especially those with woody tissues rich in phenolic compounds and polysaccharides.     

Chlorohydrins of bisphenol A diglycidyl ether (BADGE) and of bisphenol F diglycidyl ether (BFDGE) in canned foods and ready-to-drink coffees from the Japanese market

BADGE.2HCl and BFDGE.2HCl were determined in 28 samples of ready-to-drink canned coffee and 18 samples of canned vegetables (10 corn, 5 tomatoes and 3 others), all from the Japanese market. HPLC was used as the principal analytical method and GCMS for confirmation of relevant LC fractions. BADGE.2HCl was found to be present in one canned coffee and five samples of corn, BFDGE.2HCl in four samples of canned tomatoes and in one canned corn. No sample was found which exceeded the 1mg/kg limit of the EU for the BADGE chlorohydrins. However the highest concentration was found for the sum of BFDGE.2HCl and BFDGE.HCl.H₂O at a level of 1.5mg/kg. A Beilstein test confirmed that all cans containing foods contaminated with BADGE.2HCl or BFDGE.2HCl had at lest one part coated with a PVC organosol.     

European priorities for research to support legislation in the area of food contact materials and articles

A strong science base is required to underpin the planning and decision-making process involved in determining future European community legislation on materials and articles in contact with food. Significant progress has been made in the past 5 years in European funded work in this area, with many developments contributing to a much better understanding of the migration process, and better and simpler approaches to food control. In this paper this progress is reviewed against previously identified work-areas (identified in 1994) and conclusions are reached about future requirements for R&D to support legislation on food contact materials and articles over the next 5 or so years.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

Tests of potential functional barriers for laminated multilayer food packages. Part I: Low molecular weight permeants

The advent of the functional barrier concept in food packaging has brought with it a requirement for fast tests of permeation through potential barrier materials. In such tests it would be convenient for both foodstuffs and materials below the functional barrier (sub-barrier materials) to be represented by standard simulants. By means of inverse gas chromatography, liquid paraffin spiked with appropriate permeants was considered as a potential simulant of sub-barrier materials based on polypropylene (PP) or similar polyolefins. Experiments were performed to characterize the kinetics of the permeation of low molecular weight model permeants (octene, toluene and isopropanol) from liquid paraffin, through a surrogate potential functional barrier (25 μm-thick oriented PP) into the food simulants olive oil and 3% (w/v) acetic acid. These permeation results were interpreted in terms of three permeation kinetic models regarding the solubility of a particular model permeant in the post-barrier medium (i.e. the food simulant). The results obtained justify the development and evaluation of liquid sub-barrier simulants that would allow flexible yet rigorous testing of new laminated multilayer packaging materials.     

Textural Properties of Cold-set Gels Induced from Heat-denatured Whey Protein Isolates

A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.     

Influence des ions sur le pouvoir hydratant de l'ure e: e tude sur peau de porc ex vivo

This study deals with the influence of ions (NaCl and MgSO4) in a W/O emulsion containing 10% urea. Moisturization kinetics are assessed by corneometry on pig skin ex vivo. The formula's influence on urea penetration is measured by infrared spectrometry with an ATR device and the stripping method. Corneometry and spectroscopy were chosen to record simultaneously the hydratation levels and urea localization into superficial cell layers. Urea crystallization after evaporation of emulsions and aqueous solutions is described. Results show that urea does not hydrate nor penetrate when applied to the skin through an aqueous gel. In a W/O emulsion, sodium chloride increases the ability of urea to moisturize without improving penetration. In vitro urea crystallization is disturbed by sodium chloride or magnesium sulphate for solutions and emulsions. This stabilization by ions is correlated with good moisturization values. The stabilization of urea in the solute state provided by ions increases its water epidermal binding capacity without enhancing penetration.     

Occurrence of bisphenol-F-diglycidyl ether (BFDGE) in fish canned in oil

The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.     

Analysis on Economic Indicators from 62 Enterprises in Printing Machinery Industry in Q1 2014

Operation of printing machine industry was still unsatisfactory in the first quarter of 2014.Analysis on operation of printing machine industry.a.Market demand was not strong;sales of product undulated and declined.According to the statistics,the total industrial output value fell by 19.28% in the first quarter of 2014 than the average quarter value in 2013; industrial added value decreased by 4.16%; sales revenue dropped by 22.83%. h. Business operation of enterprises was in poor condition. c. R＆D of new products is an important transformation guarantee for enterprises. d. To take self explore new ways upgrading advantages,and explore new ways.