高效液相法同时测定土茯苓中五种多酚成分

本文建立了土茯苓中五种多酚成分：5-O-咖啡酰莽草酸、落新妇苷、花旗松素、黄杞苷及白藜芦醇的高效液相色谱分析方法。色谱柱为Agilem Zorbax SB Cl8柱（250mm×4．6mmi．d．,5μm）,流动相为乙腈（A）及O．1％醋酸水溶液（B）,线性梯度洗脱程序为0～15mm,16～21％A;15～40min,21～40％A。五种成分线性良好（r〉998）,保留时间相对标准偏差介于0122～0．76%峰面积相对标准偏差介于2．67～4．64%,加标回收率介于96．5～103．7％。对18批土茯苓样品分析结果表明,落新妇苷是土茯苓中最主要黄酮成分,含量范围为5．48～5．75mg/g;花旗松素、黄杞苷、异黄杞苷、落新妇苷及其三种异构体（以落新妇苷计）等七种黄酮总量介于6．72～35．3mg/g,平均含量为18士8．5mg/g;5-O-咖啡酰莽草酸含量也较高,含量范围为0．9～6．29mg/g,该成分在土茯苓中的含量测定为首次报道。但花旗松素和白藜芦醇含量较低,在一些样品中未检测到。     

高效液相色谱法测定益之康胶囊中总蒽醌(大黄素和大黄素甲醚)的含量

建立益之康胶囊中总蒽醌含量测定的高效液相色谱法。采用HPLC测定益之康胶囊中2种蒽醌类成分大黄素和大黄素甲醚的含量;流动相为甲醇-0.1%磷酸溶液(75∶25,v/v),柱温30℃,流速1.0 m L/min,检测波长254 nm。大黄素和大黄素甲醚分别在0.054~0.65μg和0.022~0.27μg范围内呈良好的线性关系,相关系数分别为0.9999和0.9999,检出限分别为0.86μg/g和0.87μg/g,平均回收率分别为97.20%(RSD=2.26%)和99.96%(RSD=2.18%)。结论:该方法简便、准确、可靠。     

树莓与蓝莓中多酚类成分的HPLC测定

利用HPLC法对树莓与蓝莓中的生理活性成分进行含量测定。HPLC法采用Kromasil C18色谱柱(150 mm,4.6 mm);流动相采用色谱纯乙腈(A)-含0.1%磷酸水溶液(B)梯度洗脱,0~16 min,5%A;19 min,10%A;23 min,13%A;40 min,14%A;43 min,17%A;48 min,22%A;51 min,24%A;52 min,24%A;58 min,26%A;60 min,30%A;65 min,60%A;68 min,70%A;72 min~78 min,100%A;流速为1 mL/min;柱温30℃;检测波长为280 nm;每次进样10μL,测定树莓与蓝莓95%乙醇提取物中没食子酸、原儿茶酸、儿茶素、表儿茶素、原花青素B2、矢车菊素、鞣花酸、树莓酮、白藜芦醇、水杨酸的含量;这十种多酚类成分在三种浆果中含量高低不等,其中鞣花酸含量在黑树莓中最高(0.97μg/g),红树莓次之(0.51μg/g),蓝莓最低(0.36μg/g)。蓝莓与树莓中富含多种多酚类物质,是其具有多种生物活性的物质基础。     

HPLC法同时测定枣叶中5种黄酮的含量

建立了一种枣叶中黄酮类成分定量分析的HPLC方法,并对14个品种的大枣及酸枣叶中这5种黄酮的含量进行了分析。结果得到采用Hypersil BDS C18色谱柱,以乙腈与0.1%甲酸水溶液为流动相梯度洗脱,流速1 m L/min,柱温30℃,检测波长360 nm,实现了槲皮素-3-O-洋槐糖苷、芦丁、槲皮素-3-O-β-D-葡萄糖苷、山奈酚-3-O-芸香糖苷、槲皮素-3-O-α-L-阿拉伯糖-(1→2)-α-L-鼠李糖苷5种黄酮苷的同时检测,最低检出限为1.44~2.59μg/m L,加标回收率在93.8%~105.9%之间。5种黄酮苷的含量测定结果表明不同品种的枣叶中黄酮类成分的组成和含量差异较大,其中芦丁和槲皮素-3-O-洋槐糖苷的含量较高,平均为7.83 mg/g D.W和4.61 mg/g D.W;8个品种枣叶中检测到槲皮素-3-O-α-L-阿拉伯糖-(1→2)-α-L-鼠李糖苷,平均5.32 mg/g D.W;而槲皮素-3-O-β-D-葡萄糖苷和山奈酚-3-O-芸香糖苷的含量较低,分别为0.14 mg/g D.W和0.41 mg/g D.W。     

油菜蜂花粉黄酮醇的测定及其抗氧化活性研究

本实验通过盐酸酸解蜂花粉乙醇提取物,薄层色谱法分离酸解液中黄酮醇,并测定酸解液中黄酮醇的含量及其抗氧化活性。结果表明：蜂花粉乙醇提取物酸解后,槲皮素(Rf 值0.59)含量为0.40mg/g,山奈酚(Rf 值0.71)含量为3.98mg/g,酸解液DPPH·清除率强于花粉乙醇提取物。经制备液相分离,采用核磁和质谱鉴定出一种酮醇苷,其结构为山奈酚3-O-(2＂-O- β-D- 吡喃葡萄糖)- β-D- 葡萄糖。采用TLC-DPPH 技术对蜂花粉乙醇提取物及其酸解液中抗氧化成分进行追踪,为花粉中黄酮醇苷的抗氧性研究提供参考。     

HPLC同时测定大黄利胆胶囊中5种蒽醌类成分的总含量

目的建立高效液相色谱法(HPLC)同时测定大黄利胆胶囊中5种蒽醌类成分总含量的方法。方法采用phenomenon luna C_(18)色谱柱,流动相为甲醇-0.1%磷酸(82:18),检测波长254 nm,流速1.0 mL/min,柱温为30℃。结果芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的线性范围分别为1.057~67.67mg/L(r=0.9999),1.117~71.49 mg/L(r=0.9999),1.047~67.02 mg/L(r=0.9999),1.089~69.71 mg/L(r=0.9999),0.5968~38.20 mg/L(r=0.9996);平均加样回收率(n=6)分别为98.0%(RSD=1.69%),99.2%(RSD=2.19%),99.4%(RSD=1.89%),98.9%(RSD=0.76%),97.8%(RSD=1.26%)。结论该方法简便,可行、重现性好,可作为大黄利胆胶囊的质量控制方法。     

HPLC-DAD同时测定野菊不同部位8种活性成分的含量

目的建立同时测定中药野菊不同部位(花、叶、嫩茎、老茎)中绿原酸、咖啡酸、1,3-二咖啡酰奎宁酸、3,5-二咖啡酰奎宁酸、木犀草素-7-O-β-D-葡糖苷、芹菜素-7-O-β-D-葡糖苷、蒙花苷和木犀草素含量的高效液相色谱-二极管阵列检测(HPLC-DAD)方法。方法采用Thermo Hypersil C18(250 mm×4.6 mm,5μm)色谱柱,乙腈-0.1%磷酸为流动相,梯度洗脱,流速1.0 ml/min,柱温35℃,检测波长327 nm。结果绿原酸、咖啡酸、1,3-二咖啡酰奎宁酸、3,5-二咖啡酰奎宁酸、木犀草素-7-O-β-D-葡糖苷、芹菜素-7-O-β-D-葡糖苷、蒙花苷和木犀草素进样量分别在0.031~0.620μg、0.009~0.180μg、0.016~0.320μg、0.081~1.620μg、0.021~0.420μg、0.011~0.220μg、0.152~3.040μg、0.017~0.340μg范围内与峰面积呈良好的线性关系,相关系数分别为0.9999,0.9998,0.9997,0.9996,0.9995,0.9996,0.9997,0.9998。绿原酸、咖啡酸、1,3-二咖啡酰奎宁酸、3,5-二咖啡酰奎宁酸、木犀草素-7-O-β-D-葡糖苷、芹菜素-7-O-β-D-葡糖苷、蒙花苷和木犀草素的平均加样回收率分别为98.29%,99.09%,99.03%,98.88%,99.22%,99.02%,98.38%,99.02%,RSD(n=6)分别为1.40%,1.05%,0.98%,1.18%,0.98%,0.91%,0.89%,1.26%。结论本法操作简便,准确性和重复性好,可用于中药野菊的质量控制,测定结果显示野菊不同部位有机酸和黄酮类活性成分含量差异较大。     

虎杖果实中白藜芦醇与大黄素提取工艺优化及其与3类根茎含量比较

目的：研究虎杖果实中白藜芦醇与大黄素提取工艺,比较其果实与雄株、未结果雌株、结果雌株3 类根茎中白藜芦醇与大黄素得率。方法：采用高效液相色谱法测定其果实与3 类根茎中白藜芦醇与大黄素含量,确定果实中白藜芦醇与大黄素提取的溶剂与方法,采用正交试验法考察微波火力档、溶剂体积分数、料液比及提取时间对提取工艺的影响,确定微波辅助提取的最佳提取工艺,比较虎杖果实、3 类根茎中二者得率。结果：正交试验与方差分析得出果实中白藜芦醇与大黄素的最佳提取条件为乙醇体积分数70%、料液比1∶20（g/mL）、额定功率800 W微波炉先40火力处理3 min冷却后60火力处理3 min、提取时间6 min,高效液相色谱法测得虎杖雄株、未结果雌株根茎中的白藜芦醇与大黄素得率均高于结果雌株根茎及果实,果实及3 类根茎中白藜芦醇与大黄素得率均超过《中国药典》（2010）规定值,提取工艺合理、稳定、可行,虎杖果实具备开发利用的价值。     

HPLC同时测定木香顺气丸中5种成分的含量

目的建立同时测定木香顺气丸中5种活性成分含量的方法。方法采用高效液相色谱法(HPLC),色谱柱为Kromasil C18柱(250 mm×4.6 mm,5μm),以乙腈为流动相A,0.2%磷酸溶液为流动相B,梯度洗脱:0~5 min,10%A;5~20 min,10%→20%A;20~40 min,20%→60%A;40~60 min,60%A;分段设定检测波长:0~20.0 min为210 nm(木香烃内酯、去氢木香内酯);20.0~30.0 min为292 nm(和厚朴酚);30.0~45.0 min为211 nm(厚朴酚);45.0~60.0 min为250 nm(甘草酸),流速1.0 m L/min,柱温30℃,进样量20μL。结果香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚和甘草酸分离度良好,进样量分别在0.025~1.008,0.031~1.232,0.022~0.864,0.058~2.304,0.045~1.800μg范围内线性关系良好,r均大于0.9990,平均加样回收率为99.2%~99.7%(RSD=0.74%~1.05%)。5批样品中香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚和甘草酸含量分别在6.17~6.51,2.74~2.89,13.2~13.66,2.54~2.87,4.40~4.65 mg/g。结论本方法专属性好、灵敏度高、准确度高,为木香顺气丸的质量控制提供依据。     

虎杖米酒的理化分析及评价

在大米中添加不同含量的虎杖粉末,发酵过程中,使虎杖中的有效成分溶解在米酒中。理化检测结果表明,虎杖的加入对米酒的糖度、酒精度等理化性质没有影响,但颜色随着虎杖量的增加黄色逐渐加深。高效液相色谱检测结果表明,米酒中含有来自于虎杖的虎杖苷和白藜芦醇成分,且其含量随虎杖粉末的添加量增加而增加。如在含2%虎杖粉末的米酒中虎杖苷和白藜芦醇的含量分别为37.82、1.75μg/m L,10%时虎杖苷和白藜芦醇的量分别为214.26、23.93μg/m L。品评结果表明,添加2%的虎杖米酒最佳。     

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.     

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.     

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 of benzo[a]pyrene in spiked fatty foods by second derivative synchronous spectrofluorimetry after microwave-assisted treatment of samples

A simple, rapid and inexpensive method has been developed for the determination of benzo[a     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. II: Certification study

This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.     

Contribution of European research to risk analysis

The European Commission's, Quality of Life Research Programme, Key Action 1—Health, Food & Nutrition is mission-oriented and aims, amongst other things, at providing a healthy, safe and high-quality food supply leading to reinforced consumer confidence in the safety of European food. Its objectives also include the enhancing of the competitiveness of the European food supply. Key Action 1 is currently supporting a number of different types of European collaborative projects in the area of risk analysis. The objectives of these projects range from the development and validation of prevention strategies including the reduction of consumers risks; development and validation of new modelling approaches; harmonization of risk assessment principles, methodologies, and terminology; standardization of methods and systems used for the safety evaluation of transgenic food; providing of tools for the evaluation of human viral contamination of shellfish and quality control; new methodologies for assessing the potential of unintended effects of genetically modified (genetically modified) foods; development of a risk assessment model for Cryptosporidium parvum related to the food and water industries; to the development of a communication platform for genetically modified organism, producers, retailers, regulatory authorities and consumer groups to improve safety assessment procedures, risk management strategies and risk communication; development and validation of new methods for safety testing of transgenic food; evaluation of the safety and efficacy of iron supplementation in pregnant women; evaluation of the potential cancer-preventing activity of pro- and pre-biotic ('synbiotic') combinations in human volunteers. An overview of these projects is presented here.     

Announcing a new international peer-reviewed journal:Food Science and Human Wellness now accepting manuscript submission in English

<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of the