HPLC测定牛黄丸中黄芩苷的含量

目的建立HPLC法测定牛黄丸中黄芩苷的含量。方法采用Kromasasil C18柱（150mm×4．6mm），以甲醇-水-磷酸（47：53：0．2）为流动相，紫外检测波长为280nm。结果黄芩苷在0．17-1．12μg范围内呈良好的线性关系（r=0．9999），黄芩苷平均回收率为98．3％（n=6），RSD分别为1．37％。结论此方法准确、可靠、重现性好，可适用于牛黄丸中黄芩苷含量的测定。     

反相HPLC法测定小儿退热口服液中栀子苷的含量

目的研究用HPLC法测定小儿退热口服液中栀子苷的含量。方法采用XTerra C18柱,以乙腈-水(12:88)为流动相,检测波长238 nm,流速1.0 mL.min-1。结果栀子苷在63.12～631.2 ng范围内线性关系良好,r=0.999 9,平均加样回收率为98.7%。结论该方法操作简便可靠,结果准确、灵敏度高,重现性好,可作为控制该产品质量的方法。     

桅子黄多酚含量与抗氧化活性的相关性研究

目的：揭示栀子黄抗氧化能力是否与多酚含量有关,为栀子黄中抗氧化能力成分的确定提供线索。方法：分别采用还原能力实验、DPPH自由基清除能力实验和亚铁离子螯合实验测定西红花苷、绿原酸、栀子粗提物和栀子黄的抗氧化活性,同时分别采用HPLC和UV来测定栀子粗提物和栀子黄中西红花苷和多酚的含量。结果：在还原能力和DPPH自由基清除活性模型中,栀子黄色素中起抗氧化作用的主要化学成分是多酚类,而不是西红花苷。另一方面．与前两个模型不同,西红花苷和多酚类成分都具有明显的亚铁离子螯合活性,栀子黄中具有螯合活性的主要化学成分同时包括西红花苷和多酚类。结论：结合前期研究结果推测,栀子黄抗氧化作用的主要化学成分是多酚类．而西红花苷具有明显的亚铁离子螯合活性。     

紫外分光光度法测定栀子中西红花苷的含量

目的:利用紫外分光光度法测定栀子中西红花苷的含量。方法:西红花苷线性关系分析及该方法的精密度、重现性、稳定性和回收率考察。结果:栀子中西红花苷的平均含量为0.928%,RSD(%)0.816。结论:该方法具有较好的线性关系,精密度、重现性、稳定性和回收率都符合要求(RSD3%);此法可以作为栀子特征成分检验的依据,为其质量评价提供前期探索。     

RP—HPLC法测定黄芩苷和黄芩素的含量

目的用反向高效液相（RP—HPLC）法测定滇黄芩和黄芩中黄芩苷和黄芩素的含量。方法乙腈（含1．0％甲酸）-1．0％甲酸溶液为流动相，梯度洗脱，流速为1．0mL／min，检测波长274nm，柱温30℃。结果在精密度，重现性，稳定性实验中，保留时间和峰面积的RSD均小于2％；加标回收率分别为100．7％和100．5％，RSD为1．78％和1．85％；黄芩苷在0．102-2．04μg之间，黄芩素在0．72-14．40μg之间呈良好的线性关系，r=0．9999。结论此实验方法简便、准确、重复性好。     

不同成熟度和产地初加工方法对栀子中4种活性成分含量的影响

研究栀子不同产地初加工方法对样品中栀子酸、绿原酸、栀子苷、西红花苷Ⅰ 4种活性成分含量的影响；采用Agilent ZORBAX SB-C₁₈（5 μm，4.6 mm×250 mm）色谱柱，以乙腈?0.1%磷酸水溶液为流动相，梯度洗脱，流速1.0 mL/min，柱温30 ℃，检测波长:栀子酸和栀子苷238 nm，绿原酸328 nm，西红花苷Ⅰ 440 nm。采用400倍40%甲醇超声提取40 min能将4种成分有效提取出来。结果表明栀子以中成熟和成熟时采收最佳，干燥前有必要进行杀青处理，120 s蒸法杀青和30 s煮法杀青效果相当且最佳；不同干燥方法样中，50℃热风干燥效果最佳；杀青后切制干燥样中活性成分含量高于不切制干燥样；室温避光储存一年半后的不同处理样品中栀子酸、绿原酸、西红花苷Ⅰ的含量均无显著变化（P>0.05），栀子苷含量均显著降低（P<0.05）。此方法以栀子酸、绿原酸、栀子苷和西红花苷Ⅰ 4种活性成分含量为指标评价栀子质量，为栀子的采收、加工、储存提供了理论依据。     

HPLC法检测黑豆乙醇提取物中活性成分的含量

采用高效液相色谱技术（HPLC），建立快速、有效、能同时分析检测黑豆乙醇提取物中大豆苷、苷元、木苷、木素含量的检测方法。结果：在一定条件下流动相及其比例对各组分的分离测定有较大的影响，我们所确定的色谱条件为：固定相：C18柱，流动相：甲醇：水：乙酸为42：57：1，检测波长为260nm；标准对照品的浓度与吸收峰面积均有较好的线性关系，r〉0．99，各组分间分离度大于1．5；测得的黑豆乙醇提取物中大豆苷、染料木苷、大豆苷元、染料木素的平均含量（％）分别为：0．341、0．386、0．0929、0．0265。RSD（％）分别为3．49、5．12、10．0、4．94。HPLC法可同时检测黑豆提取物异黄酮中大豆苷、染料木苷、大豆苷元、染料木素的含量，而且方法简单、快速、精密度高、重现性好。     

利用双水相萃取栀子黄废液中的栀子苷酶法生产栀子蓝色素的研究

研究有机溶剂/ 磷酸氢二钾双水相体系对栀子黄废液中栀子苷的萃取条件,并将萃取后的栀子苷用于栀子蓝色素的生产。根据分相后上下相中栀子苷的分配系数及两相体积比,选择合适的双水相体系,并改变溶剂与废液的体积比、磷酸氢二钾加入量、废液pH 值以及萃取温度等参数,研究萃取栀子苷的最佳条件。实验结果表明,乙醇/ 磷酸氢二钾为合适的萃取体系。当双水相体系总量为10ml 时,乙醇与栀子黄废液的体积比为6:4,加入磷酸氢二钾1.0g,体系分相完全后栀子苷分配系数(K)为4.56,两相体积比(R)为6.38,栀子黄废液pH 值及萃取温度在正常条件下对K 值及R 值影响不大。放大实验表明,以乙醇/ 磷酸氢二钾体系萃取栀子黄废液中的栀子苷,所得栀子苷纯度可达62.12%,收率可达96.32%。萃取后的栀子苷经β- 葡萄糖苷酶水解精氨酸显色后得到栀子蓝色素,色价E1% (590nm)65.92。     

栀子药材不同干燥方法水分动态过程模拟及其对多元活性成分的影响

为了探讨热风干燥、红外干燥、真空干燥与干燥温度对栀子干燥过程水分脱除及成品品质的影响,本文采用Weibull分布函数对其干燥动力学曲线进行拟合,并测定其干燥成品中栀子苷、西红花苷Ⅰ、西红花苷Ⅱ、京尼平-1-β-龙胆二糖苷的含量。结果表明:Weibull分布函数能较好地模拟栀子药材干燥过程(R~2=0.9936～0.9998),红外干燥过程属于降速干燥(β1),真空干燥与热风干燥过程脱水速率呈现先升高后降低的趋势(β1),尺度参数α随干燥温度升高而降低,不同干燥方式对尺度参数α也有较大影响,但随温度升高差异缩小。热风干燥、红外干燥、真空干燥干燥活化能分别为40.74、54.73、87.46 kJ/mol。在相同干燥方法下,随着干燥温度升高,西红花苷Ⅰ、西红花苷Ⅱ、京尼平-1-β-龙胆二糖苷呈升高趋势,栀子苷无明显升高或下降趋势;基于活性成分综合评价结果显示,50℃红外干燥方法得到的样品品质较佳,综合考虑干燥时间与干燥能耗,70℃红外干燥方法可作为栀子药材的适宜干燥方法。     

RP-HPLC测定小儿清热片中栀子苷和龙胆苦苷的含量

目的建立小儿清热片中栀子苷和龙胆苦苷的含量测定方法。方法采用反相高效液相色谱法(RPHPLC),Diamonsil C18柱,甲醇-0.1%磷酸水溶液(21:79)为流动相,流速1.0 m L/min,检测波长254 nm,柱温为室温。结果栀子苷在6.32~126.4μg/m L范围内线性关系良好(r=0.9998),平均回收率为100.9%,方法精密度(RSD)为0.76%(n=6);龙胆苦苷在2.04~40.8μg/m L范围内线性关系良好(r=0.9997),平均回收率为100.1%,RSD为0.84%(n=6)。结论该法可用于小儿清热片中栀子苷和龙胆苦苷的含量测定。     

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.     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

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.