火焰原子吸收法测定大米钙的含量

文章探讨了火焰原子吸收法测定大米中钙含量的方法。大米样品经湿法消化处理后,稀释数倍,加氧化镧溶液后测定。同时配制标准溶液,加入相同的氧化镧溶液。本法标准溶液的线性范围为0.5mg/L～5.0mg/L,相关系数为1.0。对牡丹江地区15份大米进行了检测,试验结果：钙含量平均值为82.99mg/L,重现性均在±8%以内,回收率为79.23%～87.16%。试验结论：本法结果可靠,方法简单,便于推广。     

流动分析法测定卷烟纸中的钙、镁含量

考察了消化液体积和温度对卷烟纸中钙和镁含量检测结果的影响,并采用该方法和离子色谱法检测了20个卷烟纸样品.结果表明:①卷烟纸样品消化的适宜条件:卷烟纸样品0.2 ～0.3 g;消化液5 mL硝酸-高氯酸混合液;消化温度300℃;消化时间1h;②钙、镁的RSD分别为0.93%,2.95%,回收率为96.7% ～ 102.9%和98.6%～106.7%;③国产卷烟纸样品钙、镁含量的均值各为117.4和1.09 mg/g,进口卷烟纸样品钙、镁含量均值116.0和1.17 mg/g;④2种方法的钙、镁含量检测值在0.05水平下无显著性差异.该法适合于卷烟纸中钙和镁含量的分析.     

微波消解-释放剂辅助火焰原子吸收分光光度法测定蛋白质粉中的钙

建立采用微波消解-释放剂辅助火焰原子吸收分光光度法(flame atomic absorption spectrophotometry,FAAS)测定蛋白质粉中钙的方法。探讨消解体系、消解压力、消解时间以及增压方式对消解结果的影响,选择硝酸镧为释放剂,研究待测样品中硝酸镧的质量浓度对钙元素释放的影响。结果表明,在最佳的实验条件下,钙的线性范围为1～20μg/mL,检出限为0.15μg/mL,测定蛋白质粉中钙的质量分数为0.46%,精密度为1.63%,加标平均回收率为96.8%,相对标准偏差为2.34%。该方法线性范围宽、相关性好,准确度和精密度高,具有较高的实用价值。     

火焰原子吸收光谱法测定牛奶中不同化学形态的钙

建立火焰原子吸收光谱法测定牛奶中不同化学形态钙的方法。研究乙醇体积分数、离心温度、离心力和离心时间对蛋白沉淀效果的影响,确定最佳分离条件,即乙醇体积分数50%、离心温度2℃、离心力6000×g、离心时间6min,建立沉淀剂分离牛奶中元素结合态和非结合态的方法。探讨释放剂硝酸镧的质量浓度对吸光度的影响,确定最佳质量浓度为6.00mg/mL。在此条件下,测定牛奶中总钙的质量浓度为808.6μg/mL,其中结合态钙的质量浓度为641.8μg/mL,占总钙的质量分数为79.4%;非结合态钙的质量浓度为173.0μg/mL,占总钙的质量分数为21.4%。本法的精密度(RSD)小于3.3%,仪器检出限为0.11μg/mL,加标平均回收率为97.0%,RSD为1.7%。该方法准确、稳定,具有较高的实用价值。     

自动凯氏定氮仪测定食品中蛋白质消化条件的改进

目的优化自动凯氏定氮仪测定食品中蛋白质含量的消化条件。方法选择3种不同类别的食品分别进行测量,研究样品量、催化剂配比(K_2SO_4用量/CuSO_4用量,以克计,以下同)、浓硫酸用量、消化时间和消化温度对蛋白质测定的影响。结果实验得出最佳消化条件为:大米样品量0.8 g,催化剂配比6/0.4,浓硫酸用量12.00 mL, 420℃消化80 min;香肠样品量0.8 g,催化剂配比6/0.2,浓硫酸用量10.00 mL, 420℃消化90 min;纯牛奶样品量1.00 mL,催化剂配比6/0.2,浓硫酸用量10.00 mL, 420℃消化70 min。平行测定结果的相对标准偏差分别为0.21%、0.29%、0.50%,加标回收率均在99%以上。结论采用优化消化条件后的自动凯氏定氮仪测定食品中蛋白质含量精密度高,稳定性好,测定结果准确可靠,满足日常检测要求。     

火焰原子吸收光谱法测定茶叶中的微量元素

建立了湿法消化-火焰原子吸收光谱法测定不同品种茶叶中2种微量元素的分析方法。茶叶样品经湿法消化,用原子吸收光谱法测定微量元素铜和铁的含量。方法检出限分别为Cu:0.04μg/mL、Fe:0.15μg/mL;线性范围分别为Cu:0.2～1.5μg/mL、Fe:0.3～5.0μg/mL,相关系数r>0.9980;相对标准偏差(RSD)分别为Cu:2.16%、Fe:0.32%;回收率分别为Cu:98.00%～102.40%,Fe:98.50%～101.35%。并用该方法检测了20种长春市售茶叶中铜和铁的含量。     

模拟胃肠消化提高蛹虫草蛋白的体外抗氧化活性

探究模拟胃肠消化对蛹虫草蛋白质理化性质及抗氧化活性的影响。分别采用SDS-PAGE和酸水解法分析模拟胃肠消化前后的蛋白质分子量分布及氨基酸组成。通过体外化学评价方法,测定模拟胃肠消化前后蛹虫草蛋白质及其消化产物的抗氧化活性。构建H2O2诱导氧化损伤的PC12细胞模型,使用CCK-8试剂盒测定经蛹虫草蛋白质消化产物处理后细胞模型中的细胞活力。结果表明,经模拟胃肠消化后,蛋白质分子量的主要分布范围由10~120 ku变为8~15 ku;模拟胃肠消化前后DPPH自由基清除力的IC50值分别为1.55 mg/mL和1.06 mg/mL,Fe2+螯合力的IC50值分别为1.32 mg/mL和0.18 mg/mL,0.3 mg/mL样品的ORAC值分别为467.27±46.53μmol TE/g和948.80±24.02μmol TE/g;100μg/mL消化产物预保护H2O2损伤的PC12细胞后,细胞活力显著提高(p<0.05)。蛹虫草蛋白质模拟胃肠消化前后均具有较强的抗脂质过氧化能力及较低的Fe3+还原能力。蛹虫草蛋白质经模拟胃肠消化后产生了更多小分子量多肽,抗氧化活性显著提高,因此可对消化产物中的抗氧化肽进行进一步的研究和开发。     

环氧氯丙烷交联淀粉的制备及其体外消化性能的研究

以环氧氯丙烷为交联剂,制备土豆交联淀粉。用正交实验考察环氧氯丙烷用量、氢氧化钠用量、反应温度和反应时间四个因素对交联度的影响,确定最佳工艺条件,并对体外消化条件进行优化,对不同交联度淀粉的消化速度进行研究。体外淀粉消化条件的优化实验显示,消化产物测定的最佳条件为：波长485nm,显色温度100℃,显色时间30min,葡萄糖浓度范围0～80μg/mL,其回归方程为y=0.0044x-0.005,R2=0.9988,且样品溶液在2h内显色稳定。各因素对交联淀粉制备影响的重要性依次为环氧氯丙烷用量、氢氧化钠用量、温度及反应时间;最佳工艺条件为：以50g土豆淀粉计,环氧氯丙烷用量为1.00mL,氢氧化钠用量为0.75g,温度50℃,时间6h,土豆交联淀粉和交联前相比,消化性降低了13.7%～34.5%,且与交联度呈负相关。     

微波消解——石墨炉原子吸收法在酱油铅测定中的应用

采用微波消解样品、石墨炉横向加热技术,建立了石墨炉原子吸收光谱法快速测定酱油中Pb含量的方法.优化了微波消解用量及消解条件和石墨炉工作条件,确定了基体改进剂和用量用法.测定Pb的进样量5μL,Pb浓度在10×10-9～80×10-9g/mL范围,浓度与吸光度呈良好的线性关系(r=0.9975),加标回收率为95.94%～103.07%,最低检出限为3×10-9g/mL,定量限为8×10-9g/mL,相对标准偏差为1.71%～2.73%.     

草鱼鱼鳞胶原蛋白酸酶分步提取工艺研究

为实现鱼鳞胶原蛋白的高效提取,在优化脱钙、混酸法和酶法提取工艺基础上,对鱼鳞胶原蛋白的酸酶进行分步提取。研究发现,鱼鳞最佳脱钙工艺为料液比8:100(g/mL),盐酸浓度1.0 mol/L,反应时间1.0 h,反应温度20℃;混合酸法提取鱼鳞胶原蛋白的最佳条件为醋酸料液比1:12(g/mL),柠檬酸料液比1:10(g/mL),乳酸料液比1:12(g/mL),即混合酸料液比为1:34(g/mL),其中,0.8 mol/L柠檬酸、1 mol/L乳酸、0.8 mol/L醋酸的体积比为6:5:6,提取时间2 d,胶原蛋白的提取率为48.14%;最佳酶法提取条件为胃蛋白酶用量450 U/g,提取温度30℃,提取时间72 h,该条件下提取率为45.26%。酸酶耦合法优于单一方法或同种方法两次提取的效果,可实现酸溶性和酶溶性胶原蛋白的连续提取,先酸后酶法胶原蛋白的提取率达84.61%,SDS-PAGE凝胶电泳发现其为Ⅰ型胶原蛋。     

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.     

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.