改进固相萃取-高效液相色谱法同时测定食品中7种合成着色剂

目的 建立固相萃取-高效液相色谱法同时测定食品中7种合成着色剂(柠檬黄、日落黄、苋菜红、胭脂红、新红、赤藓红和亮蓝)的含量。方法 使用Welchrom? PA聚酰胺固相萃取小柱和Welchrom? P-WAX弱阴离子交换固相萃取小柱对多种食品基质进行净化、浓缩, 并采用Ultimate? XB-C18(250 mm×4.6 mm, 5 μm)色谱柱以甲醇-0.02 mol/L乙酸铵为流动相进行梯度洗脱, 于254 nm波长下测定。结果 Welchrom? PA聚酰胺小柱和Welchrom? P-WAX弱阴离子交换固相萃取小柱分别对固体和液体样品中杂质的去除效果好、回收率高。7种合成着色剂在浓度为0.5~50 μg/mL的范围内线性关系良好(r2>0.9995), 回收率为84.7%~105.8%, 检出限为0.2~0.5 mg/kg。结论 该方法简便、灵敏度高、准确性好, 适用于食品中7种合成着色剂的定量分析。     

固相萃取-高效液相色谱-二极管阵列检测法测定饮料中9种人工合成着色剂

本文介绍了使用固相萃取-高效液相色谱-二极管阵列检测技术来简便快捷地检测饮料中柠檬黄、新红、苋菜红、靛蓝、胭脂红、日落黄、诱惑红、亮蓝、赤藓红这9种人工合成着色剂含量的方法。样品经PWAX固相萃取柱净化,采用串联两根Thermo BDS C₁₈色谱柱(4.6×150mm,5μm),以甲醇和0.02mol/L乙酸铵溶液为流动相进行梯度洗脱,DAD检测波长为254nm,以保留时间和待测物的紫外吸收光谱进行定性分析、外标法进行定量分析。结果显示,9种人工合成着色剂的线性范围为0.5~50mg/L(r~2>0.999),检出限为0.11~0.39mg/kg,平均回收率为81.5%~102.2%,相对标准偏差为0.23%~2.24%。结论为,该方法可实现对饮料中9种合成着色剂的同时检测,具有快捷、准确、灵敏的特点。     

固相萃取-超高效液相色谱法同时测定肉制品中5种合成着色剂

目的建立同时测定肉制品中柠檬黄、苋菜红、胭脂红、日落黄和诱惑红等5种合成着色剂含量的固相萃取-超高效液相色谱(SPE-UPLC)方法。方法样品以乙醇-氨水(75:25,v/v)为提取液,振荡超声提取肉制品样品中的着色剂,调节pH后经OASIS WAX固相萃取小柱净化和富集,在ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7μm)上以甲醇-乙酸铵水溶液(0.02 mol/L)为流动相进行梯度洗脱色谱分离,流速0.3 m L/min,柱温30℃,进样量3μL,检测波长200~500 nm。结果 5种合成着色剂在0.5~25.0 mg/L范围内线性关系良好(r20.9999),检出限为0.05~0.20 mg/kg,最低定量限为0.15~0.60 mg/kg,RSD为1.2%~3.3%,在加标水平为检出限3倍和6倍时,5种合成着色剂在肉制品样品中的加标回收率分别为89.7%~96.0%和91.3%~97.5%。结论本法准确度高,具有良好的重现性和精密度,可用于肉制品中柠檬黄、苋菜红、胭脂红、日落黄和诱惑红等5种合成着色剂的测定。     

液相色谱–串联质谱法测定谷类食品中5种合成着色剂

通过添加食用小苏打的甲醇水溶液提取谷类食品中的合成着色剂,采用超高效液相色谱–串联质谱技术测定加标回收率,考察食用小苏打在谷类食品中对日落黄、苋菜红、胭脂红、诱惑红和亮蓝五种合成着色剂的萃取效果。试验样品经70 mL的40%甲醇水加1.00 g食用小苏打涡混提取后,通过固相萃取柱Strata X-AW SPE净化,结果显示,在0.1~1.4 μg/mL范围内呈良好线性关系,五种合成着色剂的检出限范围为0.07~0.50 μg/g。不同食品基质和不同加标水平条件（1、2、10 μg/g）下,5种合成着色剂的加标回收率范围均在80%~110%间,相对标准偏差（RSD）范围为0.7%~5.1%(n=6),满足GB/T27404—2008《实验室质量控制规范 食品理化检测》对回收率的规定要求。     

固相萃取-高效液相色谱法测定饮料中的9种合成着色剂

本文介绍了一种运用固相萃取-高效液相色谱技术同时快速检测饮料中柠檬黄、日落黄、新红、苋菜红、胭脂红、酸性红、诱惑红、亮蓝、靛蓝等9种合成着色剂含量的方法。样品经固相萃取柱提取后,采用Purospher~? STARLP RP-18 endcapped色谱柱(4.6 mm×250 mm×5μm)分离,用20 mmol/L乙酸铵水溶液和乙腈体系作为流动相进行梯度洗脱,采用二极管阵列检测器,在200-700 nm波长下进行扫描,254 nm波长下进行检测。在此实验条件下,9种合成着色剂可在25 min内有效分离,平均回收率为77.3-98.4%,相对标准偏差为0.14%-3.81%,检出限为4.12-4.92 mg/kg。建立的方法可实现对饮料中9种合成着色剂的同时检测,具有快速、准确、灵敏的特点。     

高效液相色谱法测定烟用接装纸中水溶性着色剂

本研究建立了同时测定烟用接装纸中诱惑红、苋菜红、酸性红、胭脂红、赤藓红、喹啉黄、靛蓝、亮蓝、柠檬黄、日落黄10种着色剂的高效液相色谱-二极管阵列（HPLC-PDA）方法。样品以甲醇/乙腈/水为溶剂,微波辅助提取10种烟用接装纸中的水溶性合成着色剂。通过单因素与正交实验结合的方法研究了提取溶剂、微波功率、提取时间对提取效率的影响。结果表明,溶剂为甲醇/乙腈/水=1∶1∶3（体积比）,微波功率300 W、提取时间3 min、固液比为1∶100时,着色剂提取效果最佳。目标化合物在15 min内分离度良好,能达到基线分离,在0.5~20.0 μg/mL浓度范围内具有良好的线性关系,相关系数均大于0.999,回收率为92.6%~100.3%,相对标准偏差（n=5）为0.5%~6.7%;方法检出限为0.95~3.21 μg/g,定量限为3.16~10.72 μg/g。该方法能同时快速分析烟用材料中10种水溶性合成着色剂的含量,为卷烟安全评价提供技术支撑。     

固相萃取-高效液相色谱法测定肉制品中合成着色剂的含量

建立测定肉制品中合成着色剂苋菜红、胭脂红和诱惑红含量的固相萃取-高效液相色谱法。方法 以氨水-90%乙醇(1+99,V/V)溶液为提取液,超声提取肉制品样品中的着色剂,经PLS固相萃取柱净化,色谱柱为Dikma Spursil C18(4.6mm×150mm,5μm)。以乙腈-0.05mol/L乙酸铵溶液为流动相进行梯度洗脱色谱分离,流速1.0ml/min,柱温30℃,进样量10μl,检测波长200～700nm。结果 在0.5～25.0μg/ml,苋菜红、胭脂红和诱惑红的峰面积与其相应浓度呈良好相关性,相关系数r分别为0.9996、0.9997和0.9993,方法加标回收率为94.2%～99.1%。结论 本方法准确度高,具有良好的重现性和精密度,能快速对肉制品中3种合成着色剂进行定量检测,满足国家限量标准的要求。     

一种测定果汁饮料中7种合成色素的HPLC方法

建立了同时测定果汁饮料中7种合成着色剂(柠檬黄、新红、苋菜红、胭脂红、日落黄、亮蓝、赤藓红)的固相萃取柱净化高效液相色谱方法。试样经无水乙醇-氨水溶液-水(体积比7∶2∶1)提取,Cleanert PWAX固相萃取SPE柱富集和净化后,采用Nvcleodur C18柱(250mm×4.6mm,5μm),以0.02mol/L乙酸铵-甲醇为流动相进行梯度洗脱,采用二极管阵列检测器,多波长检测定量。结果表明:7种合成着色剂在0.5～40.0μg/mL均有良好的线性关系,相关系数(r)为0.9999;方法检出限为0.025～0.097mg/kg;3个不同水平(2.0、5.0、10.0mg/kg)的加标平均回收率为96.51%～104.41%,RSD值为0.95%～2.01%。该方法具有操作简便、灵敏度高、重现性佳等特色,适用于果汁饮料中7种合成着色剂的同时检测。     

高效液相色谱法测定饮料中12种水溶性合成着色剂

目的建立高效液相色谱法同时测定饮料中柠檬黄、喹啉黄、苋菜红、胭脂红、日落黄、诱惑红、酸性红、赤藓红、靛蓝、酸性绿S、亮蓝、专利蓝V 12种水溶性合成着色剂的方法。方法饮料样品经离心、过滤后直接进样,以甲醇-乙酸铵(0.02 mol/L)为流动相进行梯度洗脱,采用二极管阵列检测器多波长分析,外标法定量。结果 12种合成着色剂在0.5～100mg/L范围内线性关系良好,相关系数均大于0.999;检出限为0.05～0.3 mg/kg;平均回收率为91.0%～101.3%,相对标准偏差值为0.2%～2.3%。结论该方法简便、快速、准确,前处理简单,适合于基质成分较为简单的液体样品中多种着色剂的同时测定。     

固相萃取-高效液相色谱法快速测定食品中7种合成着色剂

采用固相萃取-高效液相色谱法测定食品中7种合成着色剂(柠檬黄、苋菜红、日落黄、胭脂红、诱惑红、亮蓝、赤藓红)。样品经无水乙醇∶氨水∶水(7∶2∶1)提取后,固相萃取柱净化,浓缩后采用Diamonsil C18色谱柱分离,外标法定量。结果表明,在1.0~50.0 mg/L范围内,各合成着色剂的浓度与峰面积呈良好的线性关系,线性相关系数(r)在0.999 97~0.999 99,各目标化合物回收率84.3%~100.1%,相对标准偏差(RSD)0.86%~3.56%。该方法简单、快捷、满足检测要求,可用于快速测定各类食品中7种合成着色剂的含量。     

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.     

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.     

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.     

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