高效液相色谱法快速测定食用植物油中苯并（a）芘的研究

本文研究了食用植物油中苯并(a)芘的高效液相色谱检测法。用乙腈作为样品中苯并(a)芘的提取液,采用高效液相色谱-荧光检测器测定,外标峰面积法定量。结果表明,苯并(a)芘在0.5-20 ng/mL范围内呈良好的线性关系,相关系数为0.999 7。在空白样品中添加0.2μg/kg、5.0μg/kg、10.0μg/kg三个水平苯并(a)芘的回收率为95.8-101.3%,相对标准偏差(RSD)为1.72-10.13%,检出限为0.2μg/kg。本方法适用于食用植物油中苯并(a)芘的检测。     

全自动固相萃取净化-高效液相色谱法测定食用植物油中苯并(a)芘含量

为提高工作效率,降低误差,建立分子印迹柱全自动固相萃取净化-高效液相色谱法测定食用植物油中苯并(a)芘含量的方法。样品经正己烷提取,采用全自动固相萃取仪进行分子印迹柱净化,C18色谱柱分离,高效液相色谱-荧光检测器检测。结果表明：苯并(a)芘在0.5～20.0 ng/mL质量浓度范围内与峰面积线性关系良好,相关系数为0.999 9,方法检出限为0.09μg/kg,定量限为0.30μg/kg,加标回收率为91.7%～111.8%,相对标准偏差为2.0%～8.2%,与国标方法的检测结果不存在显著性差异;对市售38份食用植物油样品进行检测发现,苯并(a)芘的检出率为76.3%。该方法准确度高、重复性好,可批量自动化前处理样品,提高工作效率,并降低人员操作误差风险,适用于食用植物油中苯并(a)芘含量的测定。     

固相萃取-高效液相法测定芝麻油中苯并(a)芘

建立一种快速、高效测定芝麻油中苯并(a)芘的固相萃取-高效液相色谱(SPE-HPLC)方法。样品前处理采用硅胶固相萃取柱串联氧化铝固相萃取小柱,稀释液和淋洗液选择正己烷,洗脱液选择二氯甲烷,在40℃下氮吹干后,乙腈复溶后检测。采用Waters RP C18色谱柱(4.6 mm×250 mm,5μm)分离,以乙腈-水(90∶10)作为流动相,用荧光检测器检测,外标法峰面积定量。结果表明,苯并(a)芘在1.00 ng/m L~20.00 ng/m L浓度范围内线性良好,相关系数r2为0.999 8,检出限为0.05μg/kg,定量限为0.16μg/kg,加标回收率达到92.2%~98.5%。     

固相萃取-高效液相色谱法测定天然维生素E中苯并(a)芘

建立了固相萃取-高效液相色谱测定天然维生素E中苯并(a)芘的方法。天然维生素E样品经Cleanert Silica串联Cleanert Bap固相萃取柱前处理净化后采用C18色谱柱分离,以乙腈-水(体积比80∶20)为流动相,荧光检测器检测。结果表明:苯并(a)芘的质量浓度在0.5~10μg/L范围内与色谱峰面积呈良好的线性关系,相关系数为0.999 8,方法检出限为0.3μg/kg;样品加标回收率在88%~96%之间,相对标准偏差在2.8%~3.6%之间。该方法简单便捷,灵敏度高,选择性好,适用于天然维生素E中苯并(a)芘的测定。     

基于HiCapt Benzo固相萃取前处理的HPLC-FLD法检测油茶籽油中苯并(a)芘

为了建立一种基于Hi Capt Benzo固相萃取快速前处理的,更灵敏、准确的高效液相色谱-荧光检测法,以用于油茶籽油中苯并(a)芘的检测。油茶籽油样品以正己烷溶解后,用Hi Capt Benzo专用固相萃取柱净化。检测条件为:LC-PAHs专用色谱柱;50%乙腈-50%水为流动相,流速1.0 m L/min;荧光检测器;外标法定量。研究结果表明,苯并(a)芘标准曲线在0.1~200 ng/m L范围内,线性关系好(R~2=0.9993);检测限很低(0.0213~0.0246μg/kg)。该法用于4个油茶籽油样品加标检测,回收率为93.06%~104.52%,相对标准偏差(RSD)为2.12%~3.98%。本文所建固相萃取-高效液相色谱(带荧光检测器)法前处理简单,结果准确可靠,是油茶籽油苯并(a)芘高效检测的适宜方法。     

固相萃取-高效液相色谱法测定食用油脂中的苯并[a]芘

采用Ploy-sery MIP-BAP固相萃取小柱富集苯并[a]芘,应用高效液相色谱梯度洗脱法,以C_(18)为色谱柱,乙腈为流动相,采用荧光法测定六种植物油中苯并[a]芘的含量。结果表明,苯并[a]芘在1.0~30 ng/m L色谱峰面积呈现良好的线性关系。用此法测定植物油中苯并[a]芘的加标含量,回收率为90.1~95.2%。     

液相色谱法测定奶油中苯并(a)芘的研究

目的建立液相色谱法检测奶油中苯并(a)芘的快速检测方法。方法试样中的苯并(a)芘经正己烷溶解提取,通过苯并(a)芘专用SPE小柱分离纯化,液相色谱-配荧光检测器检测,通过保留时间定性、外标法定量。结果该方法检测苯并芘回收率范围在88.4%~98.7%之间,相对标准偏差在1.23%~3.22%之间,最低检出限为0.3μg/kg。结论该方法简单、快速、分离度好,适用于批量样品的测定。     

固相萃取-高效液相色谱荧光法测定食用油中苯并(a)芘

建立固相萃取-高效液相色谱法测定食用油中苯并(a)芘的检测方法。样品经苯并(a)芘专用SPE小柱净化、浓缩,沃特世反相C18(150 mm×4.6 mm,5μm)色谱柱进行分离,流动相为乙腈:水(95:5,体积比),流量1.0 mL/min,激发波长384 nm,发射波长406 nm。结果表明,苯并(a)芘在浓度范围0.2~50μg/kg内线性良好,相关系数为0.999 9,最低检出限为0.1μg/kg,精密度RSD3%,回收率88.6%~101%。本方法快速便捷、准确率高、重现性好、可同时处理大量样品,为食用油中苯并(a)芘的测定提供参考。     

反相高效液相色谱法测定植物油中苯并(a)芘含量

将适量的试样溶解于石油醚中,用中性氧化铝柱净化,用石油醚洗脱苯并(a)芘,荧光检测器检测。结果显示,苯并(a)芘色谱峰面积与质量浓度在0～50μg/L的范围内呈良好的线性关系(r=0.999 5);方法的最低检测限为0.2μg/kg。苯并(a)芘的回收率为88.3%～98.5%。证明该方法准确、灵敏、快捷,建立了一种反相高效液相色谱法测定植物油中苯并(a)芘含量的方法。     

固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘

采用中性氧化铝小柱净化样品,建立固相萃取-超高效液相色谱荧光法测定植物油中苯并(a)芘的方法。样品以正己烷为提取剂,净化、蒸发浓缩后正己烷溶解,荧光检测器检测。流动相为乙腈-水(75:25,V/V),流速0.5mL/min,外标法定量。苯并(a)芘在0.10～50.0μg/L质量浓度范围内线性关系良好,相关系数R2为0.9998;在空白样品中添加3个水平的标准品,回收率在91.7%～97.5%之间,相对标准偏差均小于2%(n＝3);最低检出限为0.01μg/kg,定量限为0.03μg/kg。方法操作简便、分析时间短、稳定性好、选择性好、灵敏度高,为植物油中苯并(a)芘的测定提供参考。     

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