食品及食品包装材料溶剂残留检测方法研究概况

食品残留溶剂来源于生产加工过程或由食品包装材料带入,对人体健康存在潜在危害,食品中溶剂残留量的测定对于保证食品安全具有重要意义。本文论述了我国食品及食品包装材料溶剂残留的限量规定、检测的现行标准和技术规范。现行国家标准对食品和食品包装材料中残留溶剂的限量规定比较笼统,建议细化具体检测的残留溶剂种类并设定合理的限值。对食品及食品包装材料残留溶剂检测方法的相关文献进行了梳理总结。气相色谱法是分析残留溶剂的常用检测方法,具有专属性强、重现性好、灵敏度高等优点。本文对目前食品及食品包装材料残留溶剂检测存在问题和今后发展方向提出建议,为建立同时检测食品及食品包装材料多种残留溶剂的检测方法提供理论依据和文献参考。     

QuEChERS结合气相色谱-质谱法同时检测食品包装材料中20种光引发剂

目的 建立同时检测食品包装材料中20种光引发剂含量的检测方法。方法 采用QuEChERS技术结合气相色谱质谱联用法(GC-MS)建立食品包装材料中20种光引发剂同时测定方法。食品包装样品经乙酸乙酯超声辅助提取后,使用无水硫酸镁、N-丙基乙二胺(N-propyl ethylenediamine,PSA)、C18进行净化,再通过GC-MS在选择离子监测(SIM)模式下检测,外标法定量。结果 20种光引发剂在0.05~2.0 mg/L浓度范围内线性关系良好,相关系数均大于0.999;在0.2、0.4、2.0 mg/m2 3个浓度水平的加标回收率在70.6%～112.8%之间;相对标准偏差为1.2%～5.8% (n=6),检出限为0.01～0.05 mg/m2。结论 该方法简单、灵敏、准确,适用于食品包装材料中20种光引发剂残留量的快速分析检测。     

微波辅助萃取-气相色谱/串联质谱法同时测定皮革及其制品中21种有害有机溶剂的残留量

建立了1个气相色谱/串联质谱方法,对皮革及其制品中21种有害有机溶剂的残留量进行了同时测定,该方法以甲醇为萃取溶剂,微波萃取皮革及其制品中残留的有害有机溶剂,萃取液经硅胶固相萃取柱净化后,直接进行气相色谱/串联质谱分析,外标法定量。结果表明,21种有害有机溶剂的定量下限为15~100μg/kg。在3个加标浓度水平下,方法的加标平均回收率为80.3~94.6%,相对标准偏差为2.5~7.3%。该方法简单快速,灵敏度高,定性准确,定量下限低,定量下限远低于欧盟REACH法规的限量要求,可完全满足皮革及其制品中有害有机溶剂残留量检测工作的需要。应用该方法对市售皮革及其制品中残留的有害有机溶剂含量进行筛查,结果在部分样品中检出了不同含量水平的多种目标分析物。     

微波萃取-GC/MS-MS测定乙二醇醚类有机溶剂

建立了气相色谱/串联质谱方法,测定纺织品中残留的15种乙二醇醚类有机溶剂。该方法以乙醇为萃取溶剂,100℃下微波萃取纺织品中残留的乙二醇醚类有机溶剂,萃取液直接进行气相色谱/串联质谱分析,外标法定量。在信噪比(S/N)为10的条件下,各组分的定量下限为5~20 mg/kg。在三个加标水平下,平均回收率为81.7%~94.5%,相对标准偏差为2.1%~6.8%。该方法简单快速,可满足纺织品中乙二醇醚类有机溶剂残留量检测的技术要求。     

聚乙烯醇纳米复合膜中残留戊二醛含量的测定

戊二醛作为聚乙烯醇基纳米复合包装材料的交联剂能提高纳米复合材料的综合包装性能,但戊二醛的残留会影响食品包装材料的安全性。对聚乙烯醇纳米复合膜样品采用超声萃取其中残留的戊二醛,并与2,4-二硝基苯肼(DNPH)衍生化后,用高效液相色谱法(HPLC)检测其残留出的戊二醛含量,结果显示:该方法在0.2～5.0mg/L范围内线性相关系数为r2=0.9997,平均回收率达到76.8%～87.3%,相对标准偏差为2.83%～4.08%,最低检测浓度为0.2mg/kg,说明采用的萃取条件及色谱分析方法适合聚乙烯醇基纳米复合膜中戊二醛残留量的测定;待测聚乙烯醇基纳米复合膜中残留戊二醛的含量24.55mg/kg,符合食品包装材料安全限量标准。     

塑料食品包装材料中溶剂残留的探讨

塑料食品包装材料的安全性对食品安全有着重要影响。简要介绍国内外关于塑料食品包装材料中溶剂残留的相关标准以及检测的方法,分析影响溶剂残留的主要因素,并提出溶剂残留的控制对策。     

毒死蜱等7种农药残留在玉米酿酒加工过程中的 迁移与降解规律

目的开发了多残留检测方法并研究了以玉米为原料发酵加工白酒酿造过程中的几种农药残留变化及残留浓度。方法用改进的QuEChERS方法进行样品前处理,采用气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)对毒死蜱等7种农药残留水平及残留浓度进行检测。结果玉米和白酒中7种农药的添加回收率在81%~95%之间,方法检出限均在1~10μg/kg之间,定量限均在3~30μg/kg之间。随着发酵时间的延长,毒死蜱等7种农药的残留水平1~14 d内降低缓慢;蒸馏后的轻组分酒液样品中有痕量农药残留检出。结论发酵并不引起测试的农药残留显著降解,但酿酒过程农药迁移率很低,白酒中农药残留风险不高。     

食品包装材料中柠檬酸酯类增塑剂GC/MS/SIM分析

为研究食品包装材料中柠檬酸酯类增塑剂的含量,采用超声辅助二氯甲烷萃取,GC/MS/SIM的检测方式,建立食品包装材料中柠檬酸酯类增塑剂含量的检测方法。结果表明,柠檬酸酯类增塑剂含量在0.001~0.1 mg/mL范围内呈良好线性,线性相关系数R~20.99,检出限范围为0.061~0.066μg/g。2种柠檬酸酯类增塑剂的平均回收率为91.46%~107.73%,RSD为1.69%~4.73%(n=6)。运用该方法检测26种食品包装材料,仅有4种包装材料中存在柠檬酸三丁酯和乙酰柠檬酸三丁酯2种增塑剂。     

高效萃取吸管-在线凝胶色谱-气相色谱-质谱法测定淡水鱼中的农药残留量

目的 建立一种在线凝胶色谱-气相色谱-质谱(gel permeation chromatography coupled with gas chromatography-mass spectrometry, GPC-GC/MS)联用法测定淡水鱼中农药残留的检测方法。方法 采用超声辅助技术和高效萃取吸管法对南昌地区淡水鱼样品净化处理, 以乙腈为提取液, 采用氯化钠去除水分后, 经在线GPC-GC-MS系统进样分析, 选择离子检测方式定量检测。结果 25种化合物的质量浓度在一定范围内与其对应的峰面积有良好的线性关系, 相关系数大于0.996, 方法的检出限为9.1×10?5~3.1×10?1 mg/kg。以空白样品为基体进行加标回收实验, 回收率为71.4%~103.2%, 相对标准偏差小于9%。结论 该方法前处理简单快速, 灵敏度高, 有机溶剂使用量少, 适用于淡水鱼中农药残留的检测。     

RP-HPLC法测定织物中残留有机溶剂方法研究

随着多个国家针对纺织品中有机溶剂残留相关限制法规和标准的出台,纺织品中溶剂残留检测已成为生态纺织品检测体系中的一个重要项目。文中采用超纯水机械萃取,反相高效液相法(RPHPLC)同时检测纺织品中N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAc)和N-甲基吡咯烷酮(NMP)3种残留溶剂。结果表明,3种残留溶剂均具有良好的线性关系,其相关系数均大于0.999,方法检出限为1.1~2.8 mg/kg。各类纺织品中3种有机溶剂的加标回收率在94.8%~103.0%之间,实际样品测定表明该测试方法能满足织物中3种有机溶剂的日常检测要求。     

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.     

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     

Chinese CTP Market

According to Printing and Printing Equipment Industries Association of China（PEIAC）＇s statistics to the plate manufucturer in China, in 2013, the actual offset plate production has reached 346 million square meters in China. Among them, the CTP production volume was 245 million square meters, up by 11% than that of last year; the total sales of the CTP plate was 239 million square meters, up by 13%.     

Preparatory Work of Print China 2015 is Going Smoothly

正Held at Guangdong Modern International Exhibition Center,Print China 2015 will cover 7exhibition halls,besides the original Hall No.3,4,5,6,7,the newly built F zone of Hall 3 will be used too.The total area will be140,000 square meters.Hall 3:Offset and large printing equipment,package printing equipment,post press