凝胶渗透色谱-气相色谱-质谱法测定食用油中8种邻苯二甲酸酯类增塑剂

建立了凝胶渗透色谱-气相色谱-质谱法测定食用油中8种邻苯二甲酸酯类增塑剂的方法。采用凝胶渗透色谱(GPC)对食用油样品进行二次净化后进行气相色谱-质谱分析。结果表明:该方法的检出限在0.10~0.46μg/kg,定量限为0.35~1.52μg/kg,在2.38~9.52 mg/L范围内呈现良好的线性关系(R~20.99),加标回收率为89%~101%,相对标准偏差(RSD)在2.1%~7.7%之间。该方法可满足食用油中邻苯二甲酸酯类增塑剂的检测要求。     

液相色谱-串联质谱法检测动物源性食品中 7种抗病毒类药物残留

目的建立动物源性食品中7种抗病毒类药物残留的液相色谱-串联质谱测定方法。方法动物源性食品中的抗病毒类药物经甲醇-1%三氯乙酸(1:1,V:V)提取,通过固相萃取柱净化、浓缩后,在正离子模式下用液相色谱-串联质谱法检测。结果 7种抗病毒类药物检测限为0.3~1.5μg/kg,定量限为1.0~5.0μg/kg。在0.1~100μg/kg浓度范围内线性关系良好,相关系数r0.99。在1.0、5.0、10.0μg/kg三个浓度添加水平下,该方法的平均回收率为87.2%~121.4%,相对标准偏差为0.6%~8.4%(n=6)。结论本方法专属性强、准确性好、灵敏度高,适用于动物源性食品中抗病毒类药物残留的检测。     

气相色谱-质谱法测定鱼油胶囊壳中22种邻苯二甲酸酯类含量及迁移量

为测定鱼油胶囊壳中22种邻苯二甲酸酯类(PAEs)的含量及迁移量,本文建立了气相色谱-质谱检测方法(GC-MS)。胶囊壳经热水溶解,正己烷超声萃取,萃取液经氮吹浓缩后,以PAH色谱柱分离,在SIM模式下进行检测。并将该方法应用于鱼油胶囊壳中邻苯二甲酸酯的迁移研究,以精制玉米油作为食品模拟物,测定了鱼油胶囊壳中邻苯二甲酸酯的迁移量。结果表明,22种PAEs在10~500 μg/L浓度范围内线性关系良好,相关系数均大于0.9987,方法定量限为10~29 μg/kg;阴性样品的3个添加水平的平均回收率在82.1%~112.1%之间,相对标准偏差(RSD,n=6)为2.1%~7.7%。结果显示胶囊壳中存在明显的迁移现象。本方法适用于鱼油胶囊壳及食品模拟物中邻苯二甲酸酯类的测定。     

食品中黄曲霉毒素B_1的液相色谱-串联质谱测定法

建立了食品中黄曲霉毒素B1残留量的超高效液相色谱-串联质谱的检测方法。样品经乙腈+水(84+16)提取后,经多功能净化柱净化,超高效液相色谱-串联质谱法检测。本方法定量限为1μg/kg,线性范围为1~20 ng/mL;在黄曲霉毒素B1添加水平为1~10μg/kg时,在玉米样品中的回收率为95%~105%;在酱油样品中的回收率为96%~106%。     

超高效液相色谱-串联质谱法测定食品中高氯酸盐

目的建立食品中高氯酸盐的超高效液相色谱-串联质谱(UPLC-MS/MS)的测定方法。方法香辛料调味品用水提取,蔬菜、水果用乙腈-水(1∶1,V/V)提取,肉、禽、蛋、奶和水产品用乙腈-水(2∶1,V/V)提取,C_(18)柱(3 ml,200 mg)净化,以高氯酸根为内标定量,采用UPLC-MS/MS法测定。结果在0.3~20.0μg/L范围内,3种提取溶液中高氯酸盐有良好的线性关系,R~2≥0.999。加标浓度在2.0~50.0μg/kg范围内,内标相对平均回收率为82.6%~108.6%,相对标准偏差(RSD)为1.0%~9.9%。牛奶的定量限为2.0μg/kg,其他食品的定量限为10.0μg/kg。结论本方法简单快捷,定量准确,适用于食品中高氯酸盐的测定。     

固相萃取-气相色谱-串联质谱法测定紫菜中扑草净的残留量

目的建立固相萃取-气相色谱-串联质谱法测定紫菜中扑草净的残留量。方法样品用乙腈提取,经活性炭/氨基复合柱(Envi-Carb/NH_2)净化,经Rxi-5MS石英毛细管色谱柱分离,采用电子轰击源质谱检测,选择离子监测(selective ion monitoring,SIM)模式检测,外标法定量。结果扑草净在2~1000μg/L范围内具有良好的线性关系,相关系数r~2=0.9998。扑草净在5、10、20、50μg/kg 4种条件下,样品加标回收率在95.1%~107.9%,RSD在5.36%~7.77%(n=6),方法检出限为1μg/kg,定量限为4μg/kg。结论该方法操作简单,准确度与精密度较好,能快速简便地检测紫菜中扑草净的残留量。     

超声萃取-超高效液相色谱-静电场轨道阱高分辨质谱法测定涂布纸中邻苯二甲酸酯类增塑剂

建立了超高效液相色谱-静电场轨道阱高分辨质谱(UPLC/OrbitrapHRMS)同时测定涂布纸中多种邻苯二甲酸酯类增塑剂的方法,该方法以三氯甲烷为萃取溶剂,超声萃取涂布纸中的邻苯二甲酸酯类增塑剂,提取液经处理后进行UPLC/OrbitrapHRMS分析,外标法定量。样品用Hypersil GOLD色谱柱(100mm×2.1mm×1.9μm)进行分离,以5mmol/L乙酸铵水溶液(含0.1%甲酸)/甲醇为流动相,电喷雾正离子(ESI+)模式进行电离,以保留时间和准分子峰的精确质量数定性,以提取色谱峰的面积定量。23种邻苯二甲酸酯类增塑剂的质量准确度小于3mg/kg,在各自线性范围内,各组分线性良好,线性相关系数均大于0.997,检出限为0.1μg/kg~2.0μg/kg。在3个不同浓度的加标水平下,方法的加标平均回收率为80.2%~93.1%,相对标准偏差(RSD,n=9)为3.3%~9.9%。该方法定性可靠,定量准确,灵敏度高。采用该方法对市售涂布纸进行测定,在部分样品中检出不同含量水平的多种邻苯二甲酸酯类增塑剂。     

液相色谱-串联质谱法测定食品中壬基酚残留

试验旨在建立食品中壬基酚残留的液相色谱-三重四极杆串联质谱检测方法。样品经乙腈提取壬基酚同时除去蛋白质。以Hypersil GOLD C_(18)色谱柱(4.6 mm×50 mm, 1.9μm)分离,流动相为甲醇-水(10︰90, V/V),流速0.35 mL/min,液相色谱-串联质谱仪测定,内标法定量。在该优化条件下,包装饮用水的检出限为0.050μg/kg,定量限为0.100μg/kg, RSD为2.9%～5.6%;其它类食品的检出限均为1.00μg/kg,定量限均为2.00μg/kg, RSD为2.8%～9.4%。典型基质加标水平设定为10, 20和100μg/kg,方法平均回收率为86.0%～114.3%,平均相对标准偏差为2.8%～9.5%(n=6)。该方法前处理简单,灵敏度高,适用于食品中壬基酚残留的准确定性、定量分析。     

气相色谱-串联质谱法测定不同酒类食品中17种邻苯二甲酸酯

目的 建立酒类食品中17种邻苯二甲酸酯的气相色谱-串联质谱检测方法, 并对市场上不同类型酒类食品邻苯二甲酸酯含量的分布情况进行分析。方法 用正己烷提取样品, 气相色谱-串联质谱定量分析。结果 线性范围为5~10000 μg/L , 相关系数大于0.999, 仪器检出限为0.1~25 μg/L, 样品的检出限为0.001~0.1 mg/kg 。3个浓度梯度(0.3、3.0、30.0 mg/kg)的平均回收率在83.7%~105.9%, 相对标准偏差(RSD, n = 6)在1.9%~5.7%。抽样结果显示配制酒中邻苯二甲酸酯检出率较其他类型酒类高。结论 此方法灵敏度高、准确、重现性好, 适用于酒类食品中邻苯二甲酸酯的检测。     

超高效液相色谱-串联质谱法测定食品中新型添加剂爱德万甜

目的建立快速检测食品中爱德万甜的超高效液相色谱-串联质谱分析方法。方法样品经30%乙腈提取后,含乳样品再以正己烷除脂净化。采用C18色谱柱进行分离,以水和乙腈作为流动相进行梯度洗脱;质谱采用电喷雾正离子电离进行多反应监测模式(multiple reaction monitoring, MRM)监测。结果化合物爱德万甜在进样浓度为0.05～40μg/L范围内线性关系良好,相关系数(r)大于0.998。方法加标回收率(n=6)为86.1%～99.5%,相对标准偏差为0.5%～4.1%,方法的检出限为0.5μg/kg,方法的定量限为1.5μg/kg。结论该方法操作简便、检测准确、分析速度快,适合食品中爱德万甜的快速检测。     

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