液相色谱串联质谱法测定纺织品中PFOS和PFOA

针对国际对纺织品中全氟辛磺酸(PFOS)和全氟辛酸(PFOA)的限量要求,采用ASE-300快速溶剂萃取仪提取样品中PFOS和PFOA,经浓缩、净化、过膜、定容后用液相色谱串联质谱法测定,外标法定量。采用选择离子检测进行阳性确证,建立纺织品中PFOS和PFOA的检测方法。该方法的最低检出限、线性范围和方法回收率对PFOS为1.0μg/kg、3.0~300μg/kg和82.35%~105.60%;对PFOA为0.5μg/kg、1.5~200μg/kg和85.17%~107.78%。     

QuEChERS-同位素质谱内标法检测动物源性食品中20种头孢菌素的残留量

采用液相色谱-串联质谱同位素内标法检测动物源性食品中20种头孢菌素。以甲醇作为提取溶剂提取样品中的头孢菌素,十八烷基硅烷吸附剂净化处理提取液。采用Ascentis C₈色谱柱,以0.1%甲酸水溶液与乙腈作流动相,在多反应监测模式下分别以正、负扫描模式进行分析。结果表明,17种头孢菌素的线性范围为5~100 μg/L,3种头孢菌素的线性范围为25~500 μg/L。线性方程的决定系数范围为0.9913~0.9998。20种头孢菌素在动物源性样品中的检出限为1.0~20.0 μg/kg,定量限为3.0~60.0 μg/kg。20种头孢菌素的平均回收率为78.08%~115.47%,相对标准偏差为3.07%~12.44%。该方法操作便捷,结果准确,适用于检测动物源性食品中20种头孢菌素。     

分子印迹固相微萃取-敞开式离子化质谱法快速筛查牛奶中2种全氟化合物残留

目的 建立分子印迹固相微萃取(Molecularly imprinted solid phase microextraction,MISPME)结合敞开式质谱(ambient mass spectrometry,AMS)快速检测牛奶中两种全氟化合物(全氟辛酸(PFOA)和全氟辛烷磺酸(PFOS) )残留量的分析方法。方法 牛奶样品进行蛋白质沉淀预处理后离心,上清液经氮吹干燥后加水复溶,在涡旋的条件下经分子印迹修饰的固相微萃取木签萃取,在敞开式质谱(AMS)和多反应监测(multiple reaction monitoring, MRM)模式下分析,外标法定量。结果 PFOA和PFOS在1-500 μg/L的浓度范围内线性良好,相关系数均大于0.99。PFOA和PFOS的检出限分别为0.2和0.3 μg/L,在5,10,50 μg/L 3个添加水平下平均回收率范围均处于84.8%~89.6%之间,相对标准偏差均小于8.41%。结论 分子印迹聚合物修饰的固相微萃取材料对PFOA和PFOS的选择富集性强,MISPME-AMS 方法不需要色谱分离,极大程度提高检测效率。该方法能快速、简便、灵敏的检测牛奶中的PFOA和PFOS。     

液相色谱-串联质谱法测定皮革中PFOS及PFOA盐类

建立了皮革中全氟辛烷磺酸盐(PFOS)及全氟辛酸盐(PFOA)的萃取及液相色谱-串联质谱(LC-MS/MS)的检测方法.采用索氏抽提进行萃取,溶剂为甲醇,萃取液经弱阴离子固相萃取柱(Oasis WAX)净化处理后,采用负离子电喷雾电离、多级反应离子监测(MRM)模式进行LC-MS/MS检测.结果表明,PFOS和PFOA浓度在1 ～50 μg/L范围内,线性相关系良好,相关系数均大于0.995,在10 ～160 mg/kg范围内的添加水平回收率为80%～105%,相对标准偏差为6.3%～15.5%(n=6),定量检出限均为0.5 mg/kg.该方法可用于皮革中PFOS及PFOA盐类物质的测定.     

皮革中全氟辛烷磺酸盐和全氟辛酸盐测定方法的优化

建立并优化了皮革样品中全氟辛烷磺酸盐(PFOS)和全氟辛酸盐(PFOA)的检测方法。在优化的提取温度和提取时间下,样品用甲基叔丁基醚–四丁基硫酸氢铵水溶液超声提取。提取液经浓缩、定容、过膜后,用超高效液相色谱–串联质谱(UPLC-MS/MS)检测。试验结果表明:在浓度范围0.5～20μg/L内PFOS和PFOA的标准曲线线性关系良好,方法的检测限均为0.25mg/kg,空白样品加标回收率分别在86%～96%和89%～103%之间,重复测量结果之间的相对标准偏差(RSD)小于10%。     

食品接触材料中全氟烷基磺酸类化合物的HPLC-MS/MS测定

研究食品接触材料中全氟烷基磺酸类化合物的检测方法和该类化合物的残留水平。样品采用甲醇超声提取,液相色谱-质谱联用测定,以C18为分离柱,甲醇-5mmol/L乙酸铵溶液为梯度洗脱淋洗液,同位素内标法定量,内标物为13C标记的PFOS。该方法的检出限为0.5μg/kg,线性范围为0.5～10μg/kg,方法的平均回收率为91.1%～112.8%。结果证明,该方法准确、快速,可成功应用于16种食品接触材料实样的检测。     

食品接触用纸制品中PFOS和PFOA的测定

采用高效液相色谱串连质谱内标法检测食品接触用纸制品中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)。纸制品中PFOS和PFOA的检测标准GB 31604.35-2016、SN/T 2396-2009和CEN-TS 15968-2010主要不同是试样制备、提取温度和提取方法。配制三个不同浓度的混合标准溶液进行加标回收试验,计算得到回收率在86.0%～105.5%之间,符合标准要求。通过对提取方法分析,超声提取法的提取效果最好,而快速溶剂提取法的提取温度110℃要优于70℃,应优先用超声提取法提取纸制品中的PFOS和PFOA。8个纸制品样品均检出了PFOS和PFOA残留量,其中快餐包装纸的残留量更高,而PFOS和PFOA在样品迁移试验中均未检出,同时指出生产过程中工艺不稳定或机械损失可能造成提取量的减少。下一步的研究重点是针对C_6、C_8、C_(10)、C_(12)四种系列的氟聚合物的检测,并在不同迁移模拟物、不同的迁移试验条件下研究迁移规律。     

同位素稀释气相色谱-串联质谱法测定动物源食品中克霉唑残留量

建立了动物源食品（猪肉、鸡肉、猪脂肪、猪心、猪肝、猪肾）中克霉唑残留量的同位素稀释气相色谱-串联质谱（GC-MS/MS）测定方法。样品经加速溶剂提取后,用凝胶渗透色谱净化。采用HP-5 MS色谱柱（30 m×0.25 mm×0.25 μm）进行分离,多反应监测（MRM）模式检测,同位素内标法定量。实验结果表明,克霉唑在1~100 μg/L浓度范围内线性良好,决定系数（R2）为0.9995,定量限（LOQ,S/N≥10）为2.0 μg/kg。在2.0、5.0、20.0 μg/kg加标水平下,回收率在82.6%~116.5%之间,相对标准偏差为5.2%~13.5%。该方法灵敏度高、准确性好,能够满足动物源食品中克霉唑残留量的确证和定量分析。     

中国部分主产区鸡肉中全氟化合物残留水平调查

目的通过对中国鸡肉部分主产区2014年1月至2015年4月的619份鸡肉样品中19种全氟化合物(11种全氟羧酸和8种全氟磺酸盐)浓度的检测,进行全氟化合物在鸡肉中污染状况的分析评价。方法样品采用溶剂萃取固相填料净化结合高效液相色谱-串联质谱法(HPLC-MS/MS)进行分析。结果 619份鸡肉样品中全氟化合物的总检出率为83.8%,共检出17种全氟化合物,以全氟戊酸(perfluoropentanoic acid,PFPe A)、全氟辛酸(perfluorooctanoic acid,PFOA)和全氟壬酸(perfluorononanoic acid,PFNA)的残留为主,其含量分别为0~1.26μg/kg,0~2.19μg/kg和0~0.76μg/kg。结论鸡肉部分主产区中PFCs的残留水平具有区域差异,人体健康风险评价表明,该4省市的鸡肉中PFOA和全氟辛烷磺酸盐(PFOS)不会对人体造成即时危害。     

基于液相色谱-串联质谱法的纺织品中痕量全氟化合物的测定

采用超声法提取纺织品中的全氟化合物。以C18为分析柱,甲醇-5 mmol/L乙酸铵为梯度洗脱淋洗液, 13 min内即可分离全氟己酸(PFHxA),全氟辛酸(PFOA),全氟壬酸(PFNA),全氟癸酸(PFDA),全氟十一酸(PFuDA),全氟十二酸(PFDoA), 全氟丁烷磺酸(PFBS),全氟己烷磺酸(PFHxS),全氟辛烷磺酸(PFOS),全氟癸烷磺酸(PFDS) 10种分析物。以313.1/268.9,412.9/368.9,462.9/418.9,512.7/468.9,562.7/518.9,612.8/568.9,298.8/99,399.2/99,498.8/99,599/99分别对PFHxA,PFOA,PFNA,PFDA,PFuDA,PFDoA,PFBS,PFHxS,PFOS,PFDS进行监控和定量分析。利用同位素内标法进行定量,线性范围和添加回收率分别为0.5～10 µg/m2、84.6%～111.8%,检出限为0.5 µg/m2,低于欧盟指定针对纺织品1 µg/m2 的限定。结果表明,本方法准确、快速,并成功用于20种纺织品实样的检测。     

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.     

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