酶联免疫法检测猪肉中呋喃唑酮代谢物残留

通过检测猪肉中呋喃唑酮代谢物的残留以评价试剂盒的性能,采用酶联免疫法对猪肉中的呋喃唑酮代谢物残留量进行测定。结果表明:该方法的线性检测范围为0.025～2.025μg/L,最低检测限为0.1μg/kg,样本添加回收率为78.2%～100.3%,变异系数为4.7%～10.3%,与呋喃唑酮的交叉反应率为16.3%,与其他药物的交叉反应率均小于1%,且对实际样本的检测结果与液相色谱-串联质谱法基本一致。该法灵敏准确、重复性好、特异性高,适用于猪肉中呋喃唑酮代谢物残留的检测。     

高效液相色谱-三重四极杆质谱法测定猪肉及肝脏中肾上腺素代谢物

目的 建立可同时测定猪肉及肝脏中2种肾上腺素代谢物4-羟基-3-甲氧基扁桃酸和3,4-二羟基扁桃酸的高效液相色谱-三重四极杆质谱法。方法 待测样品经含0.2%甲酸的乙腈-水混合溶液（80:20,v/v）提取、固相萃取柱净化,在优化后的色谱条件、质谱条件下,经ZORBAX SB-Aq色谱柱,用高效液相色谱-三重四极杆质谱仪进行测定。采用内标曲线法对目标化合物进行定量分析,对方法学进行了考察。结果 本方法在线性范围2.5-120.0 ng/mL内,线性良好,相关系数为0.9999。方法检出限为0.3 μg/kg,在低、中、高三个浓度下,样品加标回收率范围为60.2%~104.9%,。结论 本文建立的分析方法前处理简便,线性、回收率、灵敏度及重复性均满足方法学要求,可同时对猪肉及肝脏中的2种肾上腺素代谢物进行测定。     

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定猪肉中9种大环内酯类抗生素

建立基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱筛查和确证猪肉中9种大环内酯类抗生素的方法。猪肉样品经乙腈提取,正己烷除脂,用Waters Acquity BEH C18柱(2.1 mm×100 mm,1.7μm)分离,以甲醇和0.1%甲酸溶液进行梯度洗脱,在全扫描-数据依赖扫描模式下进行检测。结果表明:9种大环内酯类抗生素的精确质量相对偏差小于1.0×10~(-6),在0.5～100 ng/mL范围内线性关系良好,相关系数均大于0.998;检出限范围为0.05～0.2μg/kg,定量限范围为0.1～0.4μg/kg;加标量为0.1～4.0μg/kg时,方法回收率为69.4%～107.6%,相对标准偏差低于10%。该方法简便、快速、准确,适用于猪肉中9种大环内酯类抗生素的快速筛查和定量分析。     

QuEChERS-多壁碳纳米管小柱-液质联用法测定猪肉中兽药残留

目的：建立一种基于QuEChERS提取、滤过型多壁碳纳米管(MWCNTs)净化技术,快速、准确的多兽残前处理方法,并应用液相色谱-质谱联用技术对猪肉中兽药残留量进行快速定量分析。方法：试样用2.5%甲酸乙腈溶液提取,滤过型多壁碳纳米管小柱净化,Accucore VDX色谱柱梯度分离,三重四极杆质谱测定,基质标准曲线法定量。同时以电喷雾离子源正模式和负模式扫描,多反应监测(MRM)模式进行采集分析。结果：猪肉中25种兽药残留在5～200 ng/mL范围内线性良好,相关系数为0.9906～0.9999,检出限范围在0.1～5 μg/kg;在猪肉空白基质中进行3水平加标试验,在10、20、50 μg/kg 3个加标浓度下,其回收率范围在71.8%～134.8%,精密度(n=6)范围在1.5%～15.3%。结论：多壁碳纳米管小柱净化效果良好,该方法简便快捷、可靠性好,适用于猪肉中兽药残留的快速定性定量分析。     

胶体金免疫层析法定量检测猪肉中克伦特罗

建立了基于T/C比值的胶体金免疫层析法快速定量检测猪肉中克伦特罗残留的新方法。胶体金免疫层析试纸条的定量检测线性范围为0.1～1.5 ng/g,检测猪肉中克伦特罗残留的最低检测灵敏度为0.19 ng/g。比较了5种猪肉组织样本中克伦特罗的简便提取方法,其中采用0.02 mol/L,含2.8%NaCl的HCl溶液抽提猪肉样品2次的提取方案,克伦特罗的平均回收率达到76.7%,变异系数为7.4%。实际样本加标回收实验显示,加标量为0.5、1.0、2.0及3.0 ng/g时,胶体金试纸条检测回收率分别为(60.4±12.8)%,(70.24±4.2)%,(75.9±4.9)%,(71.1±5.0)%。与传统ELISA方法比对,结果显示2种方法具有较好的相关性(R2=0.9136)。以上实验结果证实,基于T/C比值法的胶体金免疫层析试纸条可用于猪肉组织样品中克伦特罗的快速及定量检测。     

气相色谱质谱法测定猪肉中氯丙嗪残留

建立猪肉中氯丙嗪残留量的气相色谱质谱测定方法。方法 样品经乙酸乙酯提取,乙腈正己烷分配脱脂,MCS固相萃取柱净化,5%氨化甲醇洗脱,以气相色谱质谱选择86、233、272、318碎片离子进行定性定量分析。结果 氯丙嗪定量分析在0.051～0.25μg/ml呈良好的线性关系,r=0.9992,检出限为2.0μg/kg,平均回收率为87.1%～97.3%,RSD为3.15%。结论 该方法适合猪肉中氯丙嗪的检测。     

气相色谱-负化学源-质谱法测定茶叶中的氟虫腈及其代谢物

建立气相色谱-负化学源-质谱法测定茶叶中氟虫腈及其代谢物：氟甲腈、氟虫腈砜和氟虫腈亚砜。采用乙腈提取茶叶中的氟虫腈及其代谢物，并通过正己烷液液分配后，经PSA-SPE柱净化。采用气相色谱-负化学源-质谱法进行氟虫腈及其代谢物的检测，外标法定量。结果表明，茶叶中的氟虫腈及其代谢物在16 min内被分离。方法中4种目标物的线性范围为0.002～0.200?μg/mL，相关系数R²>0.999，检出限(R_SN=10)为0.002 mg/kg，相对标准偏差低于5%。在添加量为0.002、0.010 mg/kg和0.020 mg/kg时，加标回收率在96.33%～102.50%之间。本方法线性范围广、准确性高、重复性好，可以快速准确地对市售茶叶中氟虫腈及其代谢物进行痕量检测分析。     

超高效液相色谱-串联质谱法测定猪肉中肾上腺素残留量

建立了猪肉中肾上腺素残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)的检测方法。样品经乙腈+甲醇(95+5)提取,C_(18)色谱柱分离,超高效液相色谱-串联质谱仪检测。本方法定量限为10μg/kg,线性范围为5～500ng/mL。样品加标回收率为75%～98%,相对标准偏差为4.8%～7.9%,方法简便快速、灵敏度高,为猪肉中肾上腺素残留量测定提供了新的方法。     

高效液相色谱-串联质谱法测定乳制品中的莫奈太尔及其代谢物

建立测定乳制品中莫奈太尔及其代谢物的高效液相色谱-串联质谱法。试样加水-饱和氯化钠-乙腈溶液提取,正己烷净化,经Inertsil C8（2.1 mm×100 mm,3 μm）色谱柱分离,以甲醇-0.5 mmol/L乙酸铵溶液为流动相进行梯度洗脱,采用电喷雾离子源串联质谱,在负离子扫描方式下以多反应监测模式检测,外标法定量。结果表明：莫奈太尔及其代谢物在0.1～5.0 μg/L范围内线性关系良好,定量限为2.0 μg/kg。在3 个加标水平下的平均回收率为79.5%～102.9%,相对标准偏差为2.0%～5.3%。该方法操作简便、快速、准确、灵敏度高、抗干扰能力强、回收率和重复性良好,适合于乳制品中莫奈太尔及其代谢物的测定。     

液相色谱-串质谱法测定大米中异噁唑草酮及代谢物残留量

目的建立大米中异噁唑草酮及代谢物残留量的液相色谱-串联质谱法测定方法。方法试样中残留的异噁唑草酮除草剂及代谢物用乙酸乙腈溶液(1:99,V:V)高速匀浆提取,提取液经N-丙基乙二胺(PSA)、十八烷基硅烷(ODS)净化,经色谱柱为ACQUITY UPLC BEH Phenyl分离和流动相为1.5%乙酸的乙酸铵(1mmol/L)-乙腈进行梯度洗脱,用配有大气压化学电离源(APCI)的液相色谱-串联质谱仪检测和确证。结果异噁唑草酮及代谢物在0.0025~1.000μg/m L浓度范围内呈现良好线性关系(r=0.9998~0.9999)。当样品加标浓度在5~200μg/kg范围内时,其样品加标平均回收率为70.2%~110.6%,相对标准偏差为7.38%~12.84%。异噁唑草酮及代谢物的最低检出限分别为10μg/kg、5μg/kg。结论本方法适用于大米中异噁唑草酮及代谢物残留的同时测定。     

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