超高效液相色谱-四级杆-飞行时间质谱法快速筛查与确证蔬菜水果中的多种农药残留

目的应用超高效液相色谱-四极杆-飞行时间质谱技术,针对GB 2763—2014《食品安全国家标准食品中农药最大残留限量》规定的农药残留,整合多种检测方法,建立无需标准品的快速筛查与确证蔬菜、水果中多种农药残留的方法。方法通过一级精确质量数据库比对样品准分子离子的精确质量数、同位素分布与丰度,对蔬菜、水果中农药残留进行初筛,通过实际测定样品的二级谱图与二级谱库中谱图进行比对或通过图谱解析方法进行确证。结果通过基质加标进行了方法验证,10.0和50.0μg/kg添加水平检出率均为100%,90%以上的农药化合物回收率在70%~120%,并且相对标准偏差(RSD)≤20%(n=5)。对30份蔬菜、水果样品进行筛查与确证,共检出27种农药残留,并依据GB 2763—2014进行了判定,共有2份样品超标。结论该方法的灵敏度、准确性和重复性良好,可以在较短的时间内,甚至在没有标准品的情况下,对GB 2763—2014中数百种农药进行筛查与确证,可为食品安全监管提供有效保障。     

快速滤过型净化法结合气相色谱-四极杆-飞行时间质谱同时筛查果蔬中234种农药残留

建立快速滤过型净化法结合气相色谱-四极杆-飞行时间质谱同时筛查蔬菜和水果中234种农药残留的方法。样品经过乙腈提取,提取液用m-PFC柱净化后,经气相色谱-四极杆-飞行时间质谱仪测定。通过保留时间和全扫描离子精确质量数定性,基质标准曲线定量,能够有效去除基质干扰。对12种典型果蔬样品(白菜、芹菜、番茄、黄瓜、菠菜、韭菜、油菜、橘子、梨、苹果、葡萄、橙子)进行实际样品验证。结果表明,234种农药在5~500μg/kg范围内线性良好,相关系数大于0.990,方法的检出限为5~20.0μg/kg。样品在10、50、100μg/kg3个添加水平的平均加标回收率分别为73.2%~124.8%、75.5%~122.6%和74.8%~121.7%,平均相对标准偏差分别为2.4%~13.2%、2.8%~11.4%和2.2%~10.5%。该方法有效地提高了高分辨质谱在进行果蔬农药高通量筛查时的检测效率,具有较强的实际应用价值。     

气相色谱-四极杆飞行时间质谱-内标法测定果蔬中79种农药残留

目的：建立QuEChERS 前处理结合气相色谱-四极杆飞行时间质谱(Gas Chromatography Quadrupole-Time-Of-Flight Mass Spectrometry,GC-Q-TOF/MS)内标法同时检测果蔬中79种农药残留的分析方法。方法：利用GC-Q-TOF/MS结合MassHunter、个人化合物数据库与谱库(Personal Compound Database and Spectrum Library,PCDL)软件建立429种农药的谱库;样品经QuEChERS前处理方法进行萃取净化后,结合GC-Q-TOF/MS,采用EI全扫描模式,以PCDL谱库为定性依据进行农药残留高通量快速定性筛查;针对筛查出的农药残留,进行基质内标法定量分析。结果：372批果蔬样品共筛查出79种农药残留,79种农药残留在0～2.00 μg·mL^-1线性范围内,具有良好的线性关系,相关系数R>0.99,79种农药残留的定量限在0.01～0.05 mg·kg^-1。在芹菜空白基质中0.025 mg·kg^-1、0...     

基于高分辨质谱的化妆品中防腐剂类致敏成分高通量检测方法的建立及应用

目的基于静电场轨道阱高分辨质谱,建立化妆品中异噻唑啉酮类、甲醛释放剂、对羟基苯甲酸酯类、酸类4大类防腐剂类致敏成分的高通量检测方法,幵应用于实际样品中致敏成分的筛查与定量分析。方法利用致敏成分标准品通过高分辨质谱正负离子切换FullMS/ddMS2扫描方式分析,获得多种致敏成分的保留时间、一级母离子和二级碎片离子精确质量数,构建致敏成分筛查谱库。样品经50%甲醇水溶液超声提取后,经ZORBAX Eclipse Plus C18 (3.0 mm×100 mm, 1.8μm)色谱柱分离,采用高分辨质谱分析,利用TraceFinder软件对化妆品中致敏成分与谱库相关信息匹配,实现目标物的高通量筛查确证,筛查确认后利用一级母离子外标法迚行致敏成分的定量分析。结果筛查方法既有一级母离子精确质量数和保留时间,又有二级碎片离子信息,其筛查确证结果可靠;目标化合物在相应的质量浓度范围内线性关系良好(r~20.99),检出限为0.2～20μg/g,回收率为85.6%～109.7%,相对标准偏差为3.2%～12.8%,能够满足检测需求。结论该方法简单、准确、快速,可用于化妆品中多种致敏成分的高通量快速筛查和定量分析。     

气相色谱-四极杆/飞行时间质谱法非靶向快速筛查凉茶中的农药残留

为建立QuEChERS法净化,结合气相色谱-四极杆-飞行时间质谱法(QuEChERS/GC-Q-TOF/MS)非靶向快速筛查凉茶中农药残留的方法,将样品经乙酸乙酯提取,石墨化炭黑(GCB)和氨丙基粉(NH2)分散固相萃取净化,GC-Q-TOF/MS测定。利用20种质控化合物建立的筛查方法检出限范围为2.00~50.0 μg/kg,定量限范围5.00~150 μg/kg。3个不同加标水平(25,50,125 μg/kg)下的平均回收率为73.47%～106.3%,相对标准偏差为0.91%～9.11%(n=6)。在该定量方法基础上利用目标化合物特征离子的精确质量数、二级碎片丰度比、主要离子碎片的同位素丰度比等信息进行精确质量数据库筛查与确证,以数据库检索匹配得分≥80的最低浓度作为方法的筛查限,无标准品情况下实现了非靶向筛查凉茶中751种农药残留。方法快速、准确、分析通量高,可为凉茶中农药残留的非靶向快速筛查和质量控制提供重要依据。     

高分辨质谱快速筛查牛乳中10种禁用兽药残留

采用超高效液相色谱—四级杆飞行时间高分辨质谱(UHPLC-QTOF MS)技术建立了生鲜牛乳中10种雌激素类和氯霉素类药物的快速筛查方法,并建立了此10种化合物的精确分子质量数和二级质谱碎片离子数据库。牛乳样品经乙腈提取,采用QuECh?ERS(Quick,Easy,Cheap,Effective,Rugged and Safe)方法净化。目标药物经Agilent ZORBAX SB C18色谱柱分离,以乙腈和水为流动相进行梯度洗脱,使用Dual AJS ESI源,在负离子模式下进行数据采集,基质匹配标准曲线法定量。结果表明,10种雌激素类和氯霉素类药物的定量下限为10～50μg/kg,在3个加标水平的平均回收率为61.2%～116.3%,相对标准偏差为2.3%～10.8%。结合精确分子质量数、保留时间、同位素丰度和二级特征碎片离子对目标化合物进行快速筛查与确证。该方法快速简便、准确、灵敏度较高,适用于牛乳中雌激素类和氯霉素类药物残留的高通量筛查与定性鉴定。     

超高效液相色谱-四极杆串联飞行时间高分辨质谱法筛查和确证猪肉中117种兽药残留

目的 建立117种兽药化合物的高分辨质谱一级数据库和二级谱库,建立应用超高效液相色谱-四极杆串联飞行时间高分辨质谱对猪肉中多种类兽药残留进行筛查和确证的定性分析方法。方法 均匀分散的样品经提取、净化后,通过Acquity HSS T3超高效液相色谱柱（2.1 mm×100 mm, 1.8 μm）分离,流动相梯度洗脱后进入高分辨质谱检测。在正离子模式下,通过高分辨质谱一级全扫描对样品进行分析,与数据库中的目标化合物精确质量数、保留时间进行匹配。对疑似阳性样品进一步通过二级碎片离子扫描进行确证。结果 建立的分析方法对目标化合物选择性良好,检出限在1~80 μg/kg,满足对快速筛查分析的方法学要求。结论 该方法简单、灵敏、分析速度快,适用于猪肉中117种兽药化合物的筛查和确证。     

固相萃取-气相色谱-质谱联用法筛查食用菌中的农药残留

采用气相色谱-质谱联用结合NAGINATA™软件建立了筛查食用菌中多种农药残留的分析方法。采用乙腈提取,Carbon-NH2固相萃取小柱净化,气相色谱-质谱联用检测后NAGINATA™软件全智能分析,对照每个化合物的质谱质量精度以及质谱谱图的谱库给出匹配度,通过保留时间锁定对化合物作定性判断。结果表明,18 种农药在香菇中检出限为0.001～0.050 mg/kg;平均回收率为77%～110%;相对标准偏差为1.1%～6.9%。应用所建立的方法对35 个市售食用菌样品进行了筛查,检测出2 种农药残留,残留量均低于GB 2763-2014《食品中农药最大残留限量》的限量。该方法操作便捷、快速高效,适用于食用菌中农药多残留的快速筛查。     

气相色谱-高分辨质谱法定性筛查小麦面粉中农药残留

目的 开发和验证用于小麦面粉中农药残留定性筛查的气相高分辨质谱联用方法。方法 小麦面粉样品在乙腈和柠檬酸缓冲液中混匀，加入硫酸镁和氯化钠进行盐析，混匀静置后完成液液萃取。随后上清液经过N-丙基乙二胺和碳十八官能团净化除去杂质，硫酸镁去除水分。再经过氮吹浓缩，进样气相色谱飞行时间质谱进行分析，以全扫描模式进行数据采集。最后通过高分辨质谱数据库比对和质谱工作站的自动积分完成筛查工作。结果 气相色谱飞行时间质谱提供了全面准确的离子扫描结果，当截断值为20%，400种农药都能在4 μg/kg的水平下得到正确的筛查结果，其中假阴性和假阳性率都低于5%。结论 该方法实现了高通量的农药残留筛查，结果准确，适用于小麦面粉样品中的挥发性，半挥发性农药残留的多组分筛查。     

液相色谱-四极杆飞行时间质谱用于快速筛查动物组织中多种激素残留的方法研究和应用

建立了一种采用液相色谱-四极杆飞行时间质谱（LC-Q-TOF/MS）用于快速筛查动物组织中多种激素残留的检测方法。样品通过乙腈和乙酸乙酯分步提取,提取液经增强型脂质去除吸附剂（EMR）净化,盐析后经N-丙基乙二胺（PSA）和官能化聚苯乙烯/二乙烯苯（PEP-2）进一步净化,以0.1%甲酸水?0.1%甲酸乙睛作为流动相进行梯度洗脱,在EclipsePlus-C₁₈（3.0 mm×100 mm,1.8 μm）色谱柱上进行分离,在Q-TOF/MS正离子全扫描模式下采集质谱数据,以保留时间、精确分子质量数、同位素丰度比和二级特征碎片离子定性,待测物准分子离子峰面积定量。结果表明,所有药物在各自浓度范围内线性良好,相关系数大于0.995,在10、50、100 μg/kg添加水平下,平均回收率在70.3%～116.2%之间,相对标准偏差为0.87%～8.97%,方法检测限为1～10 μg/kg,定量限为3～30 μg/kg。该方法通过构建一级精确质量数据库和二级谱库,结合保留时间、精确分子质量数、同位素丰度比和二级特征碎片离子,实现对目标化合物快速筛查和确证,具有简单快速、高灵敏度,高选择性和良好精密度的优势,适用于动物组织多种激素的快速筛查和定量测定。     

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.     

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