分散固相萃取净化-气相色谱-质谱联用法测定茶叶中7种杀螨杀虫类农药残留

目的建立茶叶中7种农药残留的快速检测方法。方法采用分散固相萃取净化,气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)测定茶叶中噻螨酮、噻嗪酮、哒螨灵、喹瞒醚、苯醚甲环唑、联苯菊酯和氟氰戊菊酯7种农药的残留。结果 7种农药在0.05~5.00 mg/kg范围有良好的线性关系,相关系数均大于或等于0.9995。3个浓度的平均加标回收率为70%~115%,相对标准偏差为5.0%~13.2%;方法检出限(limit of detection,LOD)为0.005~0.05 mg/kg,定量限(limit of quantitation,LOQ)为0.015~0.15 mg/kg。采用此方法抽检了我国不同地区市场上的110批次的茶叶样品,其中有15批次样品检出联苯菊酯,含量在24~1640μg/kg之间;有4批次样品中检出噻嗪酮,含量在35~150μg/kg之间;3批次样品检出哒螨灵,含量在70~200μg/kg之间。结论本方法符合农药残留分析标准的要求,可用于茶叶中7种农药残留的快速检测和确证分析。     

进口粮谷中农药残留状况普查与分析

目的根据各进口国粮谷样品农药残留检出情况,确立进口粮谷中重点监测的农药残留品种和评估潜在的农药残留风险。方法采用修改的GB/T 19649-2006和GB/T 20770-2008方法,对粮谷主要进口口岸青岛、深圳和秦皇岛在2010~2014年期间进口的62例大豆、62例大麦和28例大米样品进行了690种农药残留检测,共获得104880个检测数据。结果来自6个进口国的62例大豆样品均未检出农药残留。来自3个进口国的62例大麦样品中,有8例样品检出5种农药,检出率12.9%;其中检出1种农药的样品占4.8%,检出2种农药的样品占6.5%,检出3种农药的样品占1.6%;检出的农药残留水平在10~1000μg/kg范围的占检出总数的85.7%,大于1000μg/kg占检出总数的14.3%。来自6个进口国的28例大米样品中,有5例样品检出5种农药,检出率17.9%;其中检出1种农药的样品占14.3%,检出2种农药的样品占3.6%;检出的农药残留水平低于10μg/kg占检出总数的50.0%,大于10μg/kg占检出总数的50.0%。大麦和大米样品中检出的农药品种为低毒农药的均占80%,检出的农药为中毒农药的均占20%。按照中国最大残留限量(MRL)标准衡量,只有1例大麦样品检出的溴氰菊酯超出标准要求;按照欧盟MRL标准衡量,4例大麦样品检出的杀螟硫磷超出标准要求;按照日本MRL标准衡量,没有样品检出超标农药。结论我国进口粮谷的农药残留检出率低于10%。农药残留水平处于安全水平。但同时也应当加强溴氰菊酯、杀螟硫磷、甲基嘧啶磷、毒死蜱、甲基毒死蜱、丙环唑、嘧菌酯、增效醚的检测,特别是溴氰菊酯和杀螟硫磷农药残留的监控,以保障消费者的食品安全。     

QuEChERS-液相色谱-串联质谱联用法测定草莓中毒死蜱及其代谢物

目的建立草莓中毒死蜱及其代谢物残留检测的QuEChERS-液相色谱-串联质谱联用方法。方法草莓样品用乙腈提取后所得液经过QuEChERS法净化去除杂质。采用5 mmol乙酸铵水-甲醇流动相体系进行洗脱,C_(18)色谱柱进行色谱分离,电喷雾正负离子模式电离,多反应监测(multiple-reaction monitoring,MRM),外标法定量。结果 3,5,6-三氯-2-羟基吡啶(3,5,6-trichloro-2-pyridi-nol,TCP)、毒死蜱、毒死蜱氧和甲基毒死蜱在1.0~200μg/L浓度范围内线性良好,相关系数均为0.999,检出限为0.008~0.279μg/kg,定量限为0.026~0.926μg/kg。在0.010、0.050和0.100 mg/kg 3个浓度水平的平均回收率为71.33%~99.43%,相对标准偏差在1.51%~5.96%之间。结论本方法操作简便,耗时较短,准确度与精密度较好,适应性广,容易形成标准化操作,可用于草莓样品中毒死蜱及其代谢物残留的分析。     

QuEChERS-HPHPLC联用法检测蔬菜中有机磷农药多残留分析

建立了QuEchERS-HPLC联用法检测蔬菜中有机磷农药多残留的方法。改进了QuEchERS前处理方法,提高回收率及结果准确性,然后运用HPLC进行分析检测,根据有机磷农药的差异,得出其最小检出限在0.02～55.75μg/kg之间,定量限0.1～189.23μg/kg,18种有机磷农药要在定量限浓度和四倍定量限浓度2个加标水平的回收率均在70~120%范围,相对标准偏差低于20%,试验表明本方法适用于蔬菜中有机磷农药的多残留检测分析。     

气相色谱-串联质谱法同时分析葡萄基质中 196种农药残留

目的建立同时分析葡萄基质中196种农药残留的气相色谱-串联质谱(GC-MS/MS)方法。方法葡萄样品经乙腈提取,QuEChERS方法净化,加入内标环氧七氯,采用GC-MS/MS在多反应监测模式(MRM)下分析,38 min内即可完成196种农药的分离,内标法定量。结果 196种农药在10~1000μg/L的浓度范围内线性关系良好,相关系数(r~2)大于0.99,各农药的检出限(S/N=3)为0.1~2.5μg/kg,各农药的定量限(S/N=10)为0.3~8.3μg/kg,在10.0μg/kg和50.0μg/kg 2个水平的添加浓度下,回收率在60.5%~126.2%之间,相对标准偏差0.2%~16.1%(n=6)。结论该方法准确可靠,灵敏度高,可用于葡萄基质中196种农药残留的同时检测。     

QuEChERS-GC-MS/MS法同时测定稻草中的106种农药残留

建立了一种稻草中106种农药残留的气相色谱-三重四极杆串联质谱检测方法。样品经QuEChERS技术提取和净化后,采用GC-MS/MS在选择反应监测模式(SRM)下定性定量。结果表明,(1)106种农药在稻草中的定量限(LOQ)为1.1~49.2μg/kg;(2)在4~492μg/L范围内,线性相关系数为0.9905~0.9999;(3)在稻草样品中添加浓度在36.5~1255.0μg/kg之间时,平均回收率在65.2%~124.1%之间,RSD在0.6%~19.4%之间;(4)该方法农药种类覆盖广、前处理简便、溶剂用量少,可应用于稻草中106种农药残留的快速筛查与定量分析。     

QuEChERS-气相色谱-串联质谱法同时测定高粱中16种农药残留

摘 要：目的 建立了三重四极杆气质联用仪GC-MS/MS 结合改良的 QuEChERS 方法同时检测高粱中16种农药多残留的分析方法。方法 高粱粉末加水浸润后,加入WondaPak QuEChERS提取盐试剂包Ⅱ均质提取,取上清液加入WondaPak QuEChERS 净化管Ⅲ净化,氮吹近干,定容至1mL,基质内标法定量。结果 在质量浓度为0.05~1.00μg/mL范围内,各农药的线性关系良好,线性回归方程的相关系数（R2）均大于0.998,方法检出限为0.00124μg/kg ~0.654μg/kg。分别向阴性高粱样品中添加16种农药标准品浓度为0.01mg/kg、0.10mg/kg和0.50mg/kg的3个水平,其加标平均回收率为78.54%~102.22%,相对标准偏差RSD%（n=6）为1.23%~9.52%。结论 与其他农药残留检测方法比,该方法具有前处理操作简单,重复性好,灵敏度高,简化样品前处理过程,降低分析成本等优势,适用于高粱样品中常用农药的高灵敏度快速检测。     

快速溶剂萃取-凝胶渗透色谱净化-气相色谱-串联质谱分析猪肉中109种农药残留

目的建立一种同时分析猪肉中109种农药残留的气相色谱-串联质谱(GC-MS/MS)方法。方法样品经快速溶剂萃取仪提取,凝胶渗透色谱仪净化,加入内标环氧七氯,采用GC-MS/MS在多反应监测模式(MRM)下分析,内标法定量。结果 109种农药在10~500μg/L的浓度范围内线性关系良好,相关系数(r~2)大于0.99。各农药的检出限(S/N=3)为0.09~1.57μg/kg,各农药的定量限(S/N=10)为0.31~4.78μg/kg,在10.0、20.0和50.0μg/kg 3个水平的添加浓度下,回收率在68.3%~112.8%之间,相对标准偏差小于14.2%(n=6)。结论该方法准确可靠、灵敏度高,可用于猪肉中109种农药残留的同时检测。     

高效液相色谱-串联飞行时间质谱法测定茶叶中6种农药的残留量

建立了茶叶中噻嗪酮、毒死蜱、啶虫脒、吡虫啉、乐果、多菌灵等6种农药残留量的高效液相色谱-串联飞行时间质谱检测方法。茶叶样品经酸化乙腈提取,基质分散固相萃取净化。经高效液相色谱分离后进入飞行时间质谱检测。6种农药浓度在1～50μg/kg下线性关系良好,相关系数R2在0.995～0.999之间,检测限在0.01～1μg/kg之间,回收率在80%～102%之间,相对标准偏差(RSD)在4%～6%之间。该方法快速、准确、灵敏度高,能够满足茶叶中多种农药残留的定性、定量检测需求。     

桃胶中多农药残留分析及风险评估

目的:研究桃胶中农药残留及风险。方法:基于液相色谱—串联质谱法(LC-MS/MS)建立桃胶中44种农药残留的定量分析方法,并对全国173份桃胶样品进行农药残留检测和风险评估分析。结果:基于LC-MS/MS农药残留检测方法的检出限(LOD)为0.05～1.80μg/kg,定量下限(LOQ)为0.20～2.42μg/kg,加标回收率为61.77%～119.48%。桃胶样品中共检出22种农药,农药总检出率为98.8%,平均每个样品检出农药次数为2.8次,苯醚甲环唑检出率最高(95%),其次是毒死蜱(54%)、多菌灵(34%)、呋虫胺(32%)、吡唑醚菌酯(19%)等。不同桃胶样品中苯醚甲环唑平均残留量最高为0.332 mg/kg,其次是呋虫胺(0.093 mg/kg)、多菌灵(0.061 mg/kg)、毒死蜱(0.033 mg/kg)。结论:桃胶中农药的残留与桃生产用药有关,其残留量总体处于低风险水平,推荐8—10月份采摘桃胶。     

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