UPLC-Quadrupole/Orbitrap HRMS同时测定玉米中多种真菌毒素和农药残留

采用直接提取稀释快速前处理技术,利用超高效液相色谱-四级杆/静电场轨道阱高分辨质谱,建立了玉米中常见的16种真菌毒素和11种农药残留的快速同时分析方法。样品采用乙腈∶水∶乙酸溶液(70∶29∶1,V/V/V)提取,提取液稀释后即可进行仪器测定。以C_(18)色谱柱进行色谱分离,通过全扫描模式进行定量检测。结果表明,16种真菌毒素和11种农药残留在本实验的线性范围内都具有良好的线性关系,相关系数(R~2)大于0.999,高中低三浓度添加水平回收率(n=6)为79.6%~116.9%,相对标准偏差为0.5%~12.2%。方法简单、快速和准确,可满足玉米真菌毒素和农药残留的日常检测和监测工作的需要。     

分散固相萃取—超高效液相色谱—串联质谱法测定液态奶中11种农药残留量

目的：评估液态乳中农药残留量的安全性。方法：建立同时测定11种农药残留的超高效液相色谱—串联质谱法。待测样品经乙腈提取，C₁₈和PSA固相萃取剂净化，经色谱柱Xbridge BEH C₁₈ （100 mm×2.1 mm，1.7 μm）分离，多反应监测模式进行测定，并使用响应曲面法优化前处理参数。结果：前处理的最佳条件为乙腈用量10 mL，C₁₈用量50 mg，PSA用量30 mg。11种农药在1.0~100.0 μg/L的浓度范围内线性关系良好，相关系数（R²）均＞0.999。在10，20，100 μg/kg添加水平内，11种农药的平均回收率为82.7%~102.0%，相对标准偏差为2.89%~8.87%，检出限和定量限分别为2.0~3.0，5.0~10.0 μg/kg。结论：该方法操作简便，分析时间短，回收率高，重现性好，能够准确定性定量分析液态乳中11种农药残留量。     

全碳标记稳定同位素内标-超高效液相色谱-串联质谱法测定粮食中16种真菌毒素

考察高效液相色谱-串联质谱-全碳标记的稳定同位素内标法精确测定小麦和玉米中16种真菌毒素方法的适用性。样品经提取稀释、加入内标,高效液相色谱-串联质谱测定。结果表明,16种真菌毒素线性相关系数大于0.997,3个水平的添加回收率为83%~114.3%,相对标准偏差为0.9%~13%,定量限为0.5~200μg/kg,通过检测FAPAS04223质控样品和小麦、玉米样品验证了方法的准确性和适用性,能够快速、批量、准确的测定小麦和玉米中16种真菌毒素,为我国粮食真菌毒素污染监测提供便利。     

固相萃取-气相色谱法同时检测草莓中13种 农药残留

目的 建立一种固相萃取-毛细管柱气相色谱方法,可以同时检测草莓中13种农药残留量。方法 草莓样品匀浆后,经乙腈提取,NH₂固相萃取柱净化,采用HP-5毛细管气相色谱柱进行分离,GC-ECD 进行定性及定量分析。结果 13 种农药残留的色谱图分离效果良好,线性相关系数均大于0.996,方法检出限在0.01 mg.kg_-1~0.5 mg.kg_-1之间。添加回收试验表明,该方法平均回收率在70.5~114.5 % 之间,相对标准偏差在2.17~6.85 %之间。结论 该方法简单、快速、灵敏、净化效果好、回收率高,适合草莓中多种农药残留的检测和安全监控。通过对50份草莓样品进行检测,检出百菌清、乙草胺、毒死蜱、粉唑醇、醚菌酯、烯酰吗啉6种农药。     

QuEChERS-高效液相色谱-串联质谱法测定粮谷中啶磺草胺的残留

目的 建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定粮谷中啶磺草胺的分析方法。方法 样品经酸化乙腈(含0.5%(V/V)乙酸的乙腈)提取,优化的QuEChERS(400 mg C₁₈、400 mg无水硫酸镁)方法净化,净化液经离心后,直接过膜上机检测。HPLC-MS/MS方法以0.1%(V/V)甲酸水-乙腈为流动相,流速为0.3 mL/min梯度洗脱,采用C₁₈色谱柱进行分离,电喷雾正离子电离(ESI^₊),多反应监测(MRM)检测,基质匹配外标法定量。结果 在11种基质(大豆、大麦、大米、高粱、黑麦、苦荞、土壤、小麦粉、小麦、燕麦、玉米)中,啶磺草胺在0.001~0.03 μg/mL质量浓度与其对应的峰面积之间线性关系良好,R^₂均大于0.996,在0.005、0.01和0.05 mg/kg 3个添加水平下,啶磺草胺的平均回收率在90.3%~112.3%之间,相对标准偏差在1.1%~7.9%之间。结论 方法准确度、精密度和灵敏度均符合农药残留检测的要求。     

气相色谱-四极杆/飞行时间质谱快速筛查紫甘蓝中406种农药残留及其在欧盟能力验证中的应用

目的 建立了紫甘蓝中406种农药残留的气相色谱-四极杆/飞行时间质谱(GC-QTOF/MS)检测方法。方法 采用1%(v/v)乙酸乙腈溶液对紫甘蓝样品均质提取,4g无水硫酸镁和1g氯化钠盐析,通过自动固相萃取装置使用Carbon/NH₂柱净化。应用GC-QTOF/MS在全扫描模式下采集数据,优化共流出得分和提取特征离子数等筛查参数,在最佳筛查参数下,将采集得到的数据与PCDL库中化合物信息比对进行筛查。结果 方法的筛查限(SDLs)范围为1-50 μg/kg,定量限(LOQs)范围为5-50 μg/kg,在1倍LOQ、2倍LOQ和10倍LOQ三个添加水平下,平均回收率范围分别为62.7%~119.6%,69.7%~119.6%和64.6%~119.8%,相对标准偏差范围分别是1.0%~17.8%,0.1%~18.4%和1.0%~18.2%,在相应的浓度范围内,406种农药的线性相关系数(r)不小于0.99。结论 应用该方法对2019年欧盟能力验证(EUPT)的紫甘蓝样品进行农药残留检测,检出了所有农药,并获得A类实验室的评价,结果表明,该方法准确、可靠,适用于紫甘蓝等色素较多的碱性样品中农药多残留筛查。     

2019年云南市售大米真菌毒素污染水平及风险评估

目的 对云南省市售大米中16种真菌毒素污染水平进行检测并对其食用安全进行风险评估。方法 采用高效液相色谱-串联质谱法(HPLC-MS/MS)检测分析,根据检测结果进行食用安全性评估。结果 云南省市售大米中16种真菌毒素检出率为73.3%,含量范围为ND～2891μg/kg,其中黄曲霉毒素B₁超过国家限量标准,超标率为10.0%;与JECFA规定的暂定每日最大耐受摄入量(PMTDI)为0.06μg/kg.d,本次调查HT₂毒素暴露量为0.0836 μg/kg.d,超过JECFA暂定的PMTDI规定值。雪腐镰刀烯醇(NIV)是JECFA规定的PMDTI的10种真菌毒素中贡献率最高的真菌毒素,达48.03%。结论 云南省市售大米中真菌毒素的污染水平较低,由其引起的健康风险较低,但仍存在一定健康风险。     

固相萃取-气相色谱法测定玉米中有机氯和 拟除虫菊酯农药残留量

目的建立气相色谱-电子捕获检测器法(GC-ECD)测定玉米中16种有机氯和拟除虫菊酯农药残留量的方法。方法玉米样品经乙腈超声提取后,使用Florisil进行固相萃取净化,样品经氮吹浓缩后,使用气相色谱电子捕获检测器测定。结果 16种有机氯和拟除虫菊酯农药在0.01~0.5 mg/L浓度范围内呈现良好线性关系,R2大于0.99;在0.02、0.05、0.2 mg/kg三个添加浓度上回收率范围为71.0%~103%,相对标准偏差1.28%~8.74%,检出限在0.1~16μg/kg之间。结论该方法前处理操作快速简单,能够有效净化样品,满足玉米中有机氯和拟除虫菊酯农药的日常检测和监管工作,适用于大批次样品的定性定量分析。     

广东省稻谷中真菌毒素污染状况研究

目的 了解广东省主要水稻种植区稻谷中真菌毒素的污染模式,分析不同地区真菌毒素的分布,为实施精准防控措施提供参考。方法 2018—2019年在广东省珠三角、粤北、粤东、粤西四个片区的8个地市采集120份稻谷样品,采用超高效液相色谱-串联质谱仪多反应监测模式测定16种真菌毒素的污染状况。结果 本次监测的稻谷中19.17%(23/120)样品检出真菌毒素,主要污染种类为黄曲霉毒素和伏马菌素。伏马菌素B₁(FB₁)检出率为9.17%(11/120);黄曲霉毒素B₁(AFB₁)的检出率为8.33%(10/120),有2份样品超过国家限量值(10 μg/kg),污染水平分别为73.90和18.80 μg/kg。6种单端孢霉烯族化合物中仅检出脱氧雪腐镰刀菌烯醇(DON)及其乙酰化化合物,其中DON的检出率为1.67%(2/120),3-Ac-DON和15-Ac-DON的检出率均为0.83%(1/120)。玉米赤霉烯酮(ZEN)的检出率为3.33%(4/120),杂色曲霉素检出率为1.67%(2/120)。监测的120份样品未检出赭曲霉毒素A(OTA)、雪腐镰刀菌烯醇(NIV)、T-2和HT-2毒素。8.33%(10/120)样品受到2种及以上真菌毒素污染,以AFB₁和其他真菌毒素的混合检出多见。不同地市的污染模式有所差异,湛江市样品中FB₁、FB₂、DON和3-Ac-DON的含量较高,河源市样品中AFB₁、AFB₂、杂色曲霉素、FB₁、FB₂的含量较高,韶关市样品中ZEN、DON和3-Ac-DON的含量较高。结论 广东省稻谷中受到多种真菌毒素污染,且受污染的真菌毒素种类存在地域差异。应针对稻谷中多种真菌毒素的混合污染模式,科学评估暴露风险,采取针对性的控制措施,保护消费者的饮食安全。     

自动QuEChERS结合气相色谱-串联质谱法测定花生油中172种农药残留

目的：基于自动QuEChERS方法建立了花生油中172种农药残留的气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)快速检测技术。方法：花生油样品加水后,加入15 mL乙腈提取,放入自动QuEChERS前处理设备,以N-丙基乙二胺(primary secondary amine,PSA)和十八烷基硅烷键合硅胶(C18)为填料进行净化。净化后,取2 mL上清液,在氮气气流下吹至近干,用1 mL乙酸乙酯复溶后,过0.22 μm有机微孔滤膜,应用气相色谱－串联质谱(GC-MS/MS)检测,HP-5MS UI气相色谱柱分离,程序升温,在多重反应监测(MRM)模式进行测定,采用基质匹配外标法进行定量。结果：方法所检测的172种农药的线性决定系数(R_²)均大于0.995,检出限范围为1～5 μg/kg,定量限范围为2～10 μg/kg;在10 μg/kg、50 μg/kg和100 μg/kg 3个添加水平下,平均回收率在70.1%～112.8%、72.6%～114.3%、71.8%～114.9%范围内,相对标准偏差(RSDs)均小于15.0%(n=6)。结论：该方法操作简单,灵敏高效,能够满足花生油中多农药残留检测的需求,也可以为复杂基质的自动化前处理提供参考。     

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