一起可疑食物中毒样品中克百威的检测分析

【【摘要】目的 快速、准确地检测出引起化学性食物中毒的毒物及其含量，为食物中毒应急处置提供科学依据。方法 根据食物中毒调查及处理原则，采用“NY／T 761—2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定”方法中气相色谱(GC/FPD)和高效液相色谱一柱后衍生、荧光光度法对基层疾控中心送检的2份可疑食物，进行农药残留量测定。结果 分别在浸泡的粉条和鸡蛋炒粉条中检测出高浓度的克百威（27.0g/kg和5.4g/kg）。结论 本次化学性食物中毒为克百威引起。     

液相色谱-串联质谱法检测一起由化学物质引起的食物中毒

目的以一起有毒化学物质引起的食物中毒事件为例,建立化学性食物中毒的检测体系。方法利用液相色谱-串联质谱(LC-MS/MS)的增强子离子扫描(EPI)模式对6份可疑食物样品进行16种有机磷类农药和12种氨基甲酸酯类农药的定性检测。结果在烩菜和肝脏样品中检出氨基甲酸酯类毒性物质克百威,其他4份样品中均未检出该毒物。所有样品均未检出有机磷类农药和其他11种氨基甲酸酯类农药。结论本次事件是由克百威引起的食物中毒。实验室建立灵敏、快速和准确的LC-MS/MS法和质谱数据库,在突发事件中具有重要的意义。     

气相色谱-质谱联用法快速检测食物中毒 案例中的克百威农药

目的通过气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)快速检测食物中毒案例的样品中克百威农药。方法使用丙酮快速提取样品,离心后取上清液,上机待测。运用全扫描方式监测,通过全扫描提供的质谱图由谱库检索出可疑物质,再根据保留时间和质谱图中特征离子准确定性。配制标准系列通过选择离子扫描模式监测方式,外标法定量。结果在导致食物中毒的现场采集的样品中检出致毒因子杀虫剂农药克百威。配制克百威标准浓度为0.10~2.00 mg/L范围内呈良好的线性关系,相关系数(r~2)=0.9989,加标回收率为86%~101%,相对标准偏差(relative standard deviation,RSD)为2.2%~5.8%。样品中克百威的含量最高达到了232 mg/kg。结论此方法操作简单、易行,是快速、有效的一种毒物分析方法。     

超高效液相色谱-四极杆飞行时间质谱筛查一起由生物碱引起的食物中毒

目的 采用超高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF MS)技术对1起食物中毒事件的样本进行筛查,为患者救治及做好此类中毒的检测提供策略和依据。方法 患者的呕吐物、洗胃液和食物样本经酸化乙腈提取,C18固相萃取填料净化,利用UPLC-QTOF MS进行非依赖型全信息质谱数据采集,经UNIFI软件进行峰谱识别和谱库检索。结果 在5份人体样本中均检出莨菪碱,含量低于1 mg/kg,其中1人的胃液样本中筛出阿奇霉素;未发现莨菪碱代谢产物,与大鼠暴露实验结果一致。结论 由实验室检测结果推断本次事件是由莨菪碱引起的家庭食物中毒。UPLC-QTOF MS高分辨质谱筛查技术在处理由化学性物质引起的食物中毒突发事件中具有重要的实用价值。     

UPLC-MS-MS法测定水产品中克百威及其代谢物

采用超高效液相色谱-串联质谱技术建立同时测定水产品中克百威及其代谢物(3-羟基克百威、3-酮基克百威和呋喃酚)含量的方法。样品经乙腈提取,正己烷脱脂,HLB固相萃取柱净化,色谱柱分离,电喷雾串联四极杆质谱进行检测,采用多反应监测分析,并对液质分离条件及参数和样品前处理条件进行优化。结果显示,克百威及其代谢物在0.08～100ng/mL范围内线性良好(0.998 3～0.999 7)。在0.25～2.5μg/kg时,平均加标回收率在87.9%～96.1%,RSD值在1.4%～9.5%。该方法测定克百威、3-羟基克百威、3-酮基克百威和呋喃酚的检出限均为0.25μg/kg。该方法快速、准确、灵敏,可用于水产品中克百威及其代谢物残留量的测定。     

QuEChERS-高效液相色谱-串联质谱法测定春笋中4种农药残留

目的建立检测春笋中吡虫啉、茚虫威、辛硫磷和克百威4种农药的QuEChERS-高效液相色谱-串联质谱法。方法前处理采用QuEChERS方法,乙腈为提取液,N-丙基乙二胺(PSA)为净化剂,结合液相色谱-质谱联用技术,正离子多反应监测(MRM)模式进行检测,外标法定量。结果吡虫啉、茚虫威、辛硫磷和克百威4种农药在0.5～20.0 ng/ml范围呈良好的线性关系,相关系数(r~2)均大于0.991,在4～40μg/kg加标范围内,4种农药的回收率为72.4%～92.8%,精密度为1.5%～9.2%,方法的检出限为0.4μg/kg,定量限为1.2μg/kg。结论建立了适用于检测春笋中吡虫啉、茚虫威、辛硫磷和克百威4种农药的QuEChERS-高效液相色谱-串联质谱法,该方法准确、灵敏、高效、简便。     

一起牛奶中脱氢乙酸钠中毒事件调查分析

目的对疑似牛奶中毒事件进行流行病学调查分析,查明引起食物中毒原因,为类似突发应急食物中毒事件处置提供参考。方法根据现场流行病学调查,采用高效液相色谱等方法对样品进行检测,综合分析判定食物中毒原因。结果本次食物中毒事件发病28人,送检的牛奶样品中检出脱氢乙酸钠,含量为1.70和1.71 g/kg,未发现含有其他毒物。结论本次中毒事件是由牛奶中违规添加高浓度脱氢乙酸钠引起。     

液相色谱-串联质谱法同时检测蔬菜中克百威和3-羟基克百威残留

目的建立一种克百威及3-羟基克百威农药残留的液相色谱-串联质谱(liquid chromatographytandem mass spectrometry,LC-MS/MS)检测方法。方法样品经乙腈提取,氯化钠盐析除水后,过氨基固相萃取柱净化,甲醇和二氯甲烷混合溶液洗脱。采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对定量离子和定性离子进行监测。结果本方法在15 min内完成2种目标化合物的分离分析。克百威和3-羟基克百威在10、30和100μg/kg添加水平的回收率为72.0%~106.4%,相对标准偏差小于6.9%(n=6),方法定量限为10μg/kg。结论该方法快速、准确、灵敏,适合测定蔬菜中克百威及3-羟基克百威药物残留。     

一起由涕灭威引起的食物中毒调查报告

快速、准确地检测出引起群体性食物中毒的有毒物质及其含量,为食物中毒应急处置提供科学依据。方法 根据食品安全事故流行病学调查技术指南及NY/T 584—2002《西瓜(含无子西瓜)》行业标准,采用多种方法对基层疾控中心送检的 3份可疑西瓜样品进行检测。结果 分别在送检的3份西瓜样品中检测出高浓度的涕灭威及其氧类似物(亚砜、砜)。结论 本次学生食物中毒由涕灭威引起。     

2004—2012年甘肃省食物中毒事件分析

分析甘肃省2004—2012年食物中毒事件的发生规律和流行特点。方法 对甘肃省2004—2012年突发公共卫生事件报告管理信息系统中所报告的食物中毒资料进行描述性流行病学分析。结果 2004—2012年全省共报告食物中毒事件78起,中毒2508人,病死率为2.15%(54/2508);报告事件多发生在第二、三季度;中毒场所以家庭最多,占总报告起数的41.03%(32/78);微生物引起的食物中毒事件报告起数和发病人数均最多,分别占总数的33.33%(26/78)和60.41%(1515/2508);化学性食物中毒引起的死亡人数最多,占总死亡人数的62.96%(34/54)。结论 甘肃省食物中毒事件的发生以微生物性食物中毒为主,但引起食物中毒死亡的主要原因是误食农药、鼠药污染的食品。     

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