葡萄中43种农药残留的快速分析方法与膳食暴露风险评估

采用改进的QuEChERS(Quick, Easy, Cheap, Effective, Rugged and Safe)方法进行样品前处理,结合气相色谱串联质谱(Gas chromatography-tandem mass spectrometry, GC-MS/MS),建立了葡萄中43种农药残留的分析方法。采用此方法对武汉市2022年采集的124份市售葡萄样品进行检测,分析其农药残留现状。通过膳食摄入风险和食品安全指数法对农药残留的膳食暴露风险进行评估。结果表明,43种农药在1～500μg/L线性关系良好,相关系数R2均大于0.99。该方法的检出限为0.08～3.11μg/kg,定量限为0.24～9.33μg/kg;在3个水平(10、50、100μg/kg)的添加浓度下,回收率为71.7%～128.8%,相对标准偏差为2.6%～9.7%,可满足葡萄中农药残留检测的要求。124份样品农药残留的检出率为46.8%,共检出12种农药。其中,氯氟氰菊酯和氯氰菊酯超标,超标率分别为3.2%和0.8%。对检出的12种农药进行膳食暴露风险评估,慢性膳食暴露风险范围为0.092%～0.598%,急...     

广西六堡茶中9,10-蒽醌残留量测定分析及膳食暴露量评估

为掌握广西地区六堡茶中有机污染物9,10-蒽醌残留情况与居民膳食暴露量,试验采用气相色谱-串联质谱法对在广西地区收集的不同陈化时间的98份六堡茶样品进行9,10-蒽醌含量检测,并进行相应膳食暴露量评估。结果表明：98份六堡茶样品中62份检测出9,10-蒽醌残留,检出率63.26%(62/98),残留量范围12.00～410.21μg/kg,平均残留量40.1μg/kg;参考欧盟EUNo 1146/2014中茶叶9,10-蒽醌残留限量20μg/kg进行判定,样品超标率56.12%(55/98),其中陈化时间15～20年组样品超标率最高,为94.12%(16/17),平均含量最高达111.68μg/kg;参考六堡茶感官审评国家标准方法浸泡茶叶样品,样品中9,10-蒽醌平均浸出率为8.12%;试验采用单项指数法对样品中9,10-蒽醌进行污染评价,发现出现轻度污染以上样品占比高达56.13%;根据点评估法对样品中9,10-蒽醌膳食暴露进行评估,结果显示：广西地区居民每周平均膳食暴露量为0.683 0 ng/(kg Bw);鉴于有机污染物9,10-蒽醌（2B组）存在对人体健康产生危害的风险,建议...     

深圳市市售动物源性食品中氯霉素残留量暴露评估

目的 调查研究深圳市市售动物源性食品中氯霉素残留状况及暴露风险,为引导消费和开展安全监管提供借鉴和参考。方法 随机采集2018—2019年深圳市市售畜肉、禽肉、水产品共计511份,使用超高效液相色谱-串联质谱法测定样品中氯霉素的含量,采用点评估法计算深圳市居民通过食用动物源性食品的氯霉素暴露量,并采用暴露边界比(MOE)法对其健康风险进行评估。结果 160份畜肉和60份禽肉中未检出氯霉素,291份水产品(包括贝类、虾、淡水鱼)中氯霉素检出率为26.80%(78/291),其中贝类样品中氯霉素含量为0.05～205.00μg/kg,平均值为13.71μg/kg,检出率为37.21%(64/172);虾样品中氯霉素含量为0.05～2.20μg/kg,平均值为0.20μg/kg,检出率为13.64%(3/22);淡水鱼样品中氯霉素含量为0.05～1.90μg/kg,平均值为0.11μg/kg,检出率为11.34%(11/97),所有样品中氯霉素总检出率为15.26%(78/511)。膳食暴露风险评估结果表明,深圳市居民膳食动物源性食品摄入氯霉素的平均日暴露量为2.06×10^-3     

HPLC-MS/MS法同时测定牛肉中80种兽药及其代谢物

为全面排查宁夏地区牛肉兽药残留风险,从农业农村部规定的禁停用药物、 GB 31650—2019《食品安全国家标准 食品中兽药最大残留限量》中规定有最大残留限量的药物以及宁夏养殖环节大量使用药物三方面筛选确定12类药物,利用简单、快捷的前处理方法和超高效液相色谱-串联质谱多反应监测分析技术,建立了一次进样可同时分析检测12类80种兽药及其代谢物残留的快速检测方法。样品采用Oasis PRiME HLB固相萃取柱净化,经Waters HSS T3色谱柱分离,多反应监测模式监测,基质匹配外标法定量。结果表明:80种兽药及其代谢物在基质匹配标准溶液1.0～50.0μg/L的质量浓度范围内呈现良好的线性关系,相关系数均大于0.990,方法定量限在2.0~5.0μg/kg,方法在2.0～100.0μg/kg的平均回收率为60%～103%,相对标准偏差(n=5)均小于20%;应用该检测方法对40份市售牛肉进行检测,其中4份牛肉检出兽药残留,分别为土霉素(54.5μg/kg)、磺胺间甲氧嘧啶(23.3μg/kg和35.4μg/kg)及恩诺沙星(118μg/kg),再分别使用GB/T 21317—2007、GB/T 20759—2006、GB/T 21312—2007方法对阳性样品进行复检,结果一致。经验证表明:该检测方法定性定量结果准确可靠、灵敏度高、重现性好,可满足对牛肉中兽药残留检测分析的要求。     

浙江省5大类食物中赭曲霉毒素A暴露评估

目的 评价浙江省居民膳食赭曲霉毒素A(OTA)暴露风险。方法 收集2018—2019年浙江省居民消费食物5大类24种共518份,结合浙江省2015—2016年膳食消费量调查数据,对居民OTA膳食暴露进行评估。结果 OTA只在谷物及其制品中检出,而水果、茶叶、膨化食品、婴幼儿谷类辅食中均未检出OTA。燕麦及其制品OTA检出率最高为16.1%(5/31);OTA阳性样本含量范围为0.53～4.00μg/kg,其中燕麦及其制品检出含量最高,为4.00μg/kg;OTA含量均未超过我国限量标准（5μg/kg）。暴露评估显示,浙江省全人群中绝大多数消费情景下谷物及其制品膳食OTA暴露量为0.004～7.360 ng/kg BW,在OTA的安全摄入范围内（14 ng/kg BW）;少数高污染高消费情景下,稻谷OTA摄入量为19.627 ng/kg BW,是安全摄入量的140.19%。不同年龄组人群以1～6岁组每日摄入量最高,为0.014～34.644 ng/kg BW,是安全摄入量的0.10%～247.46%。本研究中稻谷是浙江省居民膳食OTA的主要贡献食物,不同消费人群贡献率达到87.22%～9...     

深圳市面粉与面制品中偶氮甲酰胺及其转化产物膳食暴露评估

目的了解深圳市居民面粉与面制品中偶氮甲酰胺及其分解转化产物联二脲、氨基脲的含量水平,获得深圳市致癌致畸物氨基脲的居民膳食暴露水平。方法 2016年在深圳市超市、批发市场、农贸市场等共采集500份面粉及面制品,监测偶氮甲酰胺及其分解转化产物联二脲、氨基脲的含量。并结合深圳市居民膳食调查食物消费量计算深圳市居民面粉和面制品中氨基脲的暴露量。结果所采集的500份样品中:偶氮甲酰胺、联二脲、氨基脲的检出率分别为4.60%、25.8%、18.6%,含量范围为0.500～93.4 mg/kg、10.0～13900μg/kg、0.250～1100μg/kg;氨基脲的一般水平暴露量与高水平暴露量分别为0.005μg/kg-bw/d与0.248μg/kg-bw/d。结论面粉及面制品中的氨基脲暴露已超过水产品中的暴露,应慎重使用偶氮甲酰胺作为食品添加剂在面粉及面制品中使用,同时加强对面粉及面制品中氨基脲的监测。     

济南市居民膳食中汞暴露评估

目的了解济南市居民主要食品中总汞污染现状,评估汞暴露风险。方法对2010—2012年济南市谷类、蔬菜类、菌藻类、畜肉类、禽肉类(鸡肝)、乳类、蛋类和水产品及其制品中的总汞含量进行监测;以2002年山东省居民营养与健康状况调查和JECFA 2010年制定的汞的暂定每周耐受摄入量(PTWI)4μg/kg BW为参数,应用点评估法计算济南市居民膳食中汞暴露水平,并进行风险特征描述。结果共监测8类175份样品,总汞平均含量为19.01μg/kg,P50为9.00μg/kg,总检出率为97.14%(170/175),总超标率为8.57%(15/175)。8类食品均检出汞,水产品的检出率最低,为89.36%(42/47),鸡肝的总汞平均含量最高,达83.60μg/kg。济南市居民7类(除菌藻类)主要膳食中总汞每周平均暴露量为1.31μg/kg BW,占PTWI的32.75%。总汞贡献率较高的食品为谷类、蔬菜类及畜肉类,贡献率分别为28.24%、22.90%和22.14%,3类食品对居民膳食中汞的总贡献率为73.28%。结论济南市居民主要膳食中汞暴露水平在安全限值以内,通过膳食摄入汞风险较小。     

液相色谱-串联质谱法快速检测大米中的15种农药残留

目的建立液相色谱-串联质谱法快速检测大米中15种代表性农药残留的分析方法。方法大米样品经水溶胀后以乙腈提取,利用QuEChERS法进行净化。采用0.02%甲酸+2 mmol/L甲酸铵(A)和甲醇(B)作为流动相进行梯度洗脱,采用多离子监测模式对农药多残留进行检测。结果在9.5min内完成15种目标农药残留的分离分析。在0.010、0.10和0.50mg/kg3个添加水平的回收率为70.2%～110.0%,相对标准偏差为1.3%～14.5%(n=3);方法定量限为0.010 mg/kg、检出限为0.2～1.0μg/kg。结论该方法简便、快速、准确、实用,适合测定大米样品中的农药残留。     

QuEChERS结合高效液相色谱-串联质谱法测定禽蛋中的氯霉素药物残留

目的建立QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe)结合高效液相色谱-串联质谱法(HPLC-MS/MS)测定禽蛋(鸡蛋、鸭蛋、鹌鹑蛋、鹅蛋)中的氯霉素药物残留的分析方法。方法 禽蛋样品经乙腈提取,经(PSA∶C18=1∶1)净化处理,采用高效液相色谱-串联质谱法测定,同位素内标法定量。结果 禽蛋基质中氯霉素在0.020～2.0μg/kg线性范围内,相关系数r>0.999;方法检出限0.020μg/kg,定量限0.050μg/kg;在添加浓度水平为0.020、0.10、0.50μg/kg时,回收率范围为80.8%～119.0%,相对标准偏差为4.09%～15.21%(n=6)。采用建立的方法对市购禽蛋样品和天然污染鸡蛋样品进行验证测试,方法实用性满足残留测试要求。结论 本方法前处理操作简便、灵敏度高、可有效用于禽蛋中氯霉素药物残留的监控与定量测定。     

微波消解-石墨炉原子吸收法测定食品污染物中铅镉的含量

目的探讨微波消解-石墨炉原子吸收法测定食品污染物铅镉的含量。方法采用微波消解技术,在阶梯升高温度和加热功率条件下,用硝酸和过氧化氢彻底消解样品,消解后的样品用石墨炉原子吸收分光光度法测定铅镉。结果铅浓度在0～20.0μg/L、镉浓度在0～10.0μg/L范围内呈良好的线性关系,相关系数铅r=0.9995,镉r=0.9997;最低检出限铅为5.0μg/kg,镉为0.10μg/kg;相对标准偏差铅5.4%,镉7.8%;回收率铅镉都在90.0%～105.0%之间。检测4类食品240份样品,其中大米(面粉)、猪肝(猪肾)、水产品、干食用菌铅合格率分别为86.5%、77.5%、81.5%、87.5%,镉合格率分别为82.0%、76.5%、90.0%、88.0%。结论该方法能够满足食品污染物中铅镉的分析要求。     

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