多壁碳纳米管/N-丙基乙二胺混合吸附-超高效液相色谱-串联质谱法测定普洱茶中3种手性杀菌剂农药残留

目的建立基于手性柱/超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定普洱茶生茶和熟茶中3种手性农药(三唑酮、苯霜灵、丙环唑)对映体的分析方法。方法样品采用乙腈提取,氨基化多壁碳纳米管(aminated multi-walled carbon nanotubes,MWCNTs-NH2)和N-丙基乙二胺(primary secondary amine,PSA)混合吸附剂净化,经手性色谱柱Chiralpak-IG拆分,超高效液相-串联质谱法检测,基质外标法定量。结果 3种农药外消旋体在0.005～1.0 mg/L范围内均呈良好线性关系,定量限(limits of quantification,LOQ)为0.005～0.01 mg/kg。在3种手性农药单个对映体含量为0.1、0.01、0.0025 mg/kg加标水平下平均回收率为70.1%～110.6%,相对标准偏差(relative standard deviation,RSD)(n=6)为1.2%～13.5%。结论该方法准确、简单、灵敏,可以满足普洱茶中3种手性农药对映体残留的检测要求。     

多壁碳纳米管净化-超高效液相色谱-串联质谱法测定鸡蛋中44种药物残留

建立超高效液相色谱-串联质谱(HPLC-MS/MS)法同时测定鸡蛋中44种药物的残留量。样品加入乙腈沉淀蛋白后,再经多壁碳纳米管、十八烷基键合硅胶、乙二胺-N-丙基硅烷组合技术净化后,以0.1%甲酸溶液-0.1%甲酸甲醇为流动相进行梯度洗脱分离,以电喷雾离子源在正、负离子多反应监测模式下进行测定,用基质匹配标准曲线外标法定量。结果表明,44种药物在0.1~200 ng/mL范围内线性良好,R2为0.9909~0.9999,方法检出限0.007~0.3571 μg/kg,定量限为0.005~1.190 μg/kg,样品回收率在77.9%~114.5%,相对标准偏差小于10%(n=6)。该方法操作简便,灵敏度高,适用于鸡蛋中药物残留的高通量筛查。     

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。     

多壁碳纳米管净化-液相色谱串联质谱法测定瓜菜中双酰胺类杀虫剂

目的建立多壁碳纳米管净化,超高效液相色谱串联质谱技术同时测定瓜菜中3种双酰胺类杀虫剂残留的分析方法。方法瓜菜样品用乙腈提取后,经多壁碳纳米管净化,超高效液相色谱-电喷雾电离串联质谱法测定。结果3种双酰胺类杀虫剂在0.005～0.1 mg/L范围内线性良好,相关系数均大于0.99,定量限均为5μg/kg,平均加标回收率在71.7%～99.1%之间,相对标准偏差在0.6%～3.5%之间。与N-丙基乙二胺和石墨化炭黑吸附剂相比,多壁碳纳米管具有更好的净化性能。结论该方法具有简单灵敏、定量准确等优点,可用于瓜菜中3种双酰胺类杀虫剂残留的检测。     

超高效液相色谱–串联质谱法测定特殊医学用途配方食品中胆碱含量

目的 建立超高液相色谱–串联质谱法(ultra high performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定配方食品中胆碱的分析方法, 为胆碱及其制剂的含量测定提供参考。方法 样品中的胆碱经过盐酸水解, 提取后, 以0.1%甲酸-甲醇作为流动相经kinetex 5u XB-C18柱(4.6 mm×100 mm, 5 μm)梯度洗脱分离, 流速0.45 mL/min, 采用UPLC-MS/MS在正离子模式下检测, 外标法定量。结果 在优化实验条件下, 测得胆碱在浓度为0.1~0.5 μg/mL有良好线性关系, 线性相关系数为0.9993。方法的回收率为96.1%~103.4%, 检出限为2.27 mg/100 g。结论 超高效高效液相色谱–串联质谱法简单快速、灵敏度高、准确性强, 适用于特殊医学用途配方食品中胆碱的分析。     

超高效液相色谱-串联质谱法测定干辣椒中2种新型杀虫剂残留量

目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定干辣椒中氰氟虫腙和氯虫苯甲酰胺残留量的分析方法。方法 干辣椒样品经乙腈匀浆提取, 氨基固相萃取小柱净化, 甲醇/水(50:50, V:V)定容, 以反相C18色谱柱(100 mm×2.1 mm, 1.7 μm)分离, 0.1%甲酸-水和甲醇作为流动相进行梯度洗脱, 多反应监测模式下进行超高效液相色谱-串联质谱测定、基质匹配标准溶液外标法定量。结果 2种新型杀虫剂在5~500 μg /L范围内线性关系良好, 相关系数均大于0.999, 定量限为0.008~0.01 mg /kg; 在高、中、低3个加标水平下的回收率为80.4%~94.9%, 相对标准偏差在0.9%~8.7%之间。结论 方法简单、快速、灵敏高、准确可靠, 可操作性强, 适合测定干辣椒中氰氟虫腙和氯虫苯甲酰胺残留量。     

超高效液相色谱-串联质谱法测定食品中呋虫胺及2种代谢物残留量

目的 建立了一种超高效液相色谱-串联质谱法(UPLC-MS/MS)快速检测食品中呋虫胺及两种代谢物残留的分析方法。方法 样品经乙腈超声提取,C18固相萃取(SPE)小柱净化,上清液氮吹至近干,经初始比例液相流动相复溶后,过膜,UPLC-MS/MS测定,外标法定量。结果 本方法在在0.1 μg/L～200 μg/L范围内线性相关系数R_²≥0.999,粮谷、水果、蔬菜、鱼、肉、蛋、奶等22种基质中呋虫胺及其两种代谢物在5 μg/kg 、10 μg/kg 和50 μg/kg 3个加标水平下,回收率范围71.2 %～105.6 %,RSD的范围在1.3 %～9.8 %。结论 该分析方法准确度和精密度均达到农药残留检测要求,适用于分析粮谷、水果、蔬菜、鱼、肉、蛋、奶中呋虫胺及代谢物残留量。     

UPLC-MS/MS测定稻谷、大豆、芥菜、金桔中氟唑菌酰胺残留量

试验旨在建立超高效液相色谱-电喷雾串联四极杆质谱(UPLC-MS/MS)测定稻谷、大豆、芥菜和金桔中氟唑菌酰胺残留量的分析方法.以乙腈作为提取溶剂,经乙二胺-N-丙基硅烷(PSA)和十八烷基键合硅胶吸附剂(C18)净化,以0.1％甲酸的3 mmol/L甲酸铵溶液和乙腈作为流动相梯度洗脱,在电喷雾离子源ESI负离子模式下...     

双环磺草酮在稻田环境中的残留分析

目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定稻田环境中双环磺草酮的残留量分析方法。方法样品经0.02mol/L盐酸浸泡后,用乙腈提取,提取液经石墨化碳黑粉净化,采用乙腈和0.1%甲酸作为流动相洗脱,质谱(ESI+)采用多离子检测模式(MRM)对双环磺草酮的定量离子和定性离子进行监测。结果在0.002~10mg/L浓度范围内目标物线性良好,相关系数大于0.9999。双环磺草酮在不同水平的添加回收试验中,方法的平均回收率为78.5%~100%,相对标准偏差为0.8%~6.5%,双环磺草酮的最低检测浓度为0.002mg/kg。结论该方法灵敏度、准确度、精密度符合农药残留分析的要求。     

超高效液相色谱-串联质谱法测定苹果中的赤霉素、脱落酸、甲萘威、多效唑和烯效唑残的残留量

建立用超高效液相色谱-串联质谱法(UPLC-MS/MS)测定苹果中赤霉素、脱落酸、甲萘威、多效唑和烯效唑残留量的方法.用甲醇-水溶液提取样品中的植物生长调节剂,经固相萃取柱净化,用UPLC-MS/MS分析,采用多反应监测模式,外标法定量.采用BEH Shield RP18色谱柱,以乙酸铵和乙腈为流动相,进行梯度洗脱.结论:操作简单快捷,方法准确度和稳定性好.     

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