QuEChERS-超高效液相色谱-串联质谱法快速检测果蔬中35种甲氧基丙烯酸酯类和三唑类杀菌剂的残留量

目的 建立一种测定水果蔬菜中甲氧基丙烯酸酯类和三唑类35种杀菌剂残留量的超高压液相色谱-串联质谱检测方法。方法 样品用乙腈提取和QuEChERS方法净化, 采用C18柱子以0.2%甲酸溶液-乙腈作为流动相进行梯度洗脱, 质谱(ESI+)电喷雾正离子模式电离,采用多离子检测模式(MRM)对35种杀菌剂的定量离子和定性离子进行监测。结果 本方法中35种杀菌剂在1.0~50 μg/L的浓度范围内线性关系良好, 相关系数r2为 0.9990~0.9998;在0.005、0.050、0.100 mg/kg添加水平的回收率为61.8%~123%, 方法定量限为1.0~1.5 μg/kg。 结论 该方法快速、环境友好、准确、灵敏, 适合水果蔬菜甲氧基丙烯酸酯类和三唑类杀菌剂残留的检测。     

液相色谱-串联质谱法检测奶制品中9种 β-受体阻断剂药物残留量

目的 建立同时检测奶制品(牛奶、奶粉、奶酪)中9 种β-受体阻断剂(β-blockers, BBS)残留的液相色谱-串联质谱方法。方法 混合均匀的试样经β-葡糖醛苷酶/芳基硫酸酯酶水解, 乙腈提取, 硅藻土与BondElut分散固相萃取填料双重快速净化后, 利用液相色谱-串联质谱法进行定性定量分析。结果 9 种BBs在0.1~20.0 μg/L线性范围内线性关系良好(r≥0.995); 定量限(limit of quantity, LOQ, S/N≥10), 均达到0.5 μg/kg; 3 个添加水平(0.5、1.0和5.0 μg/kg)下的回收率为89.5%~112.5%; 相对标准偏差(relative standard deviation, RSD)为4.2%~11.5%。结论 该方法快速、准确、灵敏, 可用于奶制品样品中多种BBs残留的同时有效测定。     

分子印迹固相萃取-超高效液相色谱-串联质谱法测定牛奶中11种氨基糖苷类抗生素

目的：建立分子印迹固相萃取-超高效液相色谱-串联质谱（UPLC-MS/MS,Ultra Performance Liquid Chromatography Tandem Mass Spectrometry）检测牛奶中11种氨基糖苷类抗生素（巴龙霉素、妥布霉素、庆大霉素、卡那霉素、阿米卡星、安普霉素、链霉素、双氢链霉素、新霉素、壮观霉素、潮霉素B）残留的测定方法。方法：样品经5%三氯乙酸-乙腈提取,氨基糖苷类分子印迹聚合物（MIP）固相萃取柱净化,SiELC Obelisc R色谱柱分离,采用超高效液相色谱-串联质谱仪进行测定。结果：方法检出限为1.0~5.0 μg/kg,定量限为2.0~10.0 μg/kg。11种氨基糖苷类药物在1.0~500 μg/kg范围内关系良好（r2>0.9911）,牛奶中加标回收率为70.7%~115.6%,相对标准偏差（RSD,relative standard deviation, n=6）为1.1%~9.8%。结论：本方法准确度、灵敏度高,可用于牛奶中11种氨基糖苷类抗生素的同时检测。     

高效液相色谱法和高效液相色谱-串联质谱法测定水产品中的四环素类残留量

目的 建立高效液相色谱法定量测定水产品中四环素类残留量,同时采用高效液相色谱-串联质谱法进行定性确证和定量检测。方法 具体优化了缓冲提取液浓度、固相萃取柱类型、色谱条件选择等测定环节。样品经柠檬酸缓冲液提取,固相萃取柱净化后,以液相色谱-紫外检测器进行定量检测,同时也可通过高效液相色谱-串联质谱仪进行定性和定量。结果 在10~200 ng/mL范围内线性良好(r>0.999),四环素类目标物在10、50、100 μg/kg 3个水平上进行加标回收试验,回收率为76.0%~94.5%,相对标准偏差为3.9%~7.4%,高效液相色谱法检出限为5 μg/kg,液相色谱-串联质谱法检出限为1 μg/kg。结论 该方法简便、稳定、准确,适合测定水产品中的四环素类残留量。     

液相色谱-串联质谱法检测动物源性食品中 7种抗病毒类药物残留

目的建立动物源性食品中7种抗病毒类药物残留的液相色谱-串联质谱测定方法。方法动物源性食品中的抗病毒类药物经甲醇-1%三氯乙酸(1:1,V:V)提取,通过固相萃取柱净化、浓缩后,在正离子模式下用液相色谱-串联质谱法检测。结果 7种抗病毒类药物检测限为0.3~1.5μg/kg,定量限为1.0~5.0μg/kg。在0.1~100μg/kg浓度范围内线性关系良好,相关系数r0.99。在1.0、5.0、10.0μg/kg三个浓度添加水平下,该方法的平均回收率为87.2%~121.4%,相对标准偏差为0.6%~8.4%(n=6)。结论本方法专属性强、准确性好、灵敏度高,适用于动物源性食品中抗病毒类药物残留的检测。     

高效液相色谱-串联质谱法测定水产品中甲氧苄啶的残留

建立水产品中甲氧苄啶药物残留量测定的高效液相色谱-串联质谱方法。样品选择乙腈提取,用正己烷脱脂,固相萃取柱净化,采用LC-MS/MS选择反应监测(SRM)正离子模式测定进行定性、定量分析。结果表明:甲氧苄啶药物的检出限(LOD)为0.5μg/kg,定量限(LOQ)为1.0μg/kg,检测结果的相对标准偏差为1.78%~5.08%,加标回收率达到77.1%~93.5%。该方法具有比较高的重现性和选择性,在水产品中甲氧苄啶的残留测定中具有很好的应用前景。     

超高效液相色谱-串联质谱法测定猪肝中14种喹诺酮类药物残留

目的建立猪肝中14种喹诺酮类抗生素残留的提取、净化和超高效液相色谱串联质谱测定的方法。方法样品采用EDTA缓冲溶液提取、经正己烷除脂、固相萃取柱净化后,利用超高效液相色谱串联质谱法检测。结果本方法显著地除去了动物内脏中的磷脂类杂质的干扰,待测物均获得了良好的信号响应。方法回收率为72.7%~116.8%、相对标准偏差(relative standard deviation,RSD)为1.6%~19.5%、定量限均为1.0μg/kg。结论本方法前处理简单、重复性好、定量限低,适合作为猪肝中喹诺酮类抗生素残留的日常检测方法。     

液相色谱串联质谱法测定茶叶中氯虫苯甲酰胺残留量

目的 建立液相色谱-串联质谱法检测茶叶中氯虫苯甲酰胺残留量的方法。方法 样品采用乙腈振荡超声提取, HLB固相萃取柱净化, 液相色谱串联质谱检测, 外标法定量。结果 方法的线性范围为0.50~ 20.00 ng/mL, 相关系数r2大于0.999; 检出限为 0.05 μg/kg, 定量限为0.17 μg/kg。在不同基质中, 氯虫苯甲酰胺在0.20、0.40、2.00 μg/kg添加水平下的平均回收率为79.25%~88.42%, 相对偏差为1.50%~7.10%。结论 该方法具有快速简便、灵敏度高、准确性强等特点, 适用于茶叶中氯虫苯甲酰胺残留量的检测。     

EMR固相萃取-超高效液相色谱-串联质谱法测定虾肉中性激素残留的方法建立

本研究建立EMR固相萃取结合超高效液相色谱-串联质谱测定虾肉中15种性激素残留的分析方法。样品采用0.1 mol/L乙二胺四乙酸二钠溶液-乙腈溶液提取,经Captiva EMR固相萃取SPE小柱净化,CAPCELLPAK C₁₈ BB-H（3 μm,2.1 mm×150 mm）色谱柱分离,电喷雾离子源正负离子分开扫描;多反应监测模式的超高效液相色谱-串联质联质谱法进行检测,以空白基质匹配外标法定量。正离子流动相为甲醇和0.1%甲酸,检测雄激素与孕激素;负离子流动相为乙腈和0.01%氨水溶液,检测雌激素。结果表明,经EMR固相萃取净化的虾肉样品中的15种性激素残留在1～50 μg/kg浓度范围内线性关系良好,相关系数（r）均大于0.99,方法检出限为0.0015～0.436 μg/kg,定量限为0.0051～1.453 μg/kg,平均回收率在85.31%~119.84%,相对标准偏差为2.11%~9.86%（n=6）。本方法操作快速简单,重复性好,灵敏度较高,适用于虾肉中15种性激素残留的检测。     

QuEChERS结合高效液相色谱-串联质谱法测定大白菜中10种喹诺酮类药物残留

摘 要: 目的 建立QuEChERS结合高效液相色谱-串联质谱法测定大白菜中10种喹诺酮类药物残留的检测方法。方法 大白菜样品经提取,采用QuEChERS净化方法,以诺氟沙星-D5为内标,用高效液相色谱-串联质谱法测定,采用正离子电喷雾,多反应监测模式（multiple reactions monitoring, MRM),内标法定量分析10种喹诺酮类药物残留的含量。结果 10种喹诺酮类在5~100 ng/mL的浓度范围内线性良好,检出限为0.1~0.3 μg/kg,定量限为0.3~1.0 μg/kg,平均回收率为76.0%~107%,相对标准偏差为1.5%~8.1%。 结论 本研究建立的QuEChERS结合高效液相色谱-串联质谱法测定大白菜中10种喹诺酮类药物残留的检测方法准确、可靠, 适用于大白菜中喹诺酮类药物残留的检测。     

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