固相萃取净化-高效液相色谱串联质谱法测定鱼肉制品中链霉素、双氢链霉素、卡那霉素的含量

本文建立了一种简单、快速测定鱼肉制品中链霉素、双氢链霉素、卡那霉素的固相萃取净化-液相色谱串联质谱的分析方法。样品经庚烷磺酸钠和磷酸盐缓冲溶液提取,C18固相萃取柱净化后,在ACQUITYUPLC BEH HILIC C18色谱柱上以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱分离,采用HPLC-MS/MS选择反应监测(SRM)模式测定进行定性、定量分析,质谱采集模式为电喷雾正离子监测模式。结果表明:在5.0~100μg/kg范围内,峰面积与浓度线性良好,相关系数均大于0.9992;方法的检出限(LOD)为2.5μg/kg,定量限(LOQ)为5.0μg/kg,检测结果的相对标准偏差为1.16%~7.35%(n=6),平均加标回收率达到77.4%~107.3%。该方法具有较高的重现性和选择性,适用于鱼肉制品中链霉素、双氢链霉素、卡那霉素的残留分析检测。     

亲水作用色谱-串联质谱法测定动物源食品中10种氨基糖苷类药物的残留量

通过不同键合相亲水作用色谱柱的分离效果比较和分离条件优化,建立动物源性食品中10种氨基糖苷类药物残留量检测的亲水作用色谱-串联质谱法。样品经磷酸缓冲液提取,三氯乙酸沉淀蛋白质,C18固相萃取柱净化,Sielc Obelisc R色谱柱分离,在电喷雾正离子模式下用串联质谱检测。结果表明,丁胺卡那霉素、潮霉素B,链霉素、双氢链霉素、卡那霉素、庆大霉素、妥布霉素的定量检出限为20μg/kg,新霉素、奇霉素和安普霉素的定量检出限为100μg/kg,在猪肉、牛肉、猪肾、牛肝中的添加回收率为73.9%～103.6%,RSD为3.3%～14.8%,可以满足动物源食品中氨基糖苷类药物的检测需求。     

高效液相色谱串联质谱法同时测定9种龙虾中氨基糖苷类和四环素类抗生素残留

建立了龙虾中6种氨基糖苷类和3种四环素类抗生素残留的高效液相色谱串联质谱(HPLC-MS/MS)同时检测方法。样品中抗生素采用5%三氯乙酸-磷酸盐溶液提取,经超声萃取、固相萃取柱净化,C_(18)色谱柱分离,对样品前处理条件、液相色谱分离条件和质谱检测条件进行了优化。通过实际样品添加回收率实验,链霉素、双氢链霉素、四环素、金霉素和土霉素定量检出限均为5μg/kg,庆大霉素、卡那霉素、新霉素和妥布霉素定量检出限均为50μg/kg,9种抗生素三个添加水平下,龙虾样品加标回收率在66.1%~107.9%,相对标准偏差在0.7%~9.7%。结果表明,该方法准确、高效,适用于龙虾中6种氨基糖苷类和3种四环素类药物残留的同时检测和确证。     

液相色谱-串联质谱法检测蜂蛹粉中链霉素及双氢链霉素的残留量

目的建立全自动固相萃取-液相色谱-串联质谱法测定蜂蛹粉中链霉素及双氢链霉素含量的分析方法。方法样品经磷酸缓冲溶液提取,高氯酸沉淀蛋白后,采用watersHLB固相萃取小柱净化,以Protemix WCX色谱柱进行色谱分离,多反应监测模式测定,外标法定量。结果结果表明2种化合物在10～200μg/kg的浓度范围内线性关系良好,检出限为5μg/kg,定量限为10μg/kg。空白蜂蛹粉样品的3水平加标回收率为80.6%～93.5%,相对标准偏差为4.7%～8.8%。结论该方法适用于蜂蛹粉中链霉素和双氢链霉素残留的检测。     

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。     

弱阳离子固相萃取净化-高效液相色谱-串联质谱法检测奶酪中链霉素和双氢链霉素残留

目的 建立奶酪中链霉素和双氢链霉素高效液相色谱-串联质谱分析方法。方法 样品经20 mmol/L Na₂HPO₄(使用6 mol/L HCl调节pH到7.4)超声提取，WCX混合型弱阳离子交换柱净化，液相分离，串联四极杆质谱仪使用电喷雾电离，多反应监测正离子模式。结果 在1～200 ng/mL浓度范围，线性相关系数(r)大于0.996；加标回收率范围82.2%～116.2%，相对标准偏差范围2.67%～7.6%。链霉素和双氢链霉素方法检出限、定量限为5、20μg/kg。结论 本方法简便快速、灵敏度较高，适用于奶酪中链霉素及双氢链霉素的检测。     

加速溶剂萃取-亲水作用色谱-串联质谱法检测马铃薯中α-茄碱

目的 研究马铃薯中α-茄碱的液相色谱-串联质谱检测方法。方法 样品经酸性水溶液与有机溶剂的混合溶液加速溶剂萃取,中等极性阳离子交换固相萃取小柱净化,氮气吹扫至干,以含0.1%甲酸的乙腈-水(80∶20,V/V)溶液溶解,稀释10倍,过滤后以亲水作用的液相色谱柱(2.1 mm×50 mm,1.6 μm)进行分离,多反应离子监测定性和定量分析。对前处理和液相分离条件、质谱检测基质效应进行考察。结果 此方法检出限为0.5 μg/kg,定量限为1.6 μg/kg,标准曲线的线性范围为0.1～100 μg/L,相对标准偏差为3.41%～7.56%(n=6),样品加标回收率范围为82.8%～99.0%。结论 本方法提取简便、效率高,检测灵敏且定性准确,能够满足风险监测需求和中毒分析要求。     

茶叶中10种农药残留的液相色谱-串联质谱法和气相色谱-串联质谱法测定

建立了茶叶中啶虫脒、乐果、吡虫啉、灭多威、甲基嘧啶磷、腐霉利共6种农药残留的液相色谱-串联质谱(LC-MS/MS)测定方法和溴氰菊酯、乐果、高效氯氟氰菊酯、p,p'-滴滴伊、甲基嘧啶磷、腐霉利、哒螨灵共7种农药残留的气相色谱-串联质谱(GC-MS/MS)测定方法。其中,乐果、甲基嘧啶磷和腐霉利三种农药均能通过两种方法测定。LC-MS/MS法测定的6种农药,在5~200 μg/L范围内线性关系良好(R2>0.995),在10、50、100 μg/kg加标水平下的回收率为70.0%~105.0%,相对标准偏差为0.3%~18.7%。GC-MS/MS法测定的7种农药,在10~500 μg/L范围内线性关系良好(R2>0.996),在10、50、300 μg/kg加标水平下的回收率为82.0%~110.0%,相对标准偏差为1.8%~12.0%。该方法完善了茶叶中10种农药残留检测方法针对实际样品的检测,灵敏度满足国外限量标准要求,适合出口茶叶中农药残留的测定。     

基质固相分散-亲水交互作用色谱-串联质谱法测定牛奶中5种氨基糖苷类抗生素残留量

目的 研究亲水交互作用色谱-串联质谱测定牛奶中5种氨基糖苷类抗生素的方法。方法 样品经含二氧化硅和乙二胺四乙酸二钠混合材料进行基质固相分散提取后,用含0.1%甲酸的超纯水洗脱,亲水交互作用色谱-串联质谱分析,对样品前处理的模式和条件、色谱分析的固定相和流动相进行优化。结果 三个浓度的样品加标试验结果显示,回收率为65.7%～96.5%,相对标准偏差为4.3%～8.6%(n=6),定量限和检出限分别为8.0～80和2.5～25 μg/kg。结论 建立的分析方法简便、准确、灵敏,满足牛奶中5种氨基糖苷类抗生素残留检测要求。     

高压液相色谱-线性离子阱串联质谱法测定红葡萄酒中多菌灵和甲基硫菌灵

目的 建立红葡萄酒中多菌灵和甲基硫菌灵残留的高压液相色谱-串联线性离子阱质谱(HPLC-LIT-MS/MS)检测方法。方法 样品经过乙腈提取, 在梯度洗脱程序下经CAPCELL PAK CR 1:20色谱柱分离后, 采用HPLC-LIT-MS/MS, 在二级质谱选择反应监测(SRM)模式进行测定。结果 红葡萄酒中多菌灵和甲基硫菌灵添加水平为10、20、50 μg/L时, 平均回收率分别为82.5%~103.1%和93.7%~115.2%。检出限(LODs)分别为0.063 μg/L和0.019 μg/L, 定量限(LOQs)分别为0.125 μg/L和0.075 μg/L。结论 该方法快速简便, 灵敏度高, 准确度和精密度均满足痕量分析要求。     

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.     

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