高效液相色谱-串联质谱法测定动物源食品中氯霉素残留

目的建立高效液相色谱-串联质谱法测定几种动物源食品中氯霉素残留的方法。方法对《动物源食品中氯霉素残留量的测定高效液相色谱-串联质谱法》(农业部第781号公告)中的测定方法进行优化,样品经提取后经HLB固相萃取小柱净化,采用甲醇-水进行梯度洗脱,经Agilent Eclipse-plus C₁₈色谱柱(3.0 mm×100 mm,1.8μm)分离,采用多反应检测负离子模式进行定性及定量分析。结果在0.5~10.0 ng/mL范围内,氯霉素的浓度和色谱峰面积线性关系良好(r=0.9998),方法检出限为0.03μg/kg,定量限为0.1μg/kg,在1.0、2.0和5.0 ng/mL 3个水平的加标回收率为91.58%~109.52%,相对标准偏差小于7.5%。结论该方法快速、准确、灵敏,能满足几种动物源食品中氯霉素残留的测定。     

动物源性食品中常山酮残留量的液相色谱检测法及液相色谱-串联质谱确证法

建立了动物源性食品中常山酮残留量的液相色谱检测(High Performance Liquid Chromatography, HPLC)法及液相色谱-串联质谱(High Performance Liquid Chromatography-tandem Mass Spectrometry, HPLC-MS/MS)确证法。动物源性食品中的常山酮,用胰蛋白酶酶解,乙酸乙酯提取,固相萃取柱净化,液相色谱法测定,对于牛组织样品和疑似常山酮阳性的鸡组织样品,采用液相色谱-串联质谱法进行确证。液相色谱法:在50～1 000ng/mL线性范围内,常山酮的回归方程呈良好的线性关系,R~20.999,鸡组织样品在添加水平为50μg/kg和100μg/kg时,回收率为82.50%～96.46%,相对标准偏差(relative standard deviation,RSD)为2.71%～5.44%,方法检出限为25μg/kg,定量限为50μg/kg;液相色谱-串联质谱法:在0.5～50ng/mL线性范围内,常山酮的回归方程呈良好的线性关系,R~20.998,动物源性食品样品在添加水平为0.5μg/kg和5μg/kg时,回收率为70.20%～93.60%,RSD为6.50%～9.48%,方法检出限为0.25μg/kg,定量限为0.5μg/kg。该方法简便、快捷,灵敏度、准确度和精密度均较高,检出限低,解决了残留限量要求较低的牛组织样品中常山酮的检测问题,适用于动物源性食品中常山酮残留量的检测和确证。     

动物源性食品中氟苯尼考残留水平和 分布情况分析

目的分析动物源性食品中氟苯尼考残留水平和分布规律。方法采用超高效液相色谱-串联质谱法进行残留量测定,并借助Excel2010和社会科学统计软件包18.0对测定结果进行分析。结果方法中,以乙腈-水为最佳流动相,以Welch Xtimate C_(18)为最佳色谱柱。不同品种样品中,氟苯尼考平均回收率为80.3%～95.3%,检出限为0.052～0.095μg/kg,定量限为0.150～0.313μg/kg。472批次样品中,氟苯尼考检出率为15.9%,残留量主要为0.1～1.0μg/kg,检出品种以各鲜肉、胗、大肠以及相应的腊制品和蛋类为主。新复极差分析显示,检出品种中鸡蛋残留量不同于其他品种。结论本研究对氟苯尼考残留水平和分布规律进行了分析,可为市民选择提供参考。     

增强型除脂固相萃取技术结合超高效液相色谱- 串联质谱法测定动物源性食品中五氯酚残留量

目的建立增强型除脂固相萃取技术结合超高效液相色谱-串联质谱法测定动物源性食品中五氯酚残留量的分析方法。方法样品经8%三乙胺乙腈:水(80:20,V:V)提取,经EMR-Lipid固相萃取柱净化,以5 mmol/L乙酸铵溶液(含0.1%甲酸)-甲醇作为流动相, Waters ACQUITY BEH C_(18)(50 mm×2.1 mm, 1.7μm)进行色谱分离,在电喷雾负离子模式下,多反应监测(multiple reaction monitoring,MRM)方式进行测定,基质匹配外标法定量。结果猪肉、猪肝、鱼、河虾、蟹、牛奶等6种基质中五氯酚在0.5～10 ng/mL范围内线性良好,相关系数r0.997,方法检出限范围为0.1～0.3μg/kg,定量限范围为0.3～0.5μg/kg,在1.0、5.0、10.0μg/kg3个浓度水平下6种基质中回收率范围为81%～98%,相对标准偏差范围为1.74%～4.78%之间(n=6)。结论该方法简单快速、准确可靠,经济环保,重复性好,适用于动物源性食品中五氯酚残留量的测定。     

超高效液相色谱-串联质谱法测定鸡肉、鸡蛋中氟苯尼考和氟苯尼考胺残留

目的建立超高效液相色谱-串联质谱准确测定鸡肉、鸡蛋中氟苯尼考和氟苯尼考胺残留的分析方法。方法鸡肉和鸡蛋样品加入D5-氯霉素内标,经氨化乙酸乙酯混合溶液超声离心提取,提取液减压蒸馏浓缩后,C18固相萃取柱净化处理,采用超高效液相色谱-串联质谱法对氟苯尼考和氟苯尼考胺同时进行检测。结果氟苯尼考线性范围为0.2～20μg/L,检出限为1.0μg/kg,定量限为3.0μg/kg,方法回收率为88.0%～108.0%,相对标准偏差为4.7%～6.4%;氟苯尼考胺线性范围为0.2～20μg/L,检出限为1.0μg/kg,定量限为3.0μg/kg,方法回收率为76.0%～93.1%,相对标准偏差为4.1%～7.2%。结论本方法精确、重现性好,适用于鸡肉、鸡蛋中氟苯尼考和氟苯尼考胺残留量的测定。     

QuEChERS-超高效液相色谱-大气压化学电离-串联质谱法测定多种动物源性食品中的地塞米松残留

目的建立QuEChERS-超高效液相色谱-串联质谱法测定多种动物源性食品中地塞米松残留量的分析方法。方法样品经含1%甲酸的乙腈提取, QuEChERS方法净化后,以乙腈-0.1%甲酸水溶液为流动相,经PhenomenexKinetexF5色谱柱(100mm×3.0mm,2.6μm)分离,采用大气压化学电离源(atmosphericpressure chemicalionization,APCI),正、负模式同时扫描的离子化模式,多反应监测(MRM)模式采集,外标法定量。结果地塞米松在0.5～100 ng/mL浓度范围内线性良好,相关系数(r)为0.99946,检出限为0.10μg/kg;在3个加标水平下,平均回收率为73.2%～95.9%,精密度(n=6)为4.1%～10.7%。结论该方法简单、快速、稳定性高、重现性好,可满足多种动物源性食品中地塞米松残留量的检测。     

固相萃取-同位素稀释超高效液相色谱-串联质谱法测定动物源性食品中24种β2-受体激动剂

目的建立固相萃取-同位素稀释超高效液相色谱/串联质谱法同时测定动物源性食品中24种β2-受体激动剂残留量的检测方法。方法样品经β-葡萄糖苷酸酶水解,过混合阳离子(MCX)固相萃取柱净化。采用乙腈和含有0.1%甲酸的水为流动相,梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对24种β2-受体激动剂残留量进行检测。结果该方法各组分的最低定量限为0.1~0.5μg/kg,在0.1~20.0μg/kg浓度下呈现良好的线性关系,加标回收率为72.5%~109.3%。结论该方法操作简便,准确,快速,灵敏,可同时检测24种β2-受体激动剂的残留量。     

碱水解-SPE-LC-MS/MS法快速测定动物源食品中喹乙醇代谢物残留量

建立了一种快速准确定性定量检测动物源性食品中喹乙醇代谢物3-甲基-喹喔啉-2-羧酸(MQCA)残留量的液相色谱—串联质谱(LC-MS/MS)检测方法。样品组织通过碱水解提取MQCA,阴离子固相萃取柱净化,LCMS/MS检测,内标法定量。结果显示,在0.5～50.0ng/mL浓度范围内,MQCA线性关系良好,相关系数R2为0.999 7。MQCA检出限为0.1μg/kg,方法在0.1,0.2,1.0μg/kg的添加水平下,回收率为95.6%～108.2%,相对标准偏差为3.4%～14.3%(n=6)。该检测方法准确、快速、灵敏度高,适用于动物源食品中MQCA残留量的检测和确证。     

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     

动物源性食品中氯霉素类药物残留量的测定

本文采用QuE-UPLC/MS/MS法测定猪肉、草鱼、牛奶、蜂蜜等动物源性食品中氯霉素、甲砜霉素的残留量。该方法使用乙腈作为提取溶剂,样品经搅匀、涡旋、振荡、离心、净化处理后上机分析。本方法的优点体现在样品前处理方法简易、省时,能够同时检测氯霉素和甲砜霉素两种目标组分,在节省了检测时间的同时降低了基质效应;氯霉素和甲砜霉素的回收率均可达到85%以上,确保了实验结果的准确性和重现性;氯霉素和甲砜霉素的检出限均为0.1μg/kg,优于《可食动物肌肉、肝脏和水产品中氯霉素、甲砜霉素和氟苯尼考残留量的测定液相色谱-串联质谱法》(GB/T 20756-2006)的检测方法。     

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