超高效液相色谱-串联质谱法快速测定动物组织中地塞米松与倍他米松药物残留

在承担糖皮质激素风险监测任务时,发现2个现行有效的关于检测动物组织中糖皮质激素的国家标准(农业部1031号公告-2—2008《动物源性食品中糖皮质激素类药物多残留检测液相色谱-串联质谱法》和GB/T 21981—2008《动物源食品中激素多残留检测方法 液相色谱-质谱/质谱法》)中的样品前处理均采用了固相萃取方法,从而导致了检测过程中过柱净化烦琐、氮吹浓缩时间长、检测成本高、生态环境不友好等诸多弊端。在经过大量实验研究及经实际工作应用检验的基础上,研究简化了动物组织中地塞米松和倍他米松残留检测中样品前处理固相萃取过柱和氮吹过程,建立了快速、准确、灵敏的动物组织(牛肝、牛肉、猪肝与猪肉)中残留的地塞米松和倍他米松的超高效液相色谱-串联质谱的同时检测方法。样品在盐析条件下经乙腈提取,正己烷脱脂,采用电喷雾多反应监测、负离子模式测定,对动物组织中地塞米松和倍他米松进行定性和定量。地塞米松和倍他米松的检出限可达0.5μg/kg,定量限可达1.0μg/kg。在地塞米松和倍他米松的质量浓度为0.1～50.0μg/L,峰强度与质量浓度的线性关系良好(R²>0.99)。在地...     

QuEChERS-超高效液相色谱-串联质谱法测定 蜂蜜中41种糖皮质激素

目的建立超高效液相色谱-串联质谱检测蜂蜜中41种糖皮质激素的分析方法。方法样品用0.1%乙酸溶液及乙腈溶液提取后,经QuEChERS分散固相萃取剂进行净化,采用Agilent Eclipse Plus C_(18)(100 mm×2.1mm,1.8μm)分离,以0.1%乙酸水溶液及乙腈(含0.1%乙酸)为流动相进行梯度洗脱,电喷雾离子源正离子多反应监测(multiple reaction monitoring, MRM)模式串联质谱进行测定。结果在优化条件下, 41种化合物在5.0～200.0μg/kg含量范围内有良好的线性相关性。在5.0、50、200μg/kg添加水平的回收率为83.9%～111.2%,相对标准偏差(relative standard deviation, RSD, n=6)小于10%。结论该方法快速、简单、准确,适用于蜂蜜中41种糖皮质激素残留的定性、定量分析。     

液相质谱法同时检测猪肉中氯霉素和地塞米松

建立一种利用高效液相色谱-串联质谱法同时检测猪肉中氯霉素和地塞米松药物残留的方法。猪肉样品中的药物残留经乙酸乙酯提取后,经氮气吹干,残渣溶解后过Silica柱,洗脱液经氮气吹干,用初始流动相溶解定容。用Shim-pack GIST C18色谱柱(150 mm×2.1 mm,5μm)分离,以纯水-甲醇为流动相进行梯度洗脱,质谱采用多反应监测模式,氯霉素以内标法定量,地塞米松以外标法定量。在5 min内完成了两种目标化合物的分离分析。氯霉素和地塞米松在0.2μg/kg～40μg/kg范围内线性关系良好,相关系数r2分别为0.999 9和0.999 7。氯霉素添加水平在1、2.5、5μg/kg时,回收率在90.54%～101.73%之间;地塞米松添加量在0.5、2.5、5μg/kg时,回收率在83.82%～87.5%之间;批内标准偏差和批间标准偏差均小于10%(n=5),方法定量限均小于0.15μg/kg。     

QuEChERS-超高效液相色谱-串联质谱法快速测定化妆品中糖皮质激素类药物

目的建立QuEChERS-超高效液相色谱-串联质谱法快速测定化妆品中16种糖皮质激素类药物的检测方法。方法样品经1%(V/V)甲酸-乙腈提取,加入氯化钠进行盐析,提取液经C₁₈50 mg、N-丙基乙二胺(primary secondary amine,PSA)100 mg、MgSO₄150 mg净化,采用Thermo Acclaim RSLC 120 C₁₈(2.1 mm×100 mm,2.2μm)进行分离,电喷雾正离子多反应监测扫描(multiple reaction monitoring,MRM)模式下进行测定,外标法定量。结果16种糖皮质激素在线性范围1~100 ng/mL内线性良好,相关系数r²在0.991~0.999之间,方法定量限为10μg/kg,16种糖皮质激素平均回收率在76.5%~109.3%之间,相对标准偏差为0.77%~2.41%。结论该方法操作简单、净化效果好、灵敏度、准确度和精密度均符合多残留检测技术要求,解决了化妆品中糖皮质激素类药物检测提取过程过于繁琐的问题,可为化妆品检测提供更方便、更快捷的检测方法支持。     

固相萃取-高效液相色谱法测定卤菜中的蒂巴因

建立一种快速、高效测定卤菜中的蒂巴因的固相萃取-高效液相色谱方法。样品前处理采用乙腈-水溶剂提取,经固相萃取柱净化后检测。以乙腈-0.01%三乙胺水溶液(70∶30, V/V)作为流动相,用荧光检测器检测,外标法峰面积定量。结果表明,蒂巴因在0.5～50.0μg/mL质量浓度范围内线性关系良好,相关系数r2为0.999 9,检出限为0.20μg/kg,定量限为0.60μg/kg,在1.0, 10.0和50.0μg/kg三个添加水平进行加标回收试验(n=5),加标回收率达到91.5%～94.2%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点,适用于卤菜样品中蒂巴因的分离和定量检测。     

液相色谱-串联质谱法检测速冻调制肉制品中糖皮质激素类药物残留

建立液相色谱-串联质谱法检测速冻调制肉制品中糖皮质激素类药物残留的方法。样品经乙酸乙酯提取后,过Silica固相萃取柱净化,最后用乙腈定容,经液相色谱-串联质谱仪测定。样品采用外标峰面积法进行定量,该方法的最小检出限量分别为0.2、0.5、1.0μg/kg,定量限分别为0.5、1.0、2.0μg/kg,添加回收率范围为85.0%～96.4%,RSD为2.3%～6.1%。     

高效液相色谱法测定牛奶中氯羟吡啶的残留量

建立了牛奶中氯羟吡啶残留检测的高效液相色谱方法。样品经乙腈提取,碱性氧化铝固相萃取柱净化分离,收集流出液用氮吹仪吹干,浓缩液用1 m L体积分数为50%甲醇溶解,以磷酸盐缓冲液(p H=7.0)∶乙腈(85∶15)为流动相,用0.22μm微孔有机滤膜过滤上机。结果表明,氯羟吡啶在0~300μg/kg,质量分数范围内呈现良好的线性关系,相关系数R2大于0.99,定性检出限为5μg/kg,定量检出限为15μg/kg,从20,30,100,200和300μg/kg,5个水平添加质量分数检测结果可以看出,方法回收率在87.34%~93.52%,相对标准偏差3.67%~6.71%。     

UPLC-MS/MS法分析茶叶中的灭多威农药残留

建立了检测茶叶中灭多威残留的超高效液相色谱-串联质谱(UPLC-MS-MS)分析方法。茶叶样品经乙腈提取,氨基固相萃取柱净化,反相液相色谱对样品进行分离,采用多反应监测模式(MRM)进行定性、定量分析。结果表明:方法检出限为0.5μg/kg,定量限为2.0μg/kg;当添加浓度水平为10、100μg/kg时,加标回收率为71.9%～113.5%,相对标准偏差为5.3%～12.5%。该法灵敏度高、干扰小、定性准确,适用于茶叶中灭多威残留检测,同时可作为液相色谱检测的验证方法。     

分散固相萃取-超高效液相色谱串联质谱法测定 牛肉中7种头孢菌素类药物及其代谢物

目的建立分散固相萃取超高效液相色谱-串联质谱法(dispersion solid-phase extraction with ultra-performance liquid chromatography-tandem mass spectrometry,DSPE-UPLC-MS/MS)同时测定牛肉中7种头孢菌素类药物及其代谢物残留量的方法。方法样品经乙腈-水溶液提取,C_(18)分散固相萃取净化,在电喷雾正离子多反应监测模式下进行定量和定性分析。结果 7种头孢菌素类药物及其代谢物的方法检出限和定量限分别为0.4~0.8μg/kg和1.1~2.3μg/kg。在3个添加浓度水平的平均回收率为68.3%~95.7%,相对标准偏差为1.9%~12.5%。结论该方法快速、准确、灵敏、稳定,能够满足牛肉中头孢菌素类药物残留的检测。     

高效液相色谱串联质谱法测定饲料中8种利尿剂药物

本研究旨在建立一种高效液相色谱串联质谱法测定饲料中8种利尿剂的检测方法。样品经乙腈提取,HLB固相萃取小柱净化,氮吹浓缩,以10 mmol/L乙酸铵水溶液(含0.1%甲酸)和乙腈为流动相,C_(18)色谱柱梯度洗脱分离,采用电喷雾正、负离子源同时采集,多反应监测模式进行检测。结果表明,该方法8种化合物在(2.00～100) ng/ml的范围内均有良好的线性,相关系数r~20.99。添加浓度水平为(2.00～10.0)μg/kg时,平均回收率为68.7%～104.8%,相对标准偏差为2.3%～5.0%,方法检出限为(0.1～0.5)μg/kg,定量限为(0.3～1.5)μg/kg。该方法简便、快速、结果准确度高,适用于饲料中利尿剂的检测。     

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