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。     

UPLC-MS/MS法测定乳制品中的氯霉素类药物

建立超高效液相色谱-串联质谱(UPLC-MS/MS)法测定乳与乳制品中氯霉素、甲砜霉素和氟苯尼考的检测方法。样品经乙腈及乙酸乙酯提取、正己烷脱脂、C18柱净化后,通过超高效液相色谱-质谱联用仪进行检测,内标法定量。各标准溶液在0.1～10μg/L范围内呈线性相关(r=0.999),不同基质样品中添加回收率为75%～114%,检出限为0.1μg/kg。结果表明,该方法是一种准确测定乳与乳制品中氯霉素、甲砜霉素和氟苯尼考的检测方法。     

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。     

Captiva EMR-Lipid固相萃取结合高效液相色谱-串联质谱法同时测定猪肉中氯霉素类药物残留量

目的 建立Captiva EMR-Lipid固相萃取结合高效液相色谱-串联质谱法同时测定猪肉中氯霉素、甲砜霉素和氟苯尼考残留量的分析方法。方法 采用乙腈提取样品, 经Captiva EMR-Lipid固相萃取柱净化, 以甲醇-水为流动相, CNW Athena C18-WP色谱柱(100 mm×2.1 mm, 3 μm)进行分离, 采用电喷雾负离子扫描和多反应监测模式, 内标法定量。结果 氯霉素、甲砜霉素和氟苯尼考在0.5~20.0 ng/mL范围内呈现良好的线性关系(r＞0.9975), 方法的检出限为0.10~0.14 ?g/kg, 定量限为0.25~0.47 ?g/kg, 平均回收率为97.50%~117.00%, 相对标准偏差为5.55%~8.93%。结论 该方法简单快速、稳定可靠, 适用于猪肉中氯霉素、甲砜霉素和氟苯尼考的同时测定。     

高效液相色谱-串联质谱法快速测定动物源食品中的氯霉素残留量

目的建立高效液相色谱-串联质谱联用法快速测定动物源食品中氯霉素残留量的分析方法。方法样品采用乙酸乙酯提取、空气吹干浓缩、正己烷脱脂后,经乙腈和水梯度洗脱、色谱柱Poroshell120EC-C_(18)(50 mm×2.1 mm, 2.7μm)分离、液相色谱-串联质谱仪测定,以氘代氯霉素为内标物进行定量。结果回归方程Y=0.177X+0.0008,相关系数r为0.9996;方法检出限和定量限分别为0.03μg/kg、0.1μg/kg;在0.1～1.0μg/kg浓度梯度范围内的平均回收率为91.4%～107.5%,相对标准偏差为4.5%～5.7%,2次能力验证结果满意。结论该方法经济、简便、快捷、稳定、准确性高,能满足大批量动物源性食品样品中氯霉素残留量测定的要求。     

高效液相色谱-串联质谱法测定牛奶和奶粉中9种青霉素类药物残留量

建立一种检测牛奶和奶粉中9种青霉素类药物残留量的高效液相色谱-串联质谱方法。样品经乙腈-水提取,经HLB固相萃取柱净化,用高效液相色谱串联质谱检测,外标法定量。本方法的检出限,牛奶中氨苄西林、奈夫西林为1μg/kg,阿莫西林、哌拉西林、青霉素G、青霉素V、氯唑西林为2μg/kg,苯唑西林、双氯西林为4μg/kg;奶粉中氨苄西林、奈夫西林为8μg/kg,阿莫西林、哌拉西林、青霉素G、青霉素V、氯唑西林为16μg/kg,苯唑西林、双氯西林为32μg/kg。9种青霉素在1.0～50ng/mL范围呈良好线性,线性相关系数大于0.9888。牛奶的平均回收率为77.58%～97.77%,测定结果的相对标准偏差为4.24%～16.59%(n=10);奶粉的平均回收率在85.95%～96.78%之间,相对标准偏差为2.71%～13.41%(n=10)。该方法具有简便、快速、准确度高、检出限低的优点,适用于牛奶和奶粉中青霉素类抗生素的测定。     

QuEChERS结合高效液相色谱-串联质谱法测定禽蛋中的氯霉素药物残留

目的建立QuEChERS(Quick、Easy、Cheap、Effective、Rugged、Safe)结合高效液相色谱-串联质谱法(HPLC-MS/MS)测定禽蛋(鸡蛋、鸭蛋、鹌鹑蛋、鹅蛋)中的氯霉素药物残留的分析方法。方法 禽蛋样品经乙腈提取,经(PSA∶C18=1∶1)净化处理,采用高效液相色谱-串联质谱法测定,同位素内标法定量。结果 禽蛋基质中氯霉素在0.020～2.0μg/kg线性范围内,相关系数r>0.999;方法检出限0.020μg/kg,定量限0.050μg/kg;在添加浓度水平为0.020、0.10、0.50μg/kg时,回收率范围为80.8%～119.0%,相对标准偏差为4.09%～15.21%(n=6)。采用建立的方法对市购禽蛋样品和天然污染鸡蛋样品进行验证测试,方法实用性满足残留测试要求。结论 本方法前处理操作简便、灵敏度高、可有效用于禽蛋中氯霉素药物残留的监控与定量测定。     

超高效液相色谱串联质谱法测定液态奶中氯霉素、甲砜霉素和氟苯尼考含量

建立超高效液相色谱串联质谱法测定液态奶中氯霉素、甲砜霉素和氟苯尼考的检测方法。样品经乙酸乙酯提取,Oasis MCX小柱净化,用色谱柱WATERS ACQUITY UPLC BEH C18(1.7um, 2.1mm*100mm)分离,同位素内标法定量。在优化条件下,该方法中氯霉素的最低检出限为0.05μg /kg,定量限为0.15μg /kg, 甲砜霉素和氟苯尼考的最低检出限为0.1μg /kg,定量限为0.3μg /kg, 平均回收率为80.4~105.4%,相对标准偏差为2.8~8.4%。该方法灵敏度高、回收率好,具有良好的净化效果,提升检测效率,适用于液态奶中氯霉素、甲砜霉素和氟苯尼考的同时检测。     

超高效液相色谱-串联质谱法测定食用猪油中氯酚类物质

目的应用超高效液相色谱-串联质谱技术,建立同时测定食用猪油中2,4,5-三氯苯酚、2,4,5-三氯苯氧乙酸和五氯酚3种物质的方法。方法样品用80%乙腈提取,固相萃取(SPE)和正己烷净化萃取后,以Atlantis?T3(2.1 mm×150 mm,3μm)为分析柱,乙腈-5.0 mmol/L乙酸铵溶液为流动相,以电喷雾离子源在负离子多反应监测模式下进行测定,基质匹配外标法定量。结果 2,4,5-三氯苯酚、2,4,5-三氯苯氧乙酸和五氯酚在2.0～100.0μg/L范围内线性关系良好,相关系数(r)均大于0.999,方法检出限分别为0.09、1.59、0.90μg/kg,定量限分别为0.29、5.28、3.00μg/kg,回收率为71.9%～109.5%,相对标准偏差为0.2%～9.2%(n=6)。结论该方法简便、准确、灵敏度高,适用于食用猪油中2,4,5-三氯苯酚、2,4,5-三氯苯氧乙酸、五氯酚3种物质的高通量检测。     

QuEChERS-UPLC-MS/MS法测定动物源性食品中五氯酚及其钠盐

本文建立QuEChERS-UPLC-MS/MS测定动物源性食品中五氯酚及其钠盐残留量的分析方法。样品用酸化乙腈提取,QuEChERS方法净化。用甲醇和5 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱,C18色谱柱分离。在超高效液相色谱-串联质谱电喷雾电离动态多反应监测负离子模式下定量分析。五氯酚在0.5～15.0 ng/mL线性范围内的相关系数为0.999 96,方法检测限为0.1μg/kg。当不同基质中的标准添加量为1.0～4.0μg/kg时,平均回收率为74.7%～101.4%。本方法操作简单、快速高效,对相关检验检测工作提供参考。     

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