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。     

冻干鲤鱼粉中恩诺沙星和环丙沙星残留测定的两种前处理方法比较

采用固相萃取和液液萃取结合超高效液相色谱-串联质谱法(UPLC-MS/MS),对冻干鲤鱼粉中恩诺沙星和环丙沙星残留量进行测定,比较两种前处理方法的测定结果。固相萃取法:样品经EDTA-Mcllvaine缓冲溶液提取,HLB固相萃取柱净化,氮气浓缩;液液萃取法:样品经酸性乙腈溶液提取,正己烷液液萃取净化,旋转蒸发浓缩。两种方法的提取液浓缩定容后,以超高效液相色谱-串联质谱仪测定,外标法定量。固相萃取和液液萃取法的回收率分别为95%～112%和75%～90%,RSD分别为2.9%～7.4%和1.0%～4.6%,检出限分别为1.0μg/kg和0.1～0.2μg/kg。结果表明,两种方法简便快速、重现性好、选择性强,均适用于鱼肉和冻干鲤鱼粉中恩诺沙星和环丙沙星残留的测定。     

固相萃取-超高效液相色谱串联质谱法检测甘蔗中3-硝基丙酸的方法研究

目的建立甘蔗中3-硝基丙酸的固相萃取-超高效液相色谱串联质谱检测方法。方法样品经乙腈萃取,Sep-pak氨基固相萃取柱净化,超高效液相色谱串联质谱法测定甘蔗中3-硝基丙酸含量。色谱柱为WatersACQUITY BEH C18柱(1.7μm,50 mm×2.1 mm),柱温40℃,样品温度10℃,进样体积5μl,流动相A为水,流动相B为乙腈,梯度洗脱。结果方法的线性范围为4.0～40.0μg/kg,基质加标工作曲线线性相关系数为0.998。方法的定性检出限为1.0μg/kg,定量检出限为4.0μg/kg。高、中、低3个浓度水平的加标回收率为92.5%～93.6%,相对标准偏差小于10%。结论本方法灵敏、快速、准确,可用于甘蔗中3-硝基丙酸的测定。     

固相萃取-高效液相色谱-串联质谱法测定蜂蜜中高氯酸盐

目的建立一种固相萃取-高效液相色谱-串联质谱法测定蜂蜜中高氯酸盐的含量。方法样品用酸化甲醇水提取, WAX固相萃取柱净化,经Phenyl-hexyl色谱柱分离,以电喷雾离子源在负离子多反应监测模式下进行测定,内标法定量。结果高氯酸盐的检出限和定量限分别为0.33μg/kg和1μg/kg,高氯酸盐在1～10μg/kg的加标水平内的回收率为91.6%～108.3%,相对标准偏差为2.81%～3.47%。结论该方法准确、灵敏,适用于蜂蜜中高氯酸盐的测定。     

超高效液相色谱-串联质谱法检测蜂蜜中九种氨基糖苷类药物残留

建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定蜂蜜中9种氨基糖苷类药物(新霉素、阿米卡星、双氢链霉素、链霉素、潮霉素B、卡那霉素、庆大霉素、妥布霉素、大观霉素)残留量的方法。蜂蜜样品中的氨基糖苷类药物采用三氯乙酸的缓冲盐溶液提取,经HLB固相萃取柱富集净化,选择水性洗脱液洗脱,在最终提取液中添加离子对试剂优化色谱行为,选取乙腈-水体系作为流动相进行梯度洗脱,采用反相色谱柱进行分离,以串联质谱法正离子模式扫描,外标法定量。实验结果表明,该方法在20～1 000 ng/mL线性关系良好,新霉素、双氢链霉素、链霉素、卡那霉素、妥布霉素的定量限为5μg/kg,阿米卡星、潮霉素B、庆大霉素、大观霉素的定量限为10μg/kg,在线性范围内,分别在空白蜂蜜样品中进行3个浓度的添加实验,样品的回收率在72.6%～109.4%,相对标准偏差为2.13%～8.23%。该方法操作简单,灵敏度高,净化效果好,在流动相中避免使用离子对试剂,有效减少了对质谱仪的污染,能...     

亲水作用色谱-质谱法同时检测鱼肉中 链霉素和双氢链霉素残留

目的 建立一种亲水作用色谱串联质谱技术同时检测鱼肉中链霉素和双氢链霉素残留的分析方法。方法 以鱼肉为原料, 样品经磷酸盐缓冲溶液提取, 固相萃取柱净化后, 采用亲水作用色谱柱分离, 在正离子模式下以电喷雾电离串联质谱进行测定, 外标法定量。结果 链霉素和双氢链霉素在2.0?50 μg/L质量浓度范围内线性关系良好, 在10、20、50 μg/kg三个加标水平下, 方法的回收率为80.2%?97.1%, 相对标准偏差为3.3%?7.2%。结论 该方法简便、快速、实用、准确, 各项技术指标满足国内外法规的要求, 可用于鱼肉中链霉素和双氢链霉素残留的确证检测。     

固相萃取-气质联用法测定水产品中扑草净

建立检测水产品中扑草净残留量的固相萃取-气相色谱质谱联用法。样品用乙腈提取,浓缩后经PSA固相萃取柱净化,由气质联用仪选择离子监测模式下测定。该方法条件下扑草净在2.5μg/L~40μg/L浓度范围内线性良好,对空白样品分别添加2、10、20μg/kg扑草净标准溶液,平均回收率在80%~98%,RSD小于10%,检出限为0.5μg/kg。     

分子印迹固相萃取-气相色谱-串联质谱法测定油茶籽油中16种多环芳烃

为稳定可靠地分析油茶籽油中多环芳烃,建立了分子印迹固相萃取-气相色谱-串联质谱测定油茶籽油中16种多环芳烃方法。样品经正己烷溶解后,分别采用反相固相萃取HLB小柱、弗罗里硅土小柱和分子印迹固相萃取小柱对16种多环芳烃进行净化。以回收率和基质效应为考察指标评估3种固相萃取柱的净化,在此基础上,对净化液进行低温低速氮吹浓缩,多反应监测扫描模式下进行气相色谱-串联质谱检测,外标法定量。结果表明：分子印迹固相萃取小柱对16种多环芳烃的净化效果最佳;16种多环芳烃在质量浓度1～50μg/L范围内线性关系良好(R²≥0.995 1),检出限为0.01～0.20μg/kg,在2、10μg/kg和20μg/kg加标水平下的回收率为71.5%～116.3%,相对标准偏差为1.5%～13.8%。该方法具有灵敏度高、检出限低、重复性好等特点,适用于油茶籽油中16种多环烃的测定。     

分子印迹固相萃取-高效液相色谱法测定果汁中的展青霉素

建立了分子印迹固相萃取-高效液相色谱法测定果汁中展青霉素的方法。浓缩果汁样品经酶解,乙酸-水溶液稀释,分子印迹固相萃取小柱净化后(澄清果汁样品经乙酸-水溶液稀释后,直接进行SPE净化),以Waters XSELECT HSS T3色谱柱为分离柱,以水和乙腈作为流动相,二极管阵列检测器高效液相色谱进行检测,外标法定量。展青霉素在20～1000μg/L质量浓度范围内线性关系良好,相关系数为0.9994,方法的定量限为10.0μg/kg;添加水平为10.0、20.0μg/kg和40.0μg/kg时,加标回收率为83.0%～91.5%,相对标准偏差为2.8%～7.6%。结果表明:该方法准确、高效、特异性好、重现性高,适用于果汁中展青霉素的测定。     

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。     

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