HPLC-ICP-MS法测定纺织品中五种有机锡化合物

建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用技术测定纺织品中五种有机锡的方法。采用ZORBAX C18分析柱,在流动相为V(乙腈)∶V(水)∶V(乙酸)=65∶23∶12的混合溶液中加入0.15%三乙胺作为离子对试剂,pH=3.0条件下,可以很好地分离三甲基氯化锡(TMT)、二苯基氯化锡(DPT)、二丁基氯化锡(DBT)、三丁基氯化锡(TBT)、三苯基氯化锡(TPhT)。该方法简便、快速、灵敏度高,25μL进样量时,TMT、DPT、DBT、TBT、TPhT的检出限分别为0.15μg/L、0.47μg/L、0.72μg/L、0.58μg/L和0.28μg/L;在2μg/L和20μg/L两个加标水平下,加标回收率为87.5%～98.2%和88.4%～103.7%,方法精密度优于5.2%,可以满足测定要求。采用该方法测定棉织品、羊毛制品和涤纶制品中的五种有机锡,分析结果令人满意。     

液相色谱-原子荧光光谱联用检测海产品中不同形态锡的研究

目的建立液相色谱串联原子荧光光谱仪检测海产品中不同形态的锡的测定方法。方法选择合适的提取液和流动相乙腈(v)∶水(v)∶乙酸(v)∶三乙胺(v)=65∶23∶12∶0.005来提高三甲基锡、一丁基锡、二丁基锡和三丁基锡的提取效率和分离度。通过调整灯电流、负高压、载气和屏蔽气流量以及还原剂的浓度,优化原子荧光检测条件,使待测物的荧光强度达到最佳状态。结果 本方法的三甲基锡、一丁基锡、二丁基锡和三丁基锡在10~100μg/L范围内有良好的线性,方法的测定低限均为0.05 mg/kg;实验表明方法对不同海产品的回收率为81.5%~95.7%,相对标准偏差为1.0%~5.1%。结论 该方法简便、准确,所使用的设备价格低廉,可用于海产品中4种锡形态的测定。     

贝类水产品中有机锡和甲基汞的检测研究

目的建立贝类水产品中甲基汞、三甲基锡(TMT)、一丁基锡(MBT)、二丁基锡(DBT)、三丁基锡(TBT)和三苯基锡(TPhT)等6种有机锡和甲基汞化合物的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)的分离检测方法。方法利用Eclipse Plus C18反相色谱柱对贝类水产品中6种有机金属化合物进行分离,利用电感耦合等离子体质谱对锡和汞元素进行检测,外标法定量测定水产品中6种有机金属化合物的含量。通过优化色谱分离条件,以甲醇-0.06 mol/L乙酸铵-乙酸溶液为流动相,梯度洗脱。结果 6种有机金属化合物在30 min内得到了有效分离。6种有机金属化合物标准曲线的线性相关系数大于0.998,检出限为0.5~2.5μg/kg,样品加标回收率在70%~110%。结论该法操作简便,分离效果好,检出限低,适用于贝类水产品中有机锡和甲基汞的检测。     

固相萃取-高效液相色谱-荧光检测法测定水产品中4种丁香酚类化合物

目的建立固相萃取-高效液相色谱荧光法测定水产品中4种丁香酚类化合物(丁香酚、异丁香酚、甲基丁香酚、甲基异丁香酚)残留的方法。方法样品用乙腈提取,中性氧化铝和C18固相萃取柱净化,Inertsil ODS-SP C18柱(4.6 mm×250 mm,5μm)分离,以甲醇-乙腈(1∶1,V/V)和1%冰乙酸水溶液为流动相,荧光检测激发波长为280 nm,发射波长为320 nm,外标法定量。结果 4种丁香酚类化合物在各自范围内线性关系良好,相关系数均0.999,方法检出限为3.0~6.0μg/kg,方法定量限为10.0~20.0μg/kg,平均加标回收率为74.7%~103.0%,相对标准偏差(RSD)为2.6%~8.1%。结论本方法操作简便、灵敏度高、实用性强,适用于水产品中丁香酚、异丁香酚、甲基丁香酚、甲基异丁香酚的残留分析检测。     

气相色谱-质谱法测定塑料食品包装材料中4种有机锡

建立了气相色谱-质谱法测定塑料食品包装材料中4种有机锡(二甲基锡、三甲基锡、二乙基锡和一丁基锡)的分析方法。塑料食品包装材料样品经四氢呋喃溶解,甲醇沉淀杂质大分子后高速离心过滤,有机锡与四乙基硼酸钠反应生成有机锡的乙基衍生物,经正己烷萃取后,采用气相色谱-质谱法进行定性定量分析。在试验选定的最佳条件下,4种有机锡的线性范围在0.10~10mg/L之间,相关系数均大于为0.999,方法检出限为0.2~0.3 mg/kg之间,样品加标回收率为56.5%~109.4%,相对标准偏差小于12.6%。     

基于分子印迹富集及HPLC-ICP-MS检测海产品中三丁基锡的研究

本文以甲基丙烯酸为功能单体,三丁基锡为模板分子,二甲基丙烯酸乙二醇酯为交联剂,乙腈为致孔剂,采用分子印迹技术并联合高效液相色谱电感耦合等离子质谱(HPLC-ICP-MS)成功地制备了能特异性识别TBT的MIPs。所合成的MIPS经过选择识别、吸附动力学及再生性能等检测,对三丁基锡具有良好的吸附能力和高选择识别能力。并以分子印迹聚合物作为固相萃取吸附剂分离富集TBT,联合高效液相色谱-电感耦合等离子质谱(HPLC-ICP-MS)检测海水及海产品中的三丁基锡。结果表明,用传统分子印迹聚合物作为吸附剂富集分离,在海水、贻贝和大黄鱼样品中检测限(LOD)分别为0.06μg/L、4.0 ng/g和5.0 ng/g,加标回收率分别是61.5%~84.5%、76.2%~93.9%和74.2%~93.3%,线性范围分别是0.1μg/L~30μg/L、5 ng/g~50 ng/g和5 ng/g~500 ng/g。为海产品中有机锡等有机金属的检测提供方法。     

HPLC法定量分析微生物法制备液中产物γ-氨基丁酸和底物L-谷氨酸

建立一种测定微生物法制备液中γ-氨基丁酸(γ-aminobutyric acid,GABA)和L-谷氨酸(L-glutamic,L-Glu)的高效液相色谱法。样品经10%三氯乙酸溶液预处理后,用4 mmol/L氯甲酰芴甲酯进行柱前衍生。采用Phenomenex C18色谱柱(4.6 mm×250 mm,5μm),以A[50 mmol/L乙酸钠溶液(p H 4.8)-甲醇-乙腈-四氢呋喃(82∶8.5∶8.5∶1,V/V)]∶B[50 mmol/L乙酸钠溶液(p H 4.8)-甲醇-乙腈-四氢呋喃(22∶38.5∶38.5∶1,V/V)]=30∶70为流动相,流速1.0 m L/min,柱温40℃洗脱,检测波长265 nm。该方法稳定、灵敏、测定周期短、重复性好。在GABA和L-Glu质量浓度为20~400μg/m L范围内有良好的线性关系。与常用衍生剂邻苯二甲醛相比,衍生产物的稳定性更好,且无需梯度洗脱。     

固相萃取-高效液相色谱-串联质谱法测定酱油中4-甲基咪唑

建立固相萃取-高效液相色谱-串联质谱/质谱法(SPE-HPLC-MS/MS)测定酱油中4-甲基咪唑的分析方法。试样经水稀释提取,LC-SCX固相萃取柱净化后,以乙腈和5mmol/L乙酸铵溶液(含0.1%甲酸,V/V)作为流动相,C18色谱柱分离,采用电喷雾离子源,正离子扫描多反应监测(MRM)模式进行检测。4-甲基咪唑在5~500μg/L浓度范围内呈良好线性关系,相关系数(r2)大于0.99,加标回收率为83.6%~95.1%,相对标准偏差为7.3%~8.2%,方法检出限为5μg/kg,定量限为10μg/kg。方法简单快速、准确灵敏,适用于酱油中4-甲基咪唑的测定。     

液液萃取-气相色谱法测定黄酒中β-苯乙醇含量

建立黄酒中β-苯乙醇的液-液萃取-气相色谱检测方法,为炮制辅料黄酒的质量控制研究提供参考。用碳酸钠饱和的15%乙醇溶液与乙酸乙酯1︰1 (V/V)混合均匀,超声分层,取上层澄清液作为萃取剂;采用气相色谱法,Agilent HP-5色谱柱(30 m×0.32 mm×0.25μm), FID检测器,进样口温度230℃,检测器温度250℃,柱温程序升温为:初始温度120℃,恒温2 min,以25℃/min升温至210℃,恒温10 min,柱流量1 mL/min,进样量1.0μL,内标物4-(4-甲氧苯基)-2-丁酮。结果表明,β-苯乙醇在4.86～243.02 mg/L范围内线性关系良好(r=0.999 9),精密度试验RSD值为0.20%,重复性试验RSD值为4.66%, 3种加标浓度的回收率在94.28%～102.57%之间,检出限为0.08 mg/L,定量限为0.20mg/L。该方法具有简单、可靠、结果准确等优点,同时有效降低黄酒中糖分、色素等基质对气相色谱系统的污染,减少水分对毛细管色谱柱的危害,可用于辅料黄酒中β-苯乙醇含量检测及质量控制。     

液相色谱-原子荧光光谱联用检测海产品中 不同形态锡的研究

目的: 建立液相色谱串联原子荧光光谱仪检测海产品中不同形态的锡的测定方法。方法: 选择合适的提取液和流动相V (乙腈) ：V ( 水 ) ：V ( 乙酸)：V ( 三乙胺 ) = 65：23：12：0.005来提高三甲基锡、一丁基锡、二丁基锡和三丁基锡的提取效率和分离度; 通过调整灯电流、负高压、载气和屏蔽气流量以及还原剂的浓度, 优化原子荧光检测条件, 使待测物的荧光强度达到最佳状态。结果: 本方法的三甲基锡、一丁基锡、二丁基锡和三丁基锡在10.0~ 100 μg/L 范围内有良好的线性, 方法的测定低限均为0.05 mg /kg; 实验表明方法对不同海产品的回收率在81.5% ~ 95.7%之间, 相对标准偏差在1.0% ~ 5.1%之间。结论: 该方法简便、准确, 所使用的设备价格低廉, 可用于海产品中4种锡形态的测定。     

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