气相色谱-质谱联用法测定加热卷烟烟草材料中8种凉味剂

为分析加热卷烟用烟草材料中凉味剂的种类及含量(质量分数),通过样品前处理及色谱条件优化,建立了一种基于气相色谱-质谱联用技术测定8种凉味剂的方法,并采用该方法分析了加热卷烟薄片、烟草粉末和烟丝中凉味剂的含量。结果表明:①该方法标准工作曲线在1.0～1 000.0μg/mL之间线性良好,相关系数均大于等于0.999 6,检出限和定量限分别为0.25～0.54和0.83～1.80μg/g,日内精密度和日间精密度分别为0.29%～2.60%和0.93%～3.35%,低、中、高3个水平下加标回收率分别为85.66%～109.36%、96.08%～105.47%和94.29%～104.12%,相对标准偏差(RSD)≤3.35%。②加热卷烟薄片、烟草粉末和烟丝中凉味剂的含量分别为0.65～29.40、0.15～6.23和0.01～3.94 mg/g(n=3),RSD为0.31%～2.14%。该方法简单、快速,灵敏度和准确度高,稳定性和重复性好,适用于同时检测不同加热卷烟烟草材料中的8种凉味剂。     

鸡蛋中三聚氰胺含量HPLC检测方法研究

利用HPLC对不同区域鸡蛋中三聚氰胺的含量进行分析,探索建立HPLC法快速测定鸡蛋中三聚氰胺含量的方法。样品通过饱和醋酸铅沉淀蛋白,三氯乙酸提取,Oasis-MCX混合型阳离子交换柱净化后,使用Agilent-C18柱(4.6mm×300mm,5μm),流动相为乙腈+0.05mol/L磷酸二氢钾(pH值为3.0)=25:75(体积比),检测波长240nm,流速为1.2mL/min,柱温35℃,进样量为20μL,三聚氰胺浓度在1～20μg/mL时,浓度与峰面积呈线性关系,最低检出浓度为0.24μg/mL,定量限为0.8μg/mL,加标回收率为93.50～106.22%,相对标准偏差为2.77%～7.78。%     

反相液相色谱法测定发酵虫草菌粉腺苷含量

通过样品处理及检测条件的优化,建立发酵虫草菌粉腺苷含量的RP-HPLC检测方法.结果表明:Agilent-C18柱(4.6mm×300mm,5μm),乙腈+甲醇+水=5+5+90(体积比)作为流动相,检测波长260nm,流速为1.2mL/min,柱温35℃,进样量为20μL,腺苷浓度在10μg/mL～50μg/mL时,浓度与峰面积呈线性关系,最低检出浓度为1.2μg/mL,定量限为4.0μg/mL,加标回收率为95.30％～105.20％,相对标准偏差为2.32％～5.70％.     

高效液相色谱-荧光检测法测定保健食品中维生素K2的含量

目的建立高效液相色谱-荧光检测法快速检测保健食品中维生素K_2(四烯甲萘醌)的分析方法。方法样品使用GIST C_(18)色谱柱(250 mm×4.6 mm,5μm)分离,柱后经锌粉还原柱(4.6 mm×50 mm,50～70μm)衍生,以甲醇(含有四氢呋喃10%、冰醋酸0.03%、氯化锌1.5 g/L、无水乙酸钠0.5 g/L)为流动相,流速为1.0 mL/min,进入荧光检测器进行检测。结果四烯甲萘醌保留时间约为10 min,在浓度0.1099～2.197μg/mL范围内线性关系良好,相关系数r~2=0.9999。重复性实验RSD为0.794%,3个浓度级别的加标回收率在97.1%～101.9%之间。当取样量为1.5 g,总定容体积为500mL时,四烯甲萘醌的检出限为71μg/100 g,定量限为236μg/100 g。结论该方法准确性高、重现性好、操作简单,可用于保健食品中维生素K_2的含量测定。     

猪肉中氯丙嗪残留UPLC-MS/MS检测法的优化研究

本文在《猪肾和肌肉组织中氯丙嗪残留量的测定》(GB/T 20763-2006)的基础上优化了样品的提取净化方式,增加了定性离子,建立了操作便捷、准确度高、重现性好的猪肉中氯丙嗪残留量液质检测的新方法。具体操作为,样品在碱性条件下经特丁基甲醚提取,冷冻离心除脂后取上清液,经液相色谱质谱联用仪分析检测。结果表明,优化后的方法在0.5～20ng/mL范围内线性关系良好,相关系数r=0.9997;在0.5～5μg/kg范围内,3个浓度的加标回收率均在75%～95%之间,测定结果均满足国标方法中的重复性要求(含量范围:0.750～4.800μg/kg、r=0.4736m-0.1775)。     

在线凝胶渗透色谱-气相色谱-串联质谱法测定食用植物油中11种有机磷阻燃剂

建立在线凝胶渗透色谱–气相色谱-串联质谱法(GPC-GCMS/MS)测定食用植物油中11种有机磷阻燃剂的分析方法。0.5 g食用油样品用(3∶7)丙酮/环己烷溶液稀释定容5 mL,GPC-GCMS/MS采用多反应监测模式(MRM)测定,外标法定量。11种有机磷阻燃剂在1～50μg/L范围内,线性关系良好,相关系数r>0.997 0,方法检出限为1.0～3.0μg/kg,定量限为3.0～9.0μg/kg。空白样品中添加3个水平质量浓度,回收率在65.6%～129.0%之间,相对标准偏差RSD为0.2%～13.9%。该方法样品前处理简单,仪器自动化程度高,重复性较好,适用于食用植物油中有机磷阻燃剂的检测。     

SPE-GC/MS法同时检测地表水中6种常见农药残留物

建立了全自动固相萃取-气质联用法检测地表水中的百菌清、马拉硫磷、联苯菊酯、甲基内吸磷、莠去津、对硫磷6种常见农药残留物的方法。采用HLB固相萃取柱用于水样的富集和净化;地表水样品以6 mL/min的流速上样,然后用5 mL乙腈和10 mL二氯甲烷依次洗脱;洗脱液氮气吹至近干,用1 mL丙酮溶解残渣,过滤;采用气质联用仪对样品进行定性定量检测。6种农药残留物质量浓度在0.03～3.0μg/mL范围内线性关系良好,线性相关系数≥0.995;加标回收率均在81.2%～108.3%之间;检出限如下:百菌清0.008μg/mL,马拉硫磷0.008μg/mL,联苯菊酯0.005μg/mL,甲基内吸磷0.010μg/mL,莠去津0.010μg/mL,对硫磷0.008μg/mL。检测精密度(n=6)的RSD范围为1.47%～4.87%,方法重复性(n=6)相对标准偏差(RSD)在3.10%～4.97%之间。试验表明,该方法自动化程度较高,灵敏度好,准确度高,适用于地表水中多种农药残留物的同时检测。     

气相色谱法测定脱臭馏出物中角鲨烯的含量

建立了气相色谱法测定植物油脱臭馏出物中角鲨烯含量的方法。样品用内标液稀释,采用HP-5毛细管色谱柱,内标法定量。结果表明,角鲨烯质量浓度在10~400μg/m L范围内,方法的线性关系良好,相关系数为0.9998,最低检测限为2.0μg/m L;在10、15及20g/kg的加标水平下,角鲨烯的平均回收率为99.2%~102.8%,相对标准偏差(RSD)为1.5%~2.6%。并以此方法检测了6组不同植物油脱臭馏出物样品,其角鲨烯含量在1.75%~26.10%之间。该方法分析时间短,重现性好,灵敏度高,定量准确,样品不需要特殊处理,具有较强的实用价值,适用于植物油脱臭馏出物中角鲨烯含量的测定。     

微生物阻抗法快速测定乳粉中的叶酸含量

为建立一种基于微生物阻抗法快速测定乳粉中叶酸含量的新方法,在GB 5009.211—2022第一法的基础上制作标准系列管,优化测定条件,探索菌体的阻抗变化与叶酸含量之间的线性关系,建立微生物阻抗法标准曲线。以乳粉质控样品和市售乳粉为试验样品,考察此方法的检测性能。结果表明：当标准系列管培养20 h,采用离心+超声破碎处理时,测定菌体的电阻率值与叶酸含量在0.000～0.100 ng/mL之间的线性关系最好。拟合出标准曲线方程为Y=8866.3X+177.38,相关性系数R2=0.9952。检出限为1.26μg/100 g,定量限为4.20μg/100 g,加标回收率为96.2%～103.6%。对乳粉质控样品和4种市售乳粉的相对标准偏差(Relative standard deviation, RSD)值在3.4%～6.4%之间,总检测时间为3 d左右。与国家标准方法相比,该方法的重复性、准确度相当,但检测时间更短,可快速测定乳粉中的叶酸含量。     

pCEC法检测运动营养品中吡咯并喹啉醌的含量

建立一种快速、高效的加压毛细管电色谱法检测运动营养品中吡咯并喹啉醌含量的分析方法。样品经20%的乙腈溶液提取后,以乙腈-15mmol/L pH4.7磷酸钾缓冲液（15∶85,v/v）作为流动相,260nm检测波长下检测,在电压强度+2kV条件下,外标法峰面积定量。结果表明,吡咯并喹啉醌标准溶液在0.05μg/mL～2.00μg/mL浓度范围内线性良好,相关系数R2为0.9995,检出限为0.5μg/kg,定量限为1.5μg/kg,加标回收率达到86.4%～98.2%,相对标准偏差（RSD）为2.17%～4.35%。该方法具有前处理简单、检测速度快的优点,适用于运动营养品中吡咯并喹啉醌含量的测定。     

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