高效液相色谱-质谱法测定酒中甜蜜素含量的研究

目的 本文采用UPLC-MS/MS法对市售30种酒中甜蜜素进行测定.方法 采用Acquity UPLCTM BEHC18(2.1 mm×100 mm,1.7 μm)色谱柱分离,甲醇-0.1％乙酸(90+ 10)作为流动相洗脱,运用三重四极杆质量分析器定性定量分析.结果 该方法测定酒中甜蜜素具有良好的线性关系,测定方法检出限为0.010 μg/ml,定量限为0.021 μg/ml,加标回收率为75.0％～ 105％,精密度RSD值为10.5％～ 12.1％.30种酒样品中,有13个样品检测出甜蜜素,含量水平为0.027 ～891μg/ml.结论 该方法测定酒中甜蜜素,具有较高的灵敏度和选择性,样品测定结果表明存在乱用甜蜜素现象.     

气相色谱-串联质谱法测定酒中氨基甲酸乙酯的含量

建立利用气相色谱-串联质谱仪测定酒中氨基甲酸乙酯的方法.样品经二氯甲烷提取后,采用DB-225MS毛细管柱分离样品,以GC/MS/MS测定氨基甲酸乙酯的含量,结果表明,该方法线性范围为10～1000 μg/L,方法检出限为1.0 μg/L,标准加入5～250 μg/L的平均回收率为78.00％～81.20％.本方法具有操作简便、快速、准确等优点,可用于酒中氨基甲酸乙酯的检测.     

离子色谱法直接测定食品添加剂中的甜蜜素

建立离子色谱法直接测定食品添加剂中的甜蜜素的方法。利用甜蜜素具有较大水溶性、在水中易电离的特性,采用去离子水振荡提取样品中的甜蜜素,30mmol/L氢氧化钾溶液作为淋洗液,经阴离子交换色谱柱分离,电导检测器-离子色谱法直接测定甜蜜素。结果表明：甜蜜素含量在5～200μg/mL范围内,方法的线性关系良好(相关系数为0.9999),加标回收率为95.54%～99.24%,检出限为0.087μg/mL,方法的日内相对标准偏差小于3%,日间相对标准偏差小于2%。方法简便、稳定性好,不需对样品进行复杂的预处理,可实现对食品添加剂中甜蜜素的便捷、快速、准确测定。     

超高压液相色谱-质谱法测定水果中添加的3种人工合成甜味剂

目的 建立水果中3 种人工合成甜味剂(甜蜜素、糖精钠、安赛蜜)的超高压液相色谱-串联质谱 (UPLC-MS/MS)检测方法。方法 以反相C18 柱为色谱柱, 乙腈?0.02 mol/L 乙酸铵溶液为流动相, 样品经纯水 提取后用色谱柱进行分离, 串联质谱负离子多反应监测(MRM)模式测定。结果 3 种人工合成甜味剂在10~600 μg/L 范围内响应峰面积和样品质量浓度之间有良好的线性关系(相关系数r≥0.995); 甜蜜素、糖精钠和安赛蜜 的最低检出限分别为0.8、5.0、1.0 μg/kg; 在2 种添加水平下, 样品平均回收率为74.9%~111.2%, 相对标准偏 差<8%。结论 该方法前处理简单, 分析时间短, 具有良好的灵敏度和准确性, 可用于水果中甜蜜素、糖精钠、 安赛蜜的同时检测。     

高效液相色谱-串联质谱法同时测定糖果中24种添加剂含量

建立了糖果中24种添加剂的高效液相色谱-串联质谱检测方法。样品经50%乙腈超声提取后,取上清液过聚四氟乙烯滤膜,滤液直接上机分析,在电喷雾电离模式下采用多反应监测模式进行测定。结果显示,24种添加剂在0.01～1.0 μg/mL线性良好,线性相关系数大于0.995,方法检出限为2～124 μg/kg,空白样品加标平均回收率为81.29%～106.33%,相对标准偏差为0.92%～9.11%。将该方法应用于市售糖果的检测,发现部分样品中胭脂红、甜蜜素、羟苯甲酯超出我国限量要求。该方法简单、快速,可用于糖果中添加剂的快速筛查。     

高效液相色谱法测定白酒中甜蜜素

采用高效液相色谱法测定白酒中甜蜜素含量.检测条件:色谱柱ODSHypersil,流动相:甲醇:水=80∶20,流速1.0 mL/min,检测波长314 nm.结果表明,线性范围10～200 μg/mL,回收率93.15%～106.67%,相对标准偏差1.2%～2.8%,定性检测下限1.0 μg/mL,定量检测下限2.0μg/mL.该法简便,适合白酒中甜蜜素含量的测定.     

高效液相色谱法测定酒中甜蜜素

采用高效液相色谱法测定酒中甜蜜素含量。色谱柱ODSHypersil(5μm,125mm×4mm),流动相CH3OH:H2O=80:20,流速1.0mL,检测波长314nm。结果表明:线性范围4μg/mL~100μg/mL,回收率80.6%~102.7%,RSD10.8%~2.5%,定性检测下限为1.2μg/mL,定量检测下限4.0μg/mL。此方法简便可靠,适用于酒中甜蜜素含量的测定。     

UPLC-MS/MS法同时测定不同动物源性食品中硝基呋喃代谢物残留

采用超高效液相色谱串联质谱法(UPLC-MS/MS),建立了猪肉、猪肝、螃蟹和虾4种不同动物源性食品中同时测定4种硝基呋喃类药物代谢物的检测方法,优化了样品前处理的条件以及UPLC-MS/MS仪器条件,样品经盐酸水解,2-硝基苯甲醛衍生,乙酸乙酯提取,ESI正离子模式扫描,多反应监测(MRM)测定。结果表明:采用本方法在4种动物源性样品基质中4种代谢物浓度在1~100 ng/mL范围内线性关系良好;4种代谢物的平均回收率为84.6%~118.1%;相对标准偏差RSD为2.9%~8.1%;在4种样品基质中,3-氨基-2-唑烷基酮(AOZ)的检出限为0.1 μg/kg,定量限为0.4 μg/kg,氨基脲(SEM)和5-甲基吗啉-3-氨基-2-唑烷基酮(AMOZ)的检出限为0.2 μg/kg,定量限为0.5 μg/kg,1-氨基乙内酰脲(AHD)的检出限为0.5 μg/kg,定量限为1.0 μg/kg,均满足国家标准要求。采用本方法对市场上随机购买的80份动物源性样品和鸡肉中硝基呋喃代谢物质控样进行检测,结果与国家标准方法GB/T 20752-2006测定结果相近,质控样的检测结果在量值范围内。该方法前处理操作简便,较传统方法节省时间和成本,可为硝基呋喃类药物残留检测技术提供理论支撑和参考。     

顶空固相微萃取-气相色谱-质谱法分析啤酒的酒花香组分

采用顶空固相微萃取-GC/MS技术,建立了啤酒中酒花香组分的分析方法。啤酒样品采用PA萃取头,在40℃萃取30 min后直接进行GC/MS分析,鉴定了含量在μg/L量级的里哪醇、β-香茅醇、α-萜品醇、香叶醇、反式-橙花叔醇、乙酸香茅酯、香叶酸甲酯、乙酸香叶酯等8种酒花香组分,随后又以选择离子监测模式(SIM)并以萜品烯-4-酵为内标,实现了定量测定。样品重复测定的相对标准偏差为1.6%～14.9%,回收率为70.4%～128.6%。应用该方法测定了市售的7种啤酒中上述酒花香组分的含量。     

麻辣熟食中甜蜜素的GC检测和质谱确证

建立了气相色谱分析及液相色谱-串联质谱确证方法对麻辣熟食中甜蜜素的检测方法,比较了气相色谱法(GC)与液相色谱-串联质谱法(LC-MS/MS)检测方法的适用性。提取方法采用超声波提取,经石油醚萃取除油除脂,沉淀剂去蛋白质和脂肪,由气相色谱法初筛、高效液相色谱-串联质谱法做阳性样品确证检测麻辣熟食中甜蜜素的方法。GC法中甜蜜素含量在0.010 0~0.300 0 mg/mL的范围内与峰面积有良好的线性关系,相关系数为0.999 55,检出限为0.005 2 g/kg。甜蜜素添加浓度在0.020 0,0.040 0和0.200 g/kg时,添加回收率分别在90.0%~98.0%之间,测定结果的相对标准偏差为3.1%~5.2%(n=6);液质联用作为甜蜜素的确证方法,检测低限为2.2μg/kg。结果表明:建立的甜蜜素检测和确证方法简便、经济、快速、准确,适用于麻辣熟食中甜蜜素测定。     

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