分散固相萃取—超高效液相色谱—串联质谱法测定液态奶中11种农药残留量

目的：评估液态乳中农药残留量的安全性。方法：建立同时测定11种农药残留的超高效液相色谱—串联质谱法。待测样品经乙腈提取，C₁₈和PSA固相萃取剂净化，经色谱柱Xbridge BEH C₁₈ （100 mm×2.1 mm，1.7 μm）分离，多反应监测模式进行测定，并使用响应曲面法优化前处理参数。结果：前处理的最佳条件为乙腈用量10 mL，C₁₈用量50 mg，PSA用量30 mg。11种农药在1.0~100.0 μg/L的浓度范围内线性关系良好，相关系数（R²）均＞0.999。在10，20，100 μg/kg添加水平内，11种农药的平均回收率为82.7%~102.0%，相对标准偏差为2.89%~8.87%，检出限和定量限分别为2.0~3.0，5.0~10.0 μg/kg。结论：该方法操作简便，分析时间短，回收率高，重现性好，能够准确定性定量分析液态乳中11种农药残留量。     

超高效液相色谱-串联质谱法测定聚氯乙烯食品接触材料中3种柠檬酸酯增塑剂

目的 建立超高效液相色谱-串联质谱法测定聚氯乙烯食品接触材料中3种柠檬酸酯类增塑剂的方法。方法 采用正己烷/二氯甲烷（1∶1，V/V）提取，经硅胶固相萃取柱净化，乙腈/乙酸乙酯（1∶4，V/V）洗脱，进入UPLC-MS/MS分析，以乙腈和超纯水做流动相，经BEH C₁₈色谱柱（2.1 mm×50 mm，1.7 μm）分离，采用ESI源在MRM正离子模式下检测，外标法定量。结果 3种化合物在线性范围内决定系数R²>0.996，方法检出限0.1~0.6 μg/kg，定量限0.3~2.2 μg/kg，回收率为70.3%~103.1%，相对标准偏差为0.9%~9.8%。结论 该方法分析快速、灵敏、准确，适用于塑料材料中柠檬酸酯类增塑剂含量的检测，为新型增塑剂的添加使用监管提供方法。     

净化柱结合超高效液相色谱—串联质谱检测动物源性食品中16种喹诺酮药物

目的：加强动物源性食品安全检测市场监管。方法：动物源性食品样品使用80%乙腈（含0.2%甲酸）提取,净化柱（Speedy Prep^-Quino 1）净化后,利用超高效液相色谱—串联质谱检测16种喹诺酮类药物残留。结果：16种喹诺酮类药物的线性范围为1.6～40.0 μg/kg,相关系数r≥0.996 1,检出限为0.14～0.80 μg/kg,定量限为0.47~2.68 μg/kg。在净化柱前处理后7个基质加标回收率为62%~112%,相对标准偏差为0.9%~18.7%。结论：该方法具有检测速度快、灵敏度高的特点,适用于羊肉、鸭肉、牛肉、鱼肉、鸡蛋、猪腰、鸭皮等动物源性食品。     

气相色谱-飞行时间质谱测定鱼肉中蓝藻异味代谢物

通过优化微波蒸馏（microwave distillation,MD）及固相微萃取（solid-phase microextration,SPME）等提取富集条件,采用全二维气相色谱分离,有效实现了蓝藻中常见的8种异味代谢物的完全分离,以高分辨特征离子的精确质量数进行内标法定量分析,建立了一种鱼肉中蓝藻异味代谢物的检测方法。结果表明,8种异味代谢物在质量浓度0.01~100.00 μg/L时呈良好线性,方法的检出限为0.07~3.30 μg/kg,定量限为0.2~10.0 μg/kg,加标回收率在72.5%~103.7%,相对标准偏差（RSD）为2.26%~14.30% (n=6)。对淡水鱼肉产品进行分析检测,二甲基三硫、土臭素、β-环柠檬醛、β-紫罗兰酮、吲哚质量分数最高分别可达7.21×10²、3.18、1.85×10²、94.6、4.69×10² μg/kg。该分析方法准确、灵敏度高、稳定性好,极大降低了假阳性问题,可作为水产品中蓝藻异味筛查及确证方法。     

同位素稀释—超高效液相色谱—串联质谱法测定婴幼儿奶粉中水溶性维生素

目的：建立同时测定婴幼儿奶粉中的多种水溶性维生素的超高效液相色谱—串联质谱法。方法：样品经温水溶解后，超声提取，使用盐酸和氢氧化钠调节pH至4.6，高速离心后供UPLC-MS/MS测定。在电喷雾电离源（ESI）的正离子模式下进行电离，多反应监测（MRM）模式对目标碎片离子进行采集。结果：10种水溶性维生素的内标曲线在2.0～500.0 μg/L的质量浓度范围内线性良好，相关系数R²大于0.998 7，加标回收试验的回收率为85.7%～102.0%，相对标准偏差（RSD）为1.11%～5.69%。方法检出限（LOD）为10～50 μg/kg，方法定量限（LOQ）为30～150 μg/kg。结论：该方法操作简单、耗时短、回收率好、灵敏度高、结果稳定，可应用于婴幼儿奶粉中水溶性维生素含量的测定。     

基于1H-qNMR的水溶性镧系位移试剂识别法测定功能性食品中谷氨酰胺对映体

目的 建立基于¹H-qNMR的水溶性镧系位移试剂识别法，实现对功能性食品中谷氨酰胺（Gln）对映体各自含量的快速定性、定量分析。方法 样品经超纯水溶解，以对苯二甲酸二钠（DT）为内标，经过涡旋、离心后，取适量上层清液于NMR管中，以氘水为锁场溶剂，水溶性镧系位移试剂钐（Ⅲ）-丙二胺四乙酸钠为手性拆分试剂，采用600 MHz核磁共振波谱仪采集¹H-NMR谱，直接对功能性食品中的Gln对映体含量进行定量分析。结果 Gln对映体和DT定量峰分离良好。左、右旋Gln的质量浓度在100.0～2 000.0 μg/mL范围内线性良好，R²>0.99，检出限为30.0 μg/mL，定量限为100.0 μg/mL。方法的平均加标回收率为94.27%~116.07%，相对标准偏差（n=6）为0.18%~1.84%。结论 该方法回收率高、重现性好，前处理过程简便，15 min内可完成测样。对商超平台购买的不同剂型功能性食品进行检测，样品中Gln对映体纯度均≥99%。在Gln总量测定方面，该方法与高效液相色谱法检测结果无显著性差异（P>0.05），能够为Gln对映体含量的快速检测提供一种实用的技术。     

固相萃取—超高效液相色谱—质谱法测定食用香精中3种甲基咪唑类物质

目的：同时、快速检测食用香精中3种甲基咪唑化合物。方法：利用5%三氯乙酸溶液提取食用香精，再利用PCX混合阳离子固相萃取柱净化提取液，最后利用超高效液相色谱—质谱法和内标法进行定性和定量分析。结果：3种甲基咪唑化合物在5.0~400.0 ng/mL内呈良好线性关系，相关系数R²≥0.997。3种甲基咪唑检出限为0.030~0.450 μg/kg，定量限(LOQ)为0.10~1.50 μg/kg。3种甲基咪唑的加标回收率在82.8%~111.7%，相对标准偏差RSD在1.3%~9.3%。结论：该方法简单高效、准确度高，可作为食用香精中甲基咪唑的定量检验方法。     

钙型糖柱—高效液相色谱—蒸发光散射检测器法测定牛乳中的乳糖

目的：实现牛乳中乳糖含量快速检测。方法：建立基于钙型糖柱和高效液相色谱测定牛乳中乳糖的新方法。牛乳通过0.2 g/mL三氯乙酸溶液沉淀蛋白质，所得滤液稀释100倍并过滤膜后进入高效液相色谱系统，经过钙型糖柱分离，蒸发光散射检测器进行检测。结果：乳糖在线性范围（20～100 mg/L）内，色谱峰面积和质量浓度之间具有较好的相关性，R²为0.999 8。乳糖加标水平为15，40，80 mg/g时，回收率为90.96%～98.23%，检出限为3.6 μg/g，定量限为12 μg/g，在6 min内实现乳糖浓度的测定。并且用该方法测定11种市售乳样品，测得结果与国标（GB 5009.8—2016）法基本一致。结论：该方法的精密度、重复性、加标回收率均符合有关规定，检测结果准确且耗时短，适用于快速检测牛乳中的乳糖含量。     

SPE-GC-FID法测定婴幼儿配方奶粉中饱和烃类矿物油

目的：建立可准确测定婴幼儿配方奶粉中饱和烃类矿物油（MOSH）的固相萃取结合气相色谱—氢火焰离子化检测器（SPE-GC-FID）分析方法。方法：以MOSH的提取量为考察指标，研究了不同提取方法（浸泡提取、振荡提取、超声辅助提取及液液萃取等）和提取溶剂（正己烷、异辛烷、苯及混合溶剂等）对婴幼儿配方奶粉中MOSH的提取效果，确定了最佳提取方法和提取溶剂。在此基础上，利用AgNO₃ SPE固相萃取柱净化提取液，并用气相色谱—氢火焰离子化检测器（GC-FID）进行分析测定。结果：MOSH在10.0～1 000 μg/mL范围内具有良好线性关系，相关系数R²=0.999 97。方法的检出限为1.0 mg/kg，定量限为3.0 mg/kg。MOSH的加标回收率为93.3%～103.7%，相对标准偏差为2.3%～5.9%。应用该方法检测市售8个婴幼儿配方奶粉中的MOSH含量，结果在1.06～9.83 mg/kg，表明婴幼儿配方奶粉存在一定的MOSH污染风险。结论：该方法准确、灵敏，适用于婴幼儿配方奶粉中MOSH的检测。     

电感耦合等离子体质谱法测定薄膜包衣粉中的总砷含量

目的 建立一种薄膜包衣粉中砷的电感耦合等离子体质谱检测方法。方法 样品经过混合酸(硝酸：硫酸=10：1)微波消解, 赶酸后, 以500 μg/L锗作为内标, 以氦气作为反应气检测。结果 砷在浓度2.0~40.0 μg/L之间呈现良好的线性关系(r_²=0.9999), 该方法检出限为0.0054 mg/kg,定量限为0.018 mg/kg , 平均回收率为94.40%~101.40%, 相对标准偏差为0.65%。结论 该方法操作简便、重现性好、灵敏度高、准确,适合测定薄膜包衣粉中的砷。     

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