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。     

GPC-UPLC-MS/MS测定食用油脂中 5种辣椒素类物质

建立了凝胶渗透色谱-超高效液相色谱-串联质谱法(GPC-UPLC-MS/MS)测定食用油脂中天然辣椒素、二氢辣椒素、合成辣椒素、降二氢辣椒素、高二氢辣椒素含量的方法。样品经凝胶渗透色谱在线净化后，采用超高效液相色谱-串联质谱法分析，动态多反应监测模式（dMRM），同位素内标法定量。结果表明：方法在0.05～10 μg/L范围内线性良好，线性相关系数均大于等于0.998；检出限为0.02~0.05 μg/kg，定量限为0.10 μg/kg；在0.20、1.00、5.00 μg/kg添加水平下，平均加标回收率为90.6％～101.5％，相对标准偏差（RSD）为2.5％～9.7％。该方法前处理过程简便快捷，定量准确，可满足实验室准确测定食用油脂中5种辣椒素类物质的需求。     

气相色谱法测定氨基酸婴儿配方粉中肌醇的含量

目的建立一种适用于氨基酸婴儿配方粉中肌醇检测的气相色谱方法。方法样品中的肌醇用水和乙醇提取后,与硅烷化试剂衍生,正己烷提取,经气相色谱分离,氢火焰离子化检测器检测,外标法定量。结果优化了硅烷化条件,改进了前处理过程,肌醇衍生物在0～20mg/L范围内线性关系良好,相关系数r~2为0.9995,在3个添加水平的回收率为88.0%～108.0%,相对标准偏差为1.0%～5.4%,方法检出限为1.0 mg/100 g,定量限为3.0 mg/100 g。结论该方法准确可靠,重复性好,适用于氨基酸婴儿配方粉中肌醇含量的测定。     

气质联用法测定热带水果中嗪氨灵及其代谢物残留

该研究建立一种基于QuEChERS前处理技术，同时测定热带水果中嗪氨灵及其代谢物三氯乙醛残留量的气质联用法。样品中残留的嗪氨灵及其代谢物三氯乙醛采用乙腈提取后，用十八烷基硅烷键合硅胶和无水硫酸镁净化，经气相色谱柱前衍生化反应，三重四极杆串联质谱仪检测，基质匹配外标法定量。结果表明，方法中2种衍生产物在质量浓度5.0～600 ng/mL范围内线性良好，相关系数R²均大于0.9981，定量限为2.8～8.1μg/kg；不同热带水果样品中添加0.010、0.050、0.400 mg/kg浓度水平时，平均回收率为71.5%～116%，相对标准偏差为1.79%～9.33%。该方法简便、高效、准确，且具有良好的灵敏度和精密度，适用于热带水果中嗪氨灵及其代谢物三氯乙醛残留量的测定。     

凝胶色谱-液相色谱串联质谱法测定植物油中胆固醇含量

以植物油脂为试验材料,建立了凝胶渗透色谱-液相色谱串联质谱法(GPC-HPLC-MS/MS)测定植物油脂中胆固醇含量。样品经凝胶渗透色谱净化后,采用液相色谱串联质谱法(HPLC-APCI-MS/MS)分析,多反应监测模式下(MRM)外标法定量。结果表明:方法在50.0~1 000.0μg/L范围内线性良好,线性相关系数r为0.999,定量限为0.25 mg/kg,回收率范围为76%~89%,相对标准偏差小于15%。该方法前处理过程简便快捷,回收率高,可满足实验室大量、快速分析的需求。     

QuEChERS-GC-MS/MS法检测植物源性运动食品中肌醇含量

采用气相色谱-三重四级杆串联质谱（GC-MS/MS）技术结合改进的QuEChERS前处理测定植物源性运动食品中肌醇含量。通过考察基质效应、衍生及净化条件,系统优化植物源性运动食品中肌醇分析检测最优参数,外标法定量。样品经纯水提取后用现配衍生试剂于85℃水浴中衍生75min;衍生完毕后用Cleanert TPT固相萃取小柱对其进行净化,以正己烷-丙酮（6∶4,V/V）为淋洗液,收集净化液浓缩后经仪器测定。在质量浓度为0.0～5.0μg/mL范围内线性关系良好,相关系数（r）均≥0.9996,方法检出限为0.76～1.12mg/100g;方法定量限为2.57～3.37mg/100g,分别向所选四种试验样品中添加浓度为10、30、50mg/100g肌醇溶液,其加标平均回收率为82.56%～95.79%;相对标准偏差（RSD）为1.24%～8.15%(n=6),该方法与现有气相色谱方法相比,具有前处理简单、结果准确、灵敏度高、重复性好等优势。     

气相色谱法同时测定白酒中丁酸等7种酸酯成分的含量

建立了有关白酒中乙酸乙酯、丁酸乙酯、己酸乙酯、乳酸乙酯、乙酸、丁酸和己酸含量的检测方法，试样中的目标物直接加入内标溶液，用样品溶液定容，过滤膜后上机检测，内标法定量。结果表明，本方法在0.01～1.5 g/L范围内与色谱峰面积的相关系数(r²)均大于0.99，乙酸的检测限为0.006 g/L，定量限为0.020 g/L，其余6种酸酯的检测限为0.003 g/L，定量限为0.010 g/L；乙酸在0.02 g/L、0.06 g/L和0.20 g/L添加浓度水平上的回收率为98.67%～100.39%，其余6种酸酯在0.01 g/L、0.03 g/L和0.10 g/L添加浓度水平上的回收率为97.07%～104.28%。该方法前处理简单、分析时间短、稳定性高，为酱香型白酒中7种酸酯的检测提供了相关技术依据。     

气相色谱法测定发酵乳中的7种短链脂肪酸

建立了气相色谱法检测发酵乳中7种短链脂肪酸(甲酸、乙酸、丙酸、丁酸、异丁酸、戊酸和异戊酸)的方法。利用衍生化对样品进行前处理,通过色谱柱对样品进行分离,通过保留时间进行定性,峰面积进行定量。7种短链脂肪酸的线性范围是20～2 000 mg/L;方法定量限为20 mg/L;方法检出限为5 mg/L;相关系数(R~2)均大于0. 999,加标回收率范围是93. 57%～108. 20%,结果的相对标准偏差(RSD)为2. 40%～9. 56%。该方法准确,灵敏度高,重现性好,可用于检测发酵乳中短链脂肪酸的含量。     

改良QuEChERS-高效液相色谱-串联质谱法检测植物油中的10种植物生长调节剂

采用改良QuEChERS技术作为前处理方法,建立了植物油中10种植物生长调节剂(PGRs)的高效液相色谱-串联质谱快速检测方法。样品用酸化乙腈提取,经增强型基质去除吸附剂(EMR-Lipid)净化,然后用高效液相色谱-串联质谱仪多反应监测模式检测,外标法定量。结果表明:方法线性范围1～100μg/L,10种PGRs线性关系良好,相关系数(r)为0.991～0.998;检出限为0.014～0.188μg/kg,定量限为0.048～0.625μg/kg;10种PGRs的回收率在70.2%～94.7%之间,RSD为1.2%～10.2%。该方法准确、快速、重复性好,适用于植物油中植物生长调节剂的测定。     

快速皂化-中性氧化铝层析净化气相色谱- 质谱法测定植物油中的角鲨烯

为了快速准确地测定植物油中的角鲨烯,通过对样品前处理过程优化和质谱分析条件的摸索,建立了快速皂化-中性氧化铝层析净化气相色谱-质谱法（GC-MS）测定植物油中角鲨烯的方法。结果表明：GC-MS选择离子监测模式内标法定量下,植物油样品中角鲨烯与其他干扰物质得到了良好的分离;在0～194.4 μg/mL质量浓度范围内标准曲线回归方程的相关系数为0.998 6,线性关系良好;方法的变异系数为1.3%～2.6%,加标回收率为95.0%～96.7%;与LS/T 6120—2017相比,所建立的方法具有样品前处理快速简单、精密度好、灵敏度高等优点, 大大提高了角鲨烯的检测效率;采用该方法对10种植物油中角鲨烯含量进行检测,10种植物油中均有检出,其中橄榄油中角鲨烯含量最高,约为6 000 mg/kg。     

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