气相色谱-串联质谱法测定植物油中角鲨烯的含量

目的建立气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定植物油中角鲨烯化合物的方法。方法植物油样品经正己烷超声提取,中性氧化铝固相萃取柱(Alumina-N)净化,内标法定量。结果采用优化后的条件,角鲨烯在0.01～0.64mg/kg的定量范围内,线性关系良好,相关系数在0.99以上。选取不同含量植物油样品(菜籽油、葵花籽油、花生油),在样品添加角鲨烯化合物浓度为10、100、200 mg/kg时,平均回收率为91.5%～106%,相对标准偏差小于4.6%。在正常的光照和室温条件下,角鲨烯在放置1、3、5 d后的浓度分别较0 d时降低了14.8%、20.7%和27.8%,在放置11、13、15 d后的浓度较0 d时降低了37.0%、39.0%和40.5%。结论该方法具有高效、快速、操作简单、实验成本低等优点,可以满足实验室内植物油中角鲨烯的快速、高通量检测。     

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。     

气相色谱-质谱联用测定南瓜籽油中角鲨烯的含量

基于GB/T 22110—2008方法,建立一种简单、快速测定南瓜籽油中角鲨烯含量的气相色谱-质谱联用(GC-MS)方法,考察了甲酯化试剂浓度对角鲨烯提取效果及不同极性色谱柱对角鲨烯分离程度的影响,确定南瓜籽油中角鲨烯含量测定的最佳条件。结果表明,0.2 g南瓜籽油经1 m L0.5 mol/L的氢氧化钾-甲醇溶液进行甲酯化反应,正己烷提取后经极性色谱柱HP-FFAP分离,用GC-MS选择离子监测模式对角鲨烯可以进行定量测定。该方法在10~500 mg/L范围内线性关系良好,相关系数r=0.999 9;检出限为0.12 mg/kg,加标回收率为79.33%~91.33%,平均相对标准偏差为3.99%。采用该方法测定的14种市售南瓜籽油中角鲨烯平均含量为1.44 g/kg。     

气相色谱-串联质谱法测定食用植物油中β-谷甾醇含量

建立了气相色谱-串联质谱法(GC-MS/MS)测定食用植物油中β-谷甾醇含量的分析方法。样品经2 mol/L氢氧化钾-乙醇溶液皂化、石油醚萃取后,采用GC-MS/MS在多反应监测(MRM)模式下对β-谷甾醇含量进行测定。该方法在2.0~20.0μg/m L线性范围内具有良好的线性关系,相关系数为0.999 6;以胆固醇作替代内标,平均加标回收率为95.7%~101.4%,相对标准偏差为1.0%~3.7%;方法的检出限为0.2 mg/kg。该方法操作简便,检测灵敏度高,干扰小,适用于食用植物油中β-谷甾醇含量的检测。     

气相色谱-质谱联用法测定植物油料中角鲨烯的含量及方法比较

建立气相色谱-质谱联用法（Gas chromatography mass spectrometry,GC-MS/MS）分离和测定植物油料中角鲨烯的方法。用氢氧化钾-乙醇溶液超声皂化后,正己烷溶液萃取,氮吹浓缩,正己烷溶解,提取物经HP-5MS柱分离后进入质谱仪检测,外标法定量。该方法在角鲨烯浓度0.1~100.0 mg/L的范围内具有良好的线性关系（r=0.9998）,方法的精密度良好RSD为1.00%~3.35%,加标回收率为83.60%~110.44%,平均加标回收率为98.89%,方法的检出限（RSN=3）为0.10 mg/L。通过气相色谱质谱联用与气相色谱对四类实际油料样品的分析表明,气相色谱质谱联用方法具高效快速、操作简单、污染小以及检测灵敏度高等优点,可以满足植物油料中角鲨烯的快速、高通量检测。     

反相聚合物固相萃取-气相色谱-质谱法测定植物油中角鲨烯和四种植物甾醇

该文建立了基于反相聚合物为填料,固相萃取-气相色谱-质谱法准确测定植物油中角鲨烯和4种植物甾醇的快速分析方法。植物油样品经2 mol/L氢氧化钾-甲醇皂化,采用聚合物反相固相萃取小柱Oasis HLB净化,后经HP-5毛细管色谱柱(30 m×0.25 mm×0.25μm)分离,气相色谱-质谱仪检测,分别以角鲨烷和5α-胆甾烷-3β-醇作为内标进行定量分析。结果表明,角鲨烯和4种植物甾醇在各自的浓度范围内线性关系良好,相关系数均大于0.998,加标浓度为50、250、500 mg/kg时,方法的平均回收率为91%~107%,相对标准偏差分别为1.2%~7.2%,方法的检出限为0.30~5.87 mg/kg。该方法样品前处理简单快速,背景干扰低、灵敏度高、重现性好、回收率高,适用于食用植物油中角鲨烯和4种植物甾醇的准确定量分析。     

GC-MS测定藻油中角鲨烯含量

基于GB/T 22110—2008,建立一种利用GC-MS简单、快速测定藻油中角鲨烯含量的方法。考察了甲酯化试剂用量对甲酯化程度的影响与不同色谱柱对角鲨烯分离程度的影响。0.2 g藻油经1 m L 0.5 mol/L氢氧化钾-甲醇溶液进行甲酯化,正己烷提取后经HP-5MS色谱柱分离,用GC-MS选择离子监测模式对角鲨烯进行定量测定。方法在10~500 mg/L范围内线性关系良好,相关系数r=0.999 8,检出限为0.10 mg/L,加标回收率为92.14%~96.47%,此法也适用于其他植物油中角鲨烯含量的测定。通过比较"复合型"藻油和"非复合型"藻油样品成分及含量上的差异,得出两种类型的藻油除了脂肪酸含量存在差异外,"非复合型"藻油比"复合型"藻油角鲨烯含量高10倍多。     

气相色谱法同时测定植物油脂中的脂肪酸和角鲨烯含量

目的 建立能准确快速并同时测定植物油脂中脂肪酸和角鲨烯含量的气相色谱方法。方法 植物油脂样品皂化酯化后，经正庚烷提取，气相色谱仪分析测定，脂肪酸采用面积归一化法定量，角鲨烯则用外标法定量。结果 37种脂肪酸和角鲨烯得到了良好分离，定性定量准确；角鲨烯在2～500 mg/L范围内具有较好的线性关系，相关系数为0.999 7；在三个添加水平下，样品中角鲨烯回收率在94.1%～104.6%之间，样品相对标准偏差为1.03%、1.24%，角鲨烯的定量限为4 mg/kg，脂肪酸定量限为0.001 3 g/100 g；选用花生油脂肪酸有证标物进行了脂肪酸验证试验，结果满足证书要求，且与国标前处理方法结果一致，相对误差小于2%。结论 本方法准确可靠、检测通量高、前处理操作简便、能耗低，可大大提高检测效率，降低检测成本。     

几种功能性植物油中角鲨烯和维生素E分析

用气相色谱-质谱联用(GC-MS)方法对超临界CO2萃取出的葵花籽油、南瓜籽油、山楂籽油和省沽油籽油中角鲨烯和维生素E进行分析。植物油的萃取采用超临界CO2萃取技术,然后用GC-MS方法分析,用内标标准曲线法同时测定四种植物油中角鲨烯和维生素E的含量。结果表明:所建立的定量分析方法平均回收率在96.4%~102.2%之间,相对标准偏差小于3.0%,线性相关系数大于0.999,方法检测限在2.0~2.5 mg/L之间;四种植物油中角鲨烯和维生素E含量分别为(mg/g):0.30和1.22(葵花籽油),1.98和0.50(南瓜籽油),2.92和2.31(山楂籽油),65.23和27.60(省沽油籽油);其中省沽油籽油中角鲨烯和维生素E含量远远高于常用食用油。     

气相色谱质谱联用测定茶油中角鲨烯含量

建立茶油中角鲨烯气相色谱-质谱联用(GC-MS)的测定方法。茶油通过正己烷直接稀释,采用气相色谱-质谱(GC-MS)选择离子监测(SIM)进行分析,以三十二烷为内标,用内标标准曲线法测定了茶油中角鲨烯的含量。该内标法标准曲线的相关系数为0.999,在0.01～3.00μg/mL范围内线性关系良好,角鲨烯最低检出限为0.03ng,方法的回收率为85.0%～115.0%,相对标准偏差小于5%(n=6)。利用此方法测定广东兴宁和江西赣州两地产茶油毛油中角鲨烯含量分别为120.43μg/mL和97.05μg/mL,该法操作简便、快速,测试结果准确、可靠。     

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