高效液相色谱法测定保健食品中抗坏血酸同分异构体含量

目的 建立一种同时分离和测定保健食品中抗坏血酸同分异构体含量的高效液相色谱法。方法 样品经20 g/L的偏磷酸溶液超声提取, 选用资生堂CAPCELL PAK C18 ADME亲水色谱柱(4.6 mm×250 mm, 5 μm)分离, 以2.3 g/L磷酸二氢铵水溶液(pH值2.0±0.1)为流动相, 等度洗脱, 流速1.0 mL/min, 检测波长 245 nm。结果 该方法能很好的分离L(+)-抗坏血酸和D(-)-抗坏血酸, 2种抗坏血酸在1.0~50.0 μg/mL范围呈现良好的线性关系, 加标回收率分别为99.69%和100.34%, 检出限均为0.05 μg/mL。结论 该方法简单、快速、准确, 适用于保健食品中抗坏血酸同分异构体含量的测定。     

高效液相色谱法测定保健食品中虫草素和腺苷的含量

样品中的虫草素和腺苷用纯水经80℃水浴提取,采用 CALESIL ODS-100C_(18)柱(5 μm,4.6 × 250mm),在流动相为10mmol/LKH_2PO_4缓冲液(pH=6.0):甲醇=85:15的色谱条件下分离,紫外260nm 下检测。虫草素和腺苷的线性范围分别为1.05 μg/ml～10.5 μg/ml 和10.3 μg/ml～103 μg/ml,加标回收率分别为95.8%和96.5%,相对标准偏差分别为0.10%和1.8%,检测限均为0.05 μg/ml(以进样浓度计)。该方法简便、快速、结果准确、可靠,能应用于保健食品中虫草素和腺昔含量的测定。     

QuEChERS-液相色谱-串联质谱法快速测定保健食品中违禁添加药物托拉塞米和双醋酚丁含量

目的 建立QuEChERS-液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)快速测定保健食品中违禁添加药物托拉塞米和双醋酚丁的分析方法。方法 样品经乙腈提取后, 用QuEChERS法净化, Symmetry C18色谱柱分离, LC-MS/MS外标法定量。结果 该方法具有较高的灵敏度, 托拉塞米和双醋酚丁的定量限为0.2 μg/kg; 在0.2~50.0 μg/kg浓度范围, 线性相关系数大于等于0.9986, 平均回收率为87.6%~98.9%, 相对标准偏差为3.8%~10.5%。结论 该方法处理过程快速简便, 灵敏度高、专属性强, 适用于保健食品中物托拉塞米和双醋酚丁的含量的测定。     

高效液相色谱-串联质谱法检测保健食品中25种非甾体类抗炎药

目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)分析保健食品中25种非法添加非甾体类抗炎药的分析方法。方法 保健食品固体试样经甲醇超声提取, 液体试样经水-甲醇萃取来提取, 经液相色谱柱分离后, 在多反应监测(multiple reaction monitoring, MRM)模式下测进行25种非甾体类抗炎药含量的测定, 外标法定量。结果 25种非甾体抗炎药在1~500 ng/mL范围内呈现良好线性关系, 相关系数均大于0.99, 方法检出限为1.5~2.0 μg/kg, 定量限为5.0~6.0 μg/kg, 6.0、12.0和60.0 μg/kg 3个水平平均加标回收率为80.0%~108.2%, 相对标准偏差为6.4%~9.9% (n=6)。结论 该方法针对保健食品基质, 对固体和液体样品分别采取超声萃取和液液直接萃取的提取方式, 操作简便、节约成本、专属性强且灵敏度、回收率高, 满足保健食品中非甾体类抗炎药的检测。     

HPLC法测定保健食品中盐酸氨基葡萄糖含量的研究

目的 建立高效液相色谱法(HPLC)测定保健食品中盐酸氨基葡萄糖含量的简便方法.方法 样品用水超声提取,色谱柱:CAPCELL PAK CR(4.6 mm×150 mm,5 μm);流动相:25 mmol/L乙酸铵+乙腈(加0.1％甲酸)(25 +75,ⅣV);流量1.0 ml/min,检测波长200 nm.结果 盐酸氨基葡萄糖在0.2-26.0 μg范围内呈良好线性,相关系数为1.000;检出限为0.02 μg;回收率99.5％～101.0％;RSD 1.03％.结论 该方法操作简便快速、结果准确可靠,可作为保健食品中盐酸氨基葡萄糖的质量控制监测.     

气相色谱-质谱法检测蔬菜中3种主要塑化剂含量

目的 建立气相色谱-质谱法检测蔬菜中邻苯二甲酸二(2-乙基己基)酯(Di(2-ethylhexyl) phthalate, DEHP)、邻苯二甲酸二异丁酯(diisobutyl phthalate, DIBP)以及邻苯二甲酸二丁酯(dibutyl phthalate, DBP)3种主要塑化剂的含量。方法 样品经正己烷超声提取后, 经Ttx-5MS(30.0 m×0.25 mm×0.25 μm)色谱柱分离, 进样口温度为260 ℃; 载气流速为1.0 mL/min, 柱箱程序升温, 外标法定量检测。结果 在0.025~0.5 μg/mL浓度范围内3种塑化剂的线性关系良好(r>0.999), 检出限分别为0.0048、0.0080、0.015 μg/mL, 加标回收率为103.68%~118.65%, 相对标准偏差在1.16%~5.23%, 满足定量分析要求。结论 本方法简单, 快速, 适用于不同蔬菜中3种塑化剂的定量分析, 且部分塑化剂类化学污染物在叶菜类蔬菜中存在污染积累效应。     

反相液相色谱法测定白藜芦醇胶囊中的白藜芦醇

为监测保健食品中的有效成分 ,建立了高效液相色谱法测定白藜芦醇胶囊中白藜芦醇含量的方法。实验采用KromasilC18柱 ,以乙腈 水 (体积比 30 70 )溶液为流动相 ,用紫外检测器于30 4nm处检测。结果表明 ,白藜芦醇浓度在 10～ 2 5 0 μg/mL时 ,浓度与峰面积呈良好的线性关系 (r=0 9999) ;加标回收率为 92 5 %～ 10 2 6 % ;最低检出浓度 0 6mg/g。方法的精密度良好 ,相对标准偏差 (RSD)为 3 3%。方法快速、简便、准确 ,可作为胶囊类保健食品质量检验的一个定量检验方法。     

甲醇超声提取法测定保健食品中维生素A

目的 采用甲醇超声方法提取保健食品中的维生素A。用高效液相色谱法(high performance liquid chromatography, HPLC)法进行含量测定, 并与GB/T 5009.82-2016进行比较, 同时进行方法学验证。方法 样品前处理方法为甲醇超声提取法。采用C18(4.6 mm×250 mm, 5 μm)色谱柱, 甲醇为流动相, 检测波长为325 nm, 流速为1 mL/min, 柱温为30 ℃, 进样量为20 μL。结果 超声时间为5~15 min提取效率最高, 工作曲线在1.00~10.00 μg/mL范围内线性关系良好, 相关系数为0.9998, 相对标准偏差为1.82% (n=6), 平均回收率为101.09%, 方法检出限为10 μg/100 g, 定量限为31 μg/100 g。结论 和国标法相比, 本方法操作简单、准确度高, 适用于保健食品中维生素A含量的测定。     

气相色谱-质谱法测定蔬菜中65种除草剂的残留量

目的 建立蔬菜中65种不同类别除草剂的气相色谱-质谱(GC-MS)检测方法.方法 样品用乙腈超声提取后,经Carb/NH2柱净化,采用GC-MS检测,以基质匹配的标准校正曲线外标法定量.结果 除卞草唑的线性范围为20～1 000 μg/L,其他64种除草剂在10～1 000 μg/L范围内呈良好线性,相关系数均大于0.998;各农药的方法检出限为0.02 ～2.2 μg/kg,定量限为0.1～ 7.4 μg/kg;以空白蔬菜样品(选取油菜为代表性基质)进行加标水平为5、10和20 μg/kg的加标回收试验,除扑草灭和乙氧苯草胺的回收率在41.1％ ～59.4％之间外,各除草剂的回收率均在60.9％～117.9％之间,相对标准偏差(RSD)低于14.0％.对9份蔬菜样品(包括土豆、油菜、白菜、菠菜)进行检测,1份样品(白菜)检出氟乐灵,其含量为2.0 μg/kg.结论 该检测方法快速、简便、准确,适用于蔬菜样品中除草剂类农药残留的检测.     

高压液相色谱-线性离子阱串联质谱法测定红葡萄酒中多菌灵和甲基硫菌灵

目的 建立红葡萄酒中多菌灵和甲基硫菌灵残留的高压液相色谱-串联线性离子阱质谱(HPLC-LIT-MS/MS)检测方法。方法 样品经过乙腈提取, 在梯度洗脱程序下经CAPCELL PAK CR 1:20色谱柱分离后, 采用HPLC-LIT-MS/MS, 在二级质谱选择反应监测(SRM)模式进行测定。结果 红葡萄酒中多菌灵和甲基硫菌灵添加水平为10、20、50 μg/L时, 平均回收率分别为82.5%~103.1%和93.7%~115.2%。检出限(LODs)分别为0.063 μg/L和0.019 μg/L, 定量限(LOQs)分别为0.125 μg/L和0.075 μg/L。结论 该方法快速简便, 灵敏度高, 准确度和精密度均满足痕量分析要求。     

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