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1.
建立了免疫亲和柱净化-光化学衍生高效液相色谱荧光法测定花生饮料中黄曲霉毒素B1含量的方法。试样经乙腈-水溶液(体积比80∶20)提取,免疫亲和柱富集和净化后,采用Thermo Syncronis C_(18)色谱柱(250mm×4.6mm,5μm),以甲醇-水(体积比55∶45)为流动相,等度洗脱,荧光检测器检测(Ex:360nm,Em:440nm)。结果表明:黄曲霉毒素B1检出限为7.54×10~(-3)μg/kg;标准曲线的线性范围为0.1~20.0ng/mL(r=0.9999);3个不同水平的加标平均回收率为96.88%~98.82%,RSD值为0.85%~1.07%。10批试样中黄曲霉毒素B_1测定值为0~2.09μg/kg,均无过量残留。该方法具有操作简便、灵敏度高、重现性佳等特点,适用于花生饮料中黄曲霉毒素B_1的检测。  相似文献   

2.
为提高花生中黄曲霉毒素B_1的检测效率和准确性,试验通过对提取溶剂、色谱条件和质谱条件的优化,建立了免疫亲和柱-超高效液相色谱串联质谱(UPLC-MS/MS)快速测定花生中黄曲霉毒素B_1的方法,并对方法进行了评估。结果表明,用甲醇-水(60∶40,V/V)对样品进行提取,采用黄曲霉毒素免疫亲和柱萃取、净化,以0.1%甲酸水溶液、0.1%甲酸乙腈溶液作为超高效液相色谱的流动相,在电喷雾离子源(ESI)正离子模式下采用多反应监测(MRM)对花生中黄曲霉毒素B_1进行定性、定量检测,在5.5 min内完成一个样品的分析。结果表明,黄曲霉毒素B_1在0.1~56.0 ng/m L的线性定量范围,相关系数高达0.999 42,检出限低至0.02μg/kg,定量限精确至0.1μg/kg,低、中、高浓度回收率为82%~92%,相对标准偏差5%。该方法具有前处理简单、净化效果好和准确度高的优点,适用于花生等复杂基质样品的黄曲霉毒素B_1定性和定量检测。  相似文献   

3.
目的建立一种高效液相色谱-光化学柱后衍生法测定紫苏籽中黄曲霉毒素B_1的检测方法。方法样品经乙腈-水溶液(84:16,V:V)提取,用免疫亲和柱净化后,经光化学衍生器衍生,在高效液相色谱仪荧光检测器上检测。结果该方法对黄曲霉毒素B_1的最低检测限为0.05μg/kg,定量限为0.20μg/kg,相关系数为0.9990,加标回收率为86.0%~93.5%,相对标准偏差(relative standard deviation, RSD)为1.94%。结论该方法快速、准确、灵敏,适合测定紫苏籽中黄曲霉毒素B_1的含量。  相似文献   

4.
目的建立酶联免疫法测定混合植物油中黄曲霉毒素B_1含量的分析方法。方法采用直接竞争酶联免疫吸附法对样品进行测定。样品经甲醇溶液提取,提取的抗原及黄曲霉毒素B_1标记物与微孔板上的黄曲霉毒素B_1特异性单克隆抗体竞争结合,洗涤除去未结合杂质。将底物加入孵育,产生蓝色产物,加入终止液终止反应蓝色产物变成黄色产物,450nm处测量吸光度。结果本方法在2h内完成混合植物油中黄曲霉毒素B_1含量的测定。黄曲霉毒素B_1的加标浓度在1.0~20.0μg/kg之间时的回收率为76.5%~120.2%,方法定量限为1.00μg/kg。结论该方法快速、准确、灵敏,适合测定混合植物油中黄曲霉毒素B_1。  相似文献   

5.
目的建立酶联免疫法测定混合植物油中黄曲霉毒素B_1含量的分析方法。方法采用直接竞争酶联免疫吸附法对样品进行测定。样品经甲醇溶液提取,提取的抗原及黄曲霉毒素B_1标记物与微孔板上的黄曲霉毒素B_1特异性单克隆抗体竞争结合,洗涤除去未结合杂质。将底物加入孵育,产生蓝色产物,加入终止液终止反应蓝色产物变成黄色产物,450nm处测量吸光度。结果本方法在2h内完成混合植物油中黄曲霉毒素B_1含量的测定。黄曲霉毒素B_1的加标浓度在1.0~20.0μg/kg之间时的回收率为76.5%~120.2%,方法定量限为1.00μg/kg。结论该方法快速、准确、灵敏,适合测定混合植物油中黄曲霉毒素B_1。  相似文献   

6.
目的建立一种免疫亲和固相萃取柱净化-高效液相色谱柱后光化学衍生-荧光检测器同时测定食品中黄曲霉毒素B_1、B_2、G_1和G_2的方法。方法以甲醇-水(70:30,V:V)为提取溶剂,采用高速均质提取,并经过黄曲霉毒素免疫亲和柱净化。结果经月旭公司Welch Ultimate~XB-C_(18)色谱柱(250 mm×4.6 mm,5μm)分离后使用光化学衍生器进行柱后衍生,并采用带荧光检测器的高效液相色谱仪检测,流动相为甲醇/水(45:55,V:V)。黄曲霉毒素B_1、B_2、G_1和G_2线性范围在0.3~50.0μg/L之间,线性相关系数均大于0.999,B_1、B_2、G_1和G_2检出限分别为0.15μg/kg、0.05μg/kg、0.15μg/kg、0.05μg/kg。在3个加标浓度下大米、花生和瓜子等试样的回收率在80.7%~92.6%之间;相对标准偏差(RSD)在2.04~3.87%之间。结论该方法的灵敏度、准确度和精密度均符合黄曲霉毒素的检测技术要求,且简便快速,适用于食品中黄曲霉毒素B_1,B_2,G_1和G_2的准确测定。  相似文献   

7.
建立了一种测定大米中黄曲霉毒素B_1含量的光化学衍生-高效液相色谱方法:试样经乙腈与水的混合液(体积比84:16)提取,多功能净化柱净化、浓缩、高效液相色谱分离,在线光化学柱后衍生,荧光检测器检测,外标法定量,在优化的条件下,黄曲霉毒素B_1的浓度分别为1.0~40.0μg/L时,浓度与峰面积线性关系良好,相关系数0.9996;加标浓度为5~10μg/kg,样品回收率为80.9%~98.7%,平行相对偏差为3.87%,该方法简单快速、灵敏度高、重现性好,用于大米中黄曲霉毒素B_1的测定,效果更好。  相似文献   

8.
目的建立高效液相色谱-串联质谱法快速测定粮油制品中黄曲霉毒素B_1含量的分析方法。方法样品中的黄曲霉毒素B_1经提取、免疫亲和柱净化、浓缩等步骤,以5 mmol/L乙酸铵溶液、乙腈-甲醇溶液(50:50,V:V)为流动相,按照梯度洗脱程序,通过液相色谱-串联质谱法进行测定,外标法定量。结果黄曲霉毒素B_1在0.2~20ng/mL浓度范围内与峰面积呈现良好的线性关系,线性方程为Y=68577.3X-20845,r0.998,加标回收率在85.0%~94.1%之间,相对标准偏差(relative standard deviation, RSD)5.5%,方法检出限和定量限分别为0.07和0.2μg/kg。结论该方法测定结果准确、可靠,可用于快速测定粮油制品中黄曲霉毒素B_1的含量。  相似文献   

9.
建立了用液相色谱测定甜面酱中黄曲霉毒素B_1、B_2含量的方法。试验采用C18色谱柱,以水-甲醇(55+45)为流动相,柱温25℃,荧光检测器检测。该方法黄曲霉毒素B_1、B_2检出限0.8μg/kg(进样量为50μL,S/N=30),标准曲线的线性范围分别为5~200μg/L(r=0.999 4,0.999 2)。该方法测定甜面酱中的黄曲霉毒素B_1、B_2,样品加标回收率(3份25.0 g样品,每份加标1,2和4μg)94.0%~98.3%、93.8%~99.4%,相对标准偏差RSD(n=10)0.78%、1.13%。  相似文献   

10.
目的建立酶联免疫法检测酱油中黄曲霉毒素B_1(Aflatoxin B_1,AFB_1)的分析方法。方法酱油样本经纯乙腈(料液比=1:2,V:V)提取,再做1:9稀释,通过酶联免疫吸附法(enzyme linked immunosorbent assay,ELISA)测定样本中AFB_1。结果当加标浓度为2μg/kg和5μg/kg时,纯乙腈对酱油中AFB_1的提取回收率结果分别为121.3%和106.5%;方法检出限为1μg/kg。与国标方法检测结果的相对标准偏差小于10%。结论本方法准确、灵敏度高,可适用于酱油中AFB_1的检测。  相似文献   

11.
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.  相似文献   

12.
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.  相似文献   

13.
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.  相似文献   

14.
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.  相似文献   

15.
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.  相似文献   

16.
A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.  相似文献   

17.
18.
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.  相似文献   

19.
The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.  相似文献   

20.
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