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1.
目的 建立植物油和动物组织中55种农药残留的快速检测方法。 方法 样品用经改进的QuEChERS方法提取净化,提取液采用在线GPC/GC-MS检测。结果 在0.01~0.20 mg/L范围内各农药组分具有良好的线性关系,相关系数均在0.992以上。方法的加标回收率在60%~130%之间。55种农药定量下限范围为0.005~0.03 mg/kg。结论 该方法操作简便、快速、灵敏、准确,适合于植物油和动物组织中55种农药残留的测定。  相似文献   

2.
植物油中邻氨基苯甲二酰胺类农药残留检测技术研究   总被引:1,自引:1,他引:0  
建立了同时测定植物油中溴氰虫酰胺、氟虫双酰胺、氯虫苯甲酰胺3种邻氨基苯甲二酰胺类农药残留的凝胶渗透色谱(GPC)-液相色谱检测方法。植物油中残留的邻氨基苯甲二酰胺类农药,经环已烷-乙酸乙酯混合溶液提取后,用凝胶渗透色谱系统净化,以乙腈∶0.1mol/L的乙酸铵水溶液(58∶42)作为流动相,DAD检测器测定,外标法定量。测定结果表明:采用本方法检测植物油中3种邻氨基苯甲二酰胺类农药,方法检出限均能达到0.1mg/kg,在标准曲线质量浓度0.1~2 mg/L之间线性相关系数均大于0.999 8,在0.1、0.2、1mg/kg水平添加回收,回收率在70.1%~99.1%范围之间,准确度较高;相对标准偏差范围在3.0%~9.7%之间,精密度较好。  相似文献   

3.
建立分散固相萃取法结合气相色谱技术同时快速测定食用植物油中有机磷、有机氯和拟除虫菊酯66种农药残留的方法。样品经乙腈溶剂3次提取后,使用PSA(Primary secondary Amine,N-丙基乙二胺)和C18分散固相萃取净化,提取溶液经氮吹浓缩过滤后一部分注入气相色谱-电子捕获检测器检测,另一部分经气相色谱-火焰光度检测器检测。样品在0.08、0.16和0.40 mg/kg添加水平的回收率试验中,平均回收率为62.3%~112.3%,相对标准偏差不大于8.6%,检出限在0.001~0.018 mg/kg之间,基本满足国内外对食用植物油中农药最低残留限量的标准要求。  相似文献   

4.
建立一种快速测定稻谷中常用有机磷农药残留量的方法。采用二氯甲烷超声提取,氮吹浓缩,大口径毛细管柱气相色谱法,火焰光度检测器同时测定敌敌畏、甲拌磷和乐果的含量。结果表明:3种农药的线性关系良好,方法添加回收率80%~106%,最小检出量为0.010~0.020mg/kg,满足农药残留的检测要求。本方法操作简单、快速,重现性良好,适用于粮食中有机磷农药残留的快速分析测定。  相似文献   

5.
目的建立茶叶中7种农药残留的快速检测方法。方法采用分散固相萃取净化,气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)测定茶叶中噻螨酮、噻嗪酮、哒螨灵、喹瞒醚、苯醚甲环唑、联苯菊酯和氟氰戊菊酯7种农药的残留。结果 7种农药在0.05~5.00 mg/kg范围有良好的线性关系,相关系数均大于或等于0.9995。3个浓度的平均加标回收率为70%~115%,相对标准偏差为5.0%~13.2%;方法检出限(limit of detection,LOD)为0.005~0.05 mg/kg,定量限(limit of quantitation,LOQ)为0.015~0.15 mg/kg。采用此方法抽检了我国不同地区市场上的110批次的茶叶样品,其中有15批次样品检出联苯菊酯,含量在24~1640μg/kg之间;有4批次样品中检出噻嗪酮,含量在35~150μg/kg之间;3批次样品检出哒螨灵,含量在70~200μg/kg之间。结论本方法符合农药残留分析标准的要求,可用于茶叶中7种农药残留的快速检测和确证分析。  相似文献   

6.
气相色谱法同时测定茶叶中10种有机磷农药残留   总被引:1,自引:0,他引:1  
目的建立用气相色谱法同时测定茶叶中10种有机磷农药残留的方法。方法采用乙腈做萃取溶剂超声波提取,经CARB/NH2固相萃取小柱净化,用气相色谱法FPD检测器检测茶叶中10种有机磷农药。结果在0.05~1.0 mg/kg浓度范围内具有良好的线性关系,相关系数为0.999 63~0.999 86;在有机磷农药添加浓度为0.02~1.0 mg/kg,回收率80.0%~102.0%,相对标准偏差1.8%~5.8%,最低检出限(LOD,S/N=3)为0.002~0.013 mg/kg。结论建立的气相色谱法是一种操作简单、分离效果好、回收率高、方便快速的检测方法。  相似文献   

7.
气相色谱-质谱联用法又称为GC-MS法,广泛应用于多种食品的农药残留检测中。本文采用GC-MS法对市售的20种代饮茶进行了多种农药残留测定,结果显示,样品农药成分检出限范围为0.003~0.007 mg/kg,定量限范围为0.011~0.022 mg/kg,部分样品中检测出了乐果、克百威和甲拌磷。GC-MS法检测快速高效,可用在代饮茶农药残留检测中。  相似文献   

8.
建立植物油中8种常见农药的快速检验方法。样品采用液液萃取提取目标物和初步净化后经改进的QuEChERS方法进行提取净化,提取液经GC-MS进行检测。结果表明,8种农药在大豆油中的检出限为0.004~0.015 mg/kg;在0.02、0.04、0.1、0.2 mg/kg添加水平的平均回收率分别为99%~113%、80.8%~101.5%、71.9%~91.7%、86.3%~103.6%;相对标准偏差(RSD,n=6)分别为6.1%~13.4%、4.3%~8.5%、3.5%~7.4%、3.4%~6.7%。本方法具有操作便捷、快速等特点,适用于植物油中8种农药残留的快速检测。  相似文献   

9.
目的建立气液微萃取仪(gas-liquid microextraction,GLME)与气相色谱质谱联用仪(gas chromatographymass spectrography,GC-MS)测定食品中农药残留。方法称取0.1 g匀浆样品直接加入GLME中进行萃取净化,定容至100μL,结合内标法通过GC-MS检测分析。结果 30种农药在0.001~1 mg/kg浓度范围内线性良好,相关系数在0.9951~0.9999,检出限为0.001~0.021 mg/kg,定量限为0.003~0.070 mg/kg,平均回收率为67%~119%(n=3),相对标准偏差在1%~26%之间。结论该方法快速、准确,能满足果蔬类中多种农药残留的定性定量分析。  相似文献   

10.
建立气相色谱法测定苹果中氟啶脲、毒死蜱等6种农药残留检测的方法。此方法采用乙腈提取苹果中氟啶脲、毒死蜱等6种农药,用氨基柱对样品进行净化,利用气相色谱作为检测手段,ECD检测器进行定性定量分析。研究表明:测定苹果中6种农药残留含量重复性试验相对标准偏差为1.97%~4.92%,定量限为0.002 mg/kg~0.04 mg/kg,检出限为0.000 5 mg/kg~0.02 mg/kg。6种农药在0.05 mg/kg~2.0 mg/kg范围内线性关系良好,r值均大于0.999。此方法检测苹果中氟啶脲、毒死蜱等6种农药残留检测准确,可行,符合国家标准要求。  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   

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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.
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   

18.
Capillary electrophoresis (CE) and polarized light microscopy (PLM) were utilized in the detection of the adulteration of locust bean gum with guar gum. For CE analyses, standards of locust bean and guar gums were extracted with 30% CH3CN, removing the residual proteins from the gum matrix. A 8.75 mM NaH2PO4-20.6 mM Na2B4O7 buffer, pH 9, was used to separate these proteins and to identify marker proteins that were present in the guar gum. These markers did not co-migrate with components in the extracts of mechanically processed locust bean gum, and are used as indicators of adulteration. Using PLM with toluidine blue and iodine staining techniques, unadulterated locust bean gum samples were distinguished from mixed samples through the differential staining of components in locust bean versus guar and tara gums. These experiments in the use of CE and PLM provide orthogonal and complementary methods for the verification of 'true' positives and the elimination of 'false' positives.  相似文献   

19.
An investigation is described in which various polyfunctional compounds were applied to wool in attempts to stabilize the temporary improvements in wrinkle-recovery brought about by ‘annealing’. Several reactive systems involving formaldehyde were found to produce the desired permanently improved wrinkle-recovery.  相似文献   

20.
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