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1.
鸡肉样品经过固体基质分散,固液萃取,快速溶剂萃取仪浓缩,复溶;采用超高压高效液相色谱串联三重四级杆质谱检测器(UPLC-MS/MS)同时分析鸡肉中的6种磺胺类药物(磺胺甲嘧啶、磺胺二甲嘧啶、磺胺间甲氧嘧啶、磺胺甲噁唑、磺胺喹恶磷、磺胺间二甲氧嘧啶)。质谱采用电喷雾离子源,正离子电离模式(ESI+)和多反应扫描监测模式(MRM)进行测定,以各成分的保留时间、定性定量离子对及定性定量离子对相对离子比来定量分析。结果表明,6种磺胺化合物的浓度线性范围为1~200 ng/m L,空白样品加标回收范围为5~100μg/kg,检出限为0.05~0.10μg/kg。该方法前处理简单快捷、仪器分析快速且灵敏度高、结果准确、重复性好;不仅适用于鸡肉且适用于各种禽畜肉样品的品质监测,而且适合大批量样品的快速检测分析。  相似文献   

2.
建立了一种同时测定水产品(鳗鱼、鮰鱼、龙虾)中13种磺胺类药物残留的高效液相色谱法。样品经乙腈提取,正己烷液-液分配,阳离子固相萃取小柱净化后,采用高效液相色谱分离,紫外检测器检测,外标法定量。13种磺胺类药物在0.1~5.0μg/ml范围内线性关系良好,相关系数R2为0.9997~0.9999,加标回收率为62%~97%,相对标准偏差为2.01%~10.46%。定量测定低限磺胺二甲嘧啶、磺胺甲氧嘧啶、磺胺-6-甲氧嘧啶、磺胺氯哒嗪、磺胺甲基异恶唑、磺胺二甲异恶唑、磺胺间二甲氧嘧啶、磺胺喹恶啉为0.02mg/kg,磺胺嘧啶、磺胺吡啶、磺胺噻唑、磺胺甲基嘧啶、磺胺甲噻二唑为0.05mg/kg。  相似文献   

3.
建立水产品中14种磺胺类药物的高效液相色谱-柱后衍生荧光检测法。均质后的水产品试样用乙酸乙酯提取、盐酸溶液反萃取、正己烷脱脂、反相色谱柱分离、在线柱后衍生、荧光检测器检测、内标法定量。14种磺胺类药物(磺胺、磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶、磺胺5-甲氧嘧啶、磺胺二甲基嘧啶、磺胺甲氧哒嗪、磺胺氯哒嗪、磺胺6-甲氧嘧啶、磺胺甲基异噁唑、磺胺多辛、磺胺异噁唑、磺胺二甲氧哒嗪、磺胺喹噁啉)的线性范围为2.5~800μg/L,线性相关系数均大于0.9934;在2.5~200μg/kg三个添加水平范围内的平均回收率为88.9%~98.6%,相对标准偏差均小于6.96%。14种磺胺类药物的定量检出限为2.5~20μg/kg。方法重现性好、灵敏度高,杂质干扰少,广泛适用于水产品中磺胺类药物残留的检测。  相似文献   

4.
利用高效液相色谱-质谱联用技术,建立了对虾组织中磺胺嘧啶、磺胺二甲嘧啶、磺胺甲氧嘧啶、磺胺喹恶啉残留的分析方法。样品加入无水硫酸钠和乙腈后,进行匀质和提取,再用乙腈饱和的正己烷脱脂净化。通过优化色谱条件,以选择离子方式进行定量。选择离子分别为m/z 300.9,280.8,278.8,250.8。磺胺检测的线性范围是0.05~0.50mg/Kg,检测限为5μg/Kg,回收率为74.2~99.8%,RSD小于6.1%。  相似文献   

5.
目的建立高效液相色谱-串联质谱法(highperformanceliquidchromatography-tandemmass spectrometry, HPLC-MS/MS)同时测定鸡脂肪中磺胺嘧啶、甲氧苄啶的残留量的方法。方法样品经乙腈2次提取,以乙腈和0.1%甲酸水溶液为流动相进行溶解后,用正己烷2次脱脂,过滤膜后用于液相色谱串联质谱仪测定,基质添加标准溶液外标法定量。结果 0.5~100 ng/mL的浓度范围内磺胺嘧啶、甲氧苄啶色谱峰面积与浓度呈良好线性相关,相关系数均大于0.99;方法定量限为1.0μg/kg;鸡脂肪样品中磺胺嘧啶、甲氧苄啶在1.0~200.0μg/kg添加水平内的平均回收率在66.3%~97.5%之间,批内批间相对标准偏差均小于20%。结论该方法回收率满足残留检测要求,且方法的重现性良好,满足国内外兽药残留相关法规规定。  相似文献   

6.
目的 建立基质固相分散一高效液相色谱法测定蜂蜜中10种磺胺类药物残留量的方法,包括磺胺、磺胺嘧啶、磺胺吡啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲氧嘧啶、磺胺间甲氧嘧啶、磺胺氯哒嗪、磺胺甲噁唑和磺胺二甲异噁唑.方法 蜂蜜样品与C,:固相吸附荆于玻璃研钵中研磨均匀,得半干状混合物,装入空的固相萃取管中,盖上一层滤纸,以1+3二氯甲烷-乙酸乙酯(V/V)为洗脱剂洗脱,洗脱液经氮气吹干,用流动相溶解残渣,经0.45 μtm滤膜过滤,Agilent TC-C_18(4.6 mm×250 mm,5μm)色谱柱分离,高效液相色谱法测定.结果 10种磺胺类药物的线性范围为0.10~10.00 mg/L,相关系数r > 0.999,样品加标回收率60.0%~109.3%,相对标准偏差小于10%,方法检出限0.016-0.025 mg/L,样品中磺胺类检出限为0.050~0.079 mg/kg.  相似文献   

7.
本研究利用紫外诱变方法筛选到两株具有磺胺敏感性的菌株H1、H2。DNA鉴定为芽孢杆菌属嗜热脂肪地芽孢杆菌种。将H1、H2作为指示菌,进行牛奶磺胺残留总量检测,发现这两株菌对不同种类的磺胺药物具有不同的灵敏度。当H1、H2处理后芽孢悬液菌落总数比为3:4时,检测试剂盒有较好的灵敏度,分别为磺胺:30μg/L、磺胺嘧啶:30μg/L、磺胺甲嘧啶:30μg/L、磺胺二甲嘧啶:30μg/L、氨苯磺胺:60μg/L、磺胺噻唑:45μg/L、磺胺氯哒嗪:80μg/L、磺胺甲噁唑:75μg/L、磺胺胍:75μg/L。在此比例下对两株菌同时传代,探究菌株传代对检测试剂盒灵敏度的影响,结果表明以第四代菌为指示菌时,该检测试剂盒丧失对氨苯磺胺和磺胺胍的敏感性;第六代丧失对磺胺氯哒嗪、磺胺甲噁唑的敏感性;对于磺胺、磺胺嘧啶、磺胺甲嘧啶、磺胺噻唑的敏感性可稳定到第七代。通过与国内外商业试剂盒对比,本试剂盒灵敏度高于国内试剂盒,检测时间优于国外试剂盒。  相似文献   

8.
目的 建立基质固相分散-高压液相色谱-高分辨质谱测定猪肉中22种磺胺类药物残留量的测定方法, 包括磺胺苯酰、磺胺醋酰、磺胺氯哒嗪、磺胺嘧啶、磺胺间二甲氧嘧啶、磺胺二甲嘧啶、磺胺甲基嘧啶、磺胺多辛、磺胺间甲氧嘧啶、磺胺甲氧哒嗪、磺胺对甲氧嘧啶、磺胺甲噁唑、磺胺甲噻二唑、磺胺二甲噁唑、磺胺苯吡唑、磺胺吡啶、磺胺喹噁啉、磺胺噻唑、磺胺异噁唑、磺胺胍、甲氧苄啶、磺胺索嘧啶。方法 猪肉样品与弗罗里硅土混合, 研磨均匀, 装入空的固相萃取管中, 用15 mL 1%乙酸二氯甲烷: 乙酸乙酯(1∶3, v/v)洗脱, 洗脱液用氮气吹干, 残渣用1 mL乙腈: 10 mmol/L乙酸铵溶液(15∶85, v/v)溶解。加入1 mL正己烷混合离心, 取下层溶液, 经0.22 μm滤膜过滤后用Agilent Poroshell 120 EC-C18(2.1 mm×150 mm, 2.7 μm)色谱柱分离, 高分辨质谱测定。结果 22种磺胺类药物在 10~100 μg/kg范围内线性关系良好, 相关系数r>0.99, 除磺胺甲噻二唑、甲氧苄啶和磺胺脒/磺胺胍加标回收率小于40%外, 其余均大于60%, 定量限为 5~10 μg/kg。结论 本方法具有前处理快速、高效、有机试剂用量少、成本小等优点, 适用于猪肉中磺胺类药物残留量的测定。  相似文献   

9.
目的:建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时快速测定猪肉中氯霉素、磺胺甲嘧啶、磺胺二甲嘧啶、磺胺噻唑、甲氧苄啶和磺胺嘧啶残留量的分析方法。方法:猪肉加入乙酸乙酯后匀浆,转移有机层N_2吹干,残渣用10%乙腈水溶液溶解,正己烷除脂,采用BEH C_18(2.1 mm×50 mm,1.7μm)色谱柱分离,以乙腈和水为流动相进行梯度洗脱,采用电喷雾离子源(ESI),以多反应监测(MRM)方式检测。结果:在该实验条件下,氯霉素和5种磺胺类药物分别在9.6~384 ng/kg和0.51~20.8μg/kg浓度范围呈良好的线性关系,R~2均大于0.99;氯霉素检出限为3.2 ng/kg,定量限为9.6 ng/kg,5种磺胺类药物检出限为0.158~0.173μg/kg,定量限为0.475~0.52μg/kg;方法的平均回收率范围为70.84%~103.99%,相对标准偏差为1.98%~8.01%。结论:此方法具有简便快捷、灵敏度高、定量准确等特点。  相似文献   

10.
牛奶中多种磺胺类抗生素残留的HPLC快速分析   总被引:1,自引:0,他引:1  
孙晶玮  赵新淮 《食品科学》2007,28(6):256-259
研究了牛奶中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺二甲氧嘧啶六种磺胺类抗生素的多残留高效液相色谱(HPLC)分析方法。样品经氯仿-丙酮(2:1,V/V)提取两次,提取液浓缩至干。残渣用流动相甲醇-0.08%乙酸(60:40,V/V)溶解,净化后以反相C18柱,甲醇-0.08%乙酸等度洗脱,紫外检测器检测、外标法定量。结果表明,这六种抗生素在0.01~1.0mg/L浓度范围内呈线性关系,磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶检的检出限为0.010mg/L、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺间二甲氧嘧啶检出限分别为0.015mg/L。分析的添加回收率为69.4%~123.5%,变异系数为<8%,整体分析时间小于3h。方法具有处理简单、检测快速、准确的特点。  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.
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   

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.
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   

19.
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   

20.
《造纸信息》2014,(8):79-79
Ministr y of Industr y and Information Technology confirmed that the main expected targets for energysaving and comprehensive utilization in 2014 are:energy consumption and CO2 emissions per unit of industrial added-value decreases by 4.5%,water consumption per ten thousand Yuan of industrial added-value decreases by7%,comprehensive utilization of industrial solid waste is further improved,and pollution emissions in key industries is markedly reduced.  相似文献   

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