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1.
目的 建立高压液相色谱-电喷雾串联质谱(HPLC-MS-MS)同时测定河豚鱼和鳗鱼中9种青霉素残留量的检测方法。方法 样品经乙腈-氨水溶液提取后, 用C18色谱柱分离, 乙腈-乙酸为流动相梯度洗脱, 最后采用液相色谱-电喷雾串联质谱在正离子多反应监测模式下测定。结果 在1.0~20 μg/kg(LOQ~10LOQ)范围时, 方法线性关系良好, 相关系数大于0.999。在LOQ、2 LOQ、4 LOQ、10 LOQ四个添加水平下青霉素的回收率在81.4%~109.7%之间, 相对标准偏差2.81%~7.12%之间, 方法检出限是: 萘夫西林、青霉素 G、哌拉西林、青霉素 V、苯唑西林为1.0 μg/kg; 阿莫西林、氨苄西林、氯唑西林、双氯西林为2.0 μg/kg。结论 此方法灵敏度高, 准确性好, 适用于水产品中青霉素的定量检测。  相似文献   

2.
目的 建立分散固相萃取结合超高效液相色谱-串联四级杆质谱技术测定禽蛋中五氯苯酚残留量的分析方法。方法 取均质后的禽蛋样品经乙腈溶液提取, 加入无水硫酸镁和氯化钠进行脱水和盐析,高速离心分层后, 取适量乙腈层溶液经0.1%(V:V)甲酸稀释后, 用酸性氧化铝粉末进行样品净化并以10000 r/min离心取上清液, 过0.22 μm滤膜后上机测定。使用反相色谱柱进行分离, 流动相为乙腈:0.1%甲酸=65:35, 采用等度程序进行洗脱, 串联四级杆质谱进行定性定量分析。结果 五氯苯酚在5~250 μg/kg范围内线性关系良好(r>0.995), 方法的最低检出限为2.5 μg/kg, 最低定量限为5 μg/kg, 添加回收率在74.44%~91.91%, 相对标准偏差(relative standard deviation, RSD)<10%。结论 该方法具有较好的准确度与精密度, 适用于禽蛋中五氯苯酚残留量的测定。  相似文献   

3.
GC-MS法同时测定水产品中6种丁香酚类麻醉剂的残留量   总被引:1,自引:0,他引:1  
建立了同时检测水产品中6种丁香酚类麻醉剂残留量的气相色谱-质谱(GC-MS)检测方法。样品经乙腈超声提取,分散固相萃取净化后氮吹浓缩、定容,用气相色谱-质谱仪进行测定,外标法定量。6种丁香酚类化合物在1.0~200.0 μg/L的浓度范围内线性关系良好,相关系数R~2为0.9956~0.9995。又分别在罗非鱼、南美白对虾以及扇贝肌肉样品中添加1.0~10.0 μg/kg的混合标准溶液,测定平均回收率在82.2%~100.7%范围内,相对标准偏差在0.6%~7.4%之间。方法的定量限(LOQ),丁香酚、甲基丁香酚、异丁香酚、乙酰基异丁香酚为1.0 μg/kg,甲基异丁香酚和乙酸丁香酚酯为0.5 μg/kg。  相似文献   

4.
建立了水产品中喹乙醇(OQX)及其代谢物3-甲基-喹噁啉-2-羟酸(MQCA)的超高效液相色谱串联质谱快速测定方法。试样经乙酸乙酯+乙腈(1+1,V/V)液液萃取提取和净化后,BEH C18UPLC进行分离,多反应选择离子检测。方法的回收率和变异系数分别在62.5%~91.4%和2.6%~11.8%之间。本方法对水产品中喹乙醇和3-甲基喹噁啉-2-羧酸的检测限均为1.0μg/kg。  相似文献   

5.
本文建立了Qu ECh ERS/液相色谱-质谱/质谱(HPLC-MS/MS)测定水产品中氯硝柳胺残留量的分析方法。样品经氨化乙腈提取,C_18吸附剂与中性氧化铝净化后,采用HPLC-MS/MS选择反应监测(SRM)负离子模式测定进行定性、定量分析。结果表明:在0.5~100 ng/m L范围内,峰面积与浓度线性良好,相关系数为0.9996;氯硝柳胺检出限(LOD)为0.2μg/kg,定量限(LOQ)为0.4μg/kg,检测结果的相对标准偏差为4.33%~9.91%(n=5),平均加标回收率达到74.6%~92.1%。该方法具有较高的适用性和选择性,在水产品中氯硝柳胺的残留测定中具有很好的应用前景。  相似文献   

6.
目的 建立液相色谱-串联质谱测定肉鸡中金刚烷胺残留量的分析方法, 探究鸡肉和鸡肝中的残留代谢规律。方法 样品用乙腈-乙酸-1%三氯乙酸(70:2:30, V:V:V)溶液提取, 固相萃取小柱净化后, 用液相色谱-串联质谱仪进行测定, 利用金刚烷胺-D6为内标定量。结果 金刚烷胺在0~10 μg/kg范围内线性良好, 相关系数(r2)为0.9995, 方法检测限为1 μg/kg。在添加质量浓度1~10 μg/kg范围内回收率为90.1%~95.7%, 相对标准偏差为1.17%~1.62%(n=6)。药物饲喂实验结果表明, 金刚烷胺在肉鸡中吸收快、分布广, 鸡肉中的残留明显高于鸡肝中残留含量, 鸡肉更容易产生药物蓄积。在停药13 d后, 鸡肉中金刚烷胺仍有药物蓄积, 而鸡肝中的金刚烷胺残留量为未检出。结论 该方法操作简单、灵敏度高、稳定性好, 适用于肉鸡中金刚烷胺残留的测定, 揭示金刚烷胺在肉鸡中残留代谢规律。  相似文献   

7.
建立了固相萃取-液相色谱-电喷雾串联质谱(SPE-HPLC-ESI-MS/MS)测定水产品三卡因、苯佐卡因、喹哪啶3种鱼用麻醉剂残留量的检测方法。样品采用磷酸盐缓冲液-甲醇混合溶液提取,经过Waters Oasis HLB固相萃取柱净化,采用Accucore aQ C18色谱柱分离,以0.1%(v/v)甲酸的水溶液和乙腈溶液作为流动相,梯度洗脱,电喷雾正离子模式下分析检测,外标法定量。3种化合物在1~1000 ng/mL浓度范围内线性良好,相关系数R2均大于0.99,方法的检出限为0.10~0.25 μg/kg。在样品中添加0.5、2、5 μg/kg 3个浓度水平的加标实验中,平均添加回收率在76.8%~93.6%,相对标准偏差(RSD)在2.7%~11.2%,符合残留检测的要求。该方法快速、准确、可靠,适用于水产品中鱼用麻醉剂残留的测定。  相似文献   

8.
高效液相色谱-串联质谱法测定水产品中的喹乙醇   总被引:6,自引:0,他引:6  
为测定水产品中喹乙醇的残留量,建立了高效液相色谱-串联质谱联用(HPLC-MS/MS)的测定方法。均质后的试样经水提取、液-液分配净化后,采用ZORBAXSB-C18色谱柱,并以0·1%乙酸 乙腈(70 30,体积分数)为流动相,色谱分离后直接进入串联质谱检测器。采用电喷雾正离子,多反应监测(MRM)模式检测,外标法定量。方法的检出限为10μg/kg,浓度在0·5~500μg/L范围内,线性良好(r=0·9989),添加浓度在10~500μg/kg时,不同水产品基质的回收率在74·3%~93·5%之间,相对标准偏差(RSD)小于5·6%。本方法检出限低,回收率高,定性可靠,定量准确,适合于水产品中喹乙醇残留的检测。  相似文献   

9.
卢剑  范素芳  李强  夏静  李挥  张岩 《食品科学》2016,37(10):193-197
建立猪肉样品中万古霉素、去甲万古霉素和替考拉宁的高效液相色谱-串联质谱测定方法,采用选择反应监测方式,外标法定量。猪肉样品经0.1%甲酸-乙腈(85:15,V/V)溶液提取,正己烷脱脂后,万古霉素和去甲万古霉素经阳离子交换柱净化、替考拉宁经C18固相萃取柱净化,以乙腈-0.1%甲酸为流动相梯度洗脱,经C18柱分离、质谱进行测定。添加量为10、20 μg/kg和50 μg/kg时,方法回收率范围为75.3%~83.3%,相对标准偏差小于9%。猪肉中万古霉素、去甲万古霉素的检出限、定量限分别为2 μg/kg和4 μg/kg,替考拉宁的检出限、定量限分别为4 μg/kg和8 μg/kg。该方法适用于猪肉样品中万古霉素、去甲万古霉素和替考拉宁的定性、定量检测。  相似文献   

10.
目的 建立高效液相色谱法定量测定水产品中四环素类残留量,同时采用高效液相色谱-串联质谱法进行定性确证和定量检测。方法 具体优化了缓冲提取液浓度、固相萃取柱类型、色谱条件选择等测定环节。样品经柠檬酸缓冲液提取,固相萃取柱净化后,以液相色谱-紫外检测器进行定量检测,同时也可通过高效液相色谱-串联质谱仪进行定性和定量。结果 在10~200 ng/mL范围内线性良好(r>0.999),四环素类目标物在10、50、100 μg/kg 3个水平上进行加标回收试验,回收率为76.0%~94.5%,相对标准偏差为3.9%~7.4%,高效液相色谱法检出限为5 μg/kg,液相色谱-串联质谱法检出限为1 μg/kg。结论 该方法简便、稳定、准确,适合测定水产品中的四环素类残留量。  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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