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1.
目的建立高效液相色谱-串联质谱法测定几种动物源食品中氯霉素残留的方法。方法对《动物源食品中氯霉素残留量的测定高效液相色谱-串联质谱法》(农业部第781号公告)中的测定方法进行优化,样品经提取后经HLB固相萃取小柱净化,采用甲醇-水进行梯度洗脱,经Agilent Eclipse-plus C18色谱柱(3.0 mm×100 mm,1.8μm)分离,采用多反应检测负离子模式进行定性及定量分析。结果在0.5~10.0 ng/mL范围内,氯霉素的浓度和色谱峰面积线性关系良好(r=0.9998),方法检出限为0.03μg/kg,定量限为0.1μg/kg,在1.0、2.0和5.0 ng/mL 3个水平的加标回收率为91.58%~109.52%,相对标准偏差小于7.5%。结论该方法快速、准确、灵敏,能满足几种动物源食品中氯霉素残留的测定。  相似文献   

2.
建立了动物源性食品中常山酮残留量的液相色谱检测(High Performance Liquid Chromatography, HPLC)法及液相色谱-串联质谱(High Performance Liquid Chromatography-tandem Mass Spectrometry, HPLC-MS/MS)确证法。动物源性食品中的常山酮,用胰蛋白酶酶解,乙酸乙酯提取,固相萃取柱净化,液相色谱法测定,对于牛组织样品和疑似常山酮阳性的鸡组织样品,采用液相色谱-串联质谱法进行确证。液相色谱法:在50~1 000ng/mL线性范围内,常山酮的回归方程呈良好的线性关系,R~20.999,鸡组织样品在添加水平为50μg/kg和100μg/kg时,回收率为82.50%~96.46%,相对标准偏差(relative standard deviation,RSD)为2.71%~5.44%,方法检出限为25μg/kg,定量限为50μg/kg;液相色谱-串联质谱法:在0.5~50ng/mL线性范围内,常山酮的回归方程呈良好的线性关系,R~20.998,动物源性食品样品在添加水平为0.5μg/kg和5μg/kg时,回收率为70.20%~93.60%,RSD为6.50%~9.48%,方法检出限为0.25μg/kg,定量限为0.5μg/kg。该方法简便、快捷,灵敏度、准确度和精密度均较高,检出限低,解决了残留限量要求较低的牛组织样品中常山酮的检测问题,适用于动物源性食品中常山酮残留量的检测和确证。  相似文献   

3.
动物源性食品中氟苯尼考残留水平和 分布情况分析   总被引:1,自引:0,他引:1  
目的分析动物源性食品中氟苯尼考残留水平和分布规律。方法采用超高效液相色谱-串联质谱法进行残留量测定,并借助Excel2010和社会科学统计软件包18.0对测定结果进行分析。结果方法中,以乙腈-水为最佳流动相,以Welch Xtimate C_(18)为最佳色谱柱。不同品种样品中,氟苯尼考平均回收率为80.3%~95.3%,检出限为0.052~0.095μg/kg,定量限为0.150~0.313μg/kg。472批次样品中,氟苯尼考检出率为15.9%,残留量主要为0.1~1.0μg/kg,检出品种以各鲜肉、胗、大肠以及相应的腊制品和蛋类为主。新复极差分析显示,检出品种中鸡蛋残留量不同于其他品种。结论本研究对氟苯尼考残留水平和分布规律进行了分析,可为市民选择提供参考。  相似文献   

4.
目的建立增强型除脂固相萃取技术结合超高效液相色谱-串联质谱法测定动物源性食品中五氯酚残留量的分析方法。方法样品经8%三乙胺乙腈:水(80:20,V:V)提取,经EMR-Lipid固相萃取柱净化,以5 mmol/L乙酸铵溶液(含0.1%甲酸)-甲醇作为流动相, Waters ACQUITY BEH C_(18)(50 mm×2.1 mm, 1.7μm)进行色谱分离,在电喷雾负离子模式下,多反应监测(multiple reaction monitoring,MRM)方式进行测定,基质匹配外标法定量。结果猪肉、猪肝、鱼、河虾、蟹、牛奶等6种基质中五氯酚在0.5~10 ng/mL范围内线性良好,相关系数r0.997,方法检出限范围为0.1~0.3μg/kg,定量限范围为0.3~0.5μg/kg,在1.0、5.0、10.0μg/kg3个浓度水平下6种基质中回收率范围为81%~98%,相对标准偏差范围为1.74%~4.78%之间(n=6)。结论该方法简单快速、准确可靠,经济环保,重复性好,适用于动物源性食品中五氯酚残留量的测定。  相似文献   

5.
提供一种利用超高效液相色谱-串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)法快速测定动物源性食品中万古霉素残留量的方法。冻猪背膘、冻猪去骨前腿皮和冻猪去骨前腿肉样品用0.1%甲酸水溶液-乙腈溶液(90∶10,V/V)提取,所得提取液用水饱和正己烷除脂、MCX固相萃取柱净化,净化液经氮吹浓缩、流动相定容后用UPLC-MS/MS仪测定。结果表明:在2.0~100.0μg/L质量浓度范围内,万古霉素的线性关系良好,R~20.999 9;该方法的最低检出限为0.3μg/kg,定量限为1.0μg/kg;在10.0、20.0、50.0、100.0μg/kg 4个添加水平下,3种样品中万古霉素的回收率为70.05%~102.97%,相对标准偏差≤4.65%。该方法有效解决了样品基质效应大、灵敏度低等问题,能够保证分析结果的准确性,适用于动物源性食品,尤其是高脂肪含量的动物源性食品中万古霉素的残留量测定。  相似文献   

6.
目的建立超高效液相色谱-串联质谱准确测定鸡肉、鸡蛋中氟苯尼考和氟苯尼考胺残留的分析方法。方法鸡肉和鸡蛋样品加入D5-氯霉素内标,经氨化乙酸乙酯混合溶液超声离心提取,提取液减压蒸馏浓缩后,C18固相萃取柱净化处理,采用超高效液相色谱-串联质谱法对氟苯尼考和氟苯尼考胺同时进行检测。结果氟苯尼考线性范围为0.2~20μg/L,检出限为1.0μg/kg,定量限为3.0μg/kg,方法回收率为88.0%~108.0%,相对标准偏差为4.7%~6.4%;氟苯尼考胺线性范围为0.2~20μg/L,检出限为1.0μg/kg,定量限为3.0μg/kg,方法回收率为76.0%~93.1%,相对标准偏差为4.1%~7.2%。结论本方法精确、重现性好,适用于鸡肉、鸡蛋中氟苯尼考和氟苯尼考胺残留量的测定。  相似文献   

7.
目的建立固相萃取-同位素稀释超高效液相色谱/串联质谱法同时测定动物源性食品中24种β2-受体激动剂残留量的检测方法。方法样品经β-葡萄糖苷酸酶水解,过混合阳离子(MCX)固相萃取柱净化。采用乙腈和含有0.1%甲酸的水为流动相,梯度洗脱,质谱(ESI+)采用多离子检测模式(MRM)对24种β2-受体激动剂残留量进行检测。结果该方法各组分的最低定量限为0.1~0.5μg/kg,在0.1~20.0μg/kg浓度下呈现良好的线性关系,加标回收率为72.5%~109.3%。结论该方法操作简便,准确,快速,灵敏,可同时检测24种β2-受体激动剂的残留量。  相似文献   

8.
目的建立QuEChERS-超高效液相色谱-串联质谱法测定多种动物源性食品中地塞米松残留量的分析方法。方法样品经含1%甲酸的乙腈提取, QuEChERS方法净化后,以乙腈-0.1%甲酸水溶液为流动相,经PhenomenexKinetexF5色谱柱(100mm×3.0mm,2.6μm)分离,采用大气压化学电离源(atmosphericpressure chemicalionization,APCI),正、负模式同时扫描的离子化模式,多反应监测(MRM)模式采集,外标法定量。结果地塞米松在0.5~100 ng/mL浓度范围内线性良好,相关系数(r)为0.99946,检出限为0.10μg/kg;在3个加标水平下,平均回收率为73.2%~95.9%,精密度(n=6)为4.1%~10.7%。结论该方法简单、快速、稳定性高、重现性好,可满足多种动物源性食品中地塞米松残留量的检测。  相似文献   

9.
建立了一种快速准确定性定量检测动物源性食品中喹乙醇代谢物3-甲基-喹喔啉-2-羧酸(MQCA)残留量的液相色谱—串联质谱(LC-MS/MS)检测方法。样品组织通过碱水解提取MQCA,阴离子固相萃取柱净化,LCMS/MS检测,内标法定量。结果显示,在0.5~50.0ng/mL浓度范围内,MQCA线性关系良好,相关系数R2为0.999 7。MQCA检出限为0.1μg/kg,方法在0.1,0.2,1.0μg/kg的添加水平下,回收率为95.6%~108.2%,相对标准偏差为3.4%~14.3%(n=6)。该检测方法准确、快速、灵敏度高,适用于动物源食品中MQCA残留量的检测和确证。  相似文献   

10.
目的 调查研究深圳市市售动物源性食品中氯霉素残留状况及暴露风险,为引导消费和开展安全监管提供借鉴和参考。方法 随机采集2018—2019年深圳市市售畜肉、禽肉、水产品共计511份,使用超高效液相色谱-串联质谱法测定样品中氯霉素的含量,采用点评估法计算深圳市居民通过食用动物源性食品的氯霉素暴露量,并采用暴露边界比(MOE)法对其健康风险进行评估。结果 160份畜肉和60份禽肉中未检出氯霉素,291份水产品(包括贝类、虾、淡水鱼)中氯霉素检出率为26.80%(78/291),其中贝类样品中氯霉素含量为0.05~205.00μg/kg,平均值为13.71μg/kg,检出率为37.21%(64/172);虾样品中氯霉素含量为0.05~2.20μg/kg,平均值为0.20μg/kg,检出率为13.64%(3/22);淡水鱼样品中氯霉素含量为0.05~1.90μg/kg,平均值为0.11μg/kg,检出率为11.34%(11/97),所有样品中氯霉素总检出率为15.26%(78/511)。膳食暴露风险评估结果表明,深圳市居民膳食动物源性食品摄入氯霉素的平均日暴露量为2.06×10-3  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.
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   

18.
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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