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1.
建立了固相萃取-离子对色谱法测定酱油与黄豆酱中的三聚氰胺。样品经甲醇提取,WatersMCX固相萃取柱净化。分析时用InertsillODS-SPC18色谱柱(5μm,4.6×250mm)分离。水(缓冲液:0.01moL/L柠檬酸+0.01moL/L辛烷磺酸钠,pH=3.0)∶乙腈=92∶8(V/V)溶液为流动相,流速1.0mL/min,在紫外波长240nm下检测。三聚氰胺在0.02~2.00mg/L的范围内,有良好的线性关系(r2=0.9999),方法检出限为1.0mg/kg,加标回收率在83.5%~109.3%范围内,相对标准偏差小于5.0%。  相似文献   

2.
连庚寅  侯美军  林勤保  宋欢  李波  武京  李梅 《食品科学》2009,30(18):255-257
建立动物源性食品中三聚氰胺含量测定的超高效液相色谱法。鸡蛋样品用1% 三氯乙酸- 乙腈(3:1,V/V)溶液提取、离心、固相萃取柱净化,然后采用CR 色谱柱(阳离子交换填料SCX 与C18 包被型填料按质量比1:4 混合)进行超高效液相色谱分析。兔肉样品用乙腈提取,离心后以强阳离子色谱柱进行超高效液相色谱分析。对色谱条件进行优化,选用236nm 作为检测波长,鸡蛋中三聚氰胺在浓度为1.00~5.00mg/L 的范围内线性关系良好,在添加浓度为1.00、2.00、5.00mg/kg 时,添加回收率在89.24%~91.06% 之间,RSD 小于6.00%。对于兔肉中三聚氰胺浓度在0.4~4mg/L 的范围内线性良好,在添加浓度为2.00、5.00、10.00mg/kg 时,添加回收率在82.65%~86.54% 之间,RSD 小于7.50%。该方法简便、快速,检测灵敏度、准确度及精密度均满足检测要求。  相似文献   

3.
建立了大米中甲萘威农药残留量的固相萃取-高效液相色谱(SPE-HPLC)分析方法。以乙腈为提取剂,振荡提取,采用C_(18)固相萃取柱净化,经C_(18)柱(3.9 mm×300 mm,10μm)分离,乙腈-水(55︰45,V/V)为流动相,柱温40℃,流速1.0 m L/min进行分离,紫外检测器280 nm下进行检测。甲萘威的质量浓度在0.05~2.00μg/mL范围内线性良好,相关系数为0.999 9。在0.50,1.25和2.50 mg/kg 3个添加水平下,甲萘威的加标回收率为92.41%~110.18%,相对标准偏差在2.91%~4.35%(n=6),检出限为0.006 mg/kg。该方法具有样品前处理操作简单、灵敏度高、试剂用量少、重现性好等优点,适用于大米中甲萘威的定性定量分析。  相似文献   

4.
建立奶粉中地塞米松的高效液相色谱-质谱/质谱测定方法。样品经甲酸乙腈溶液超声提取,经Oasis PRiME HLB固相萃取柱净化后上样。色谱条件采用Waters XBridge C18柱(2.1 mm×150 mm,5μm),流动相为0.1%甲酸水溶液-乙腈梯度洗脱,流速为0.3 mL/min,柱温40℃,采用电喷雾正离子扫描模式。结果表明:该物质检出限为1.0μg/kg,定量限为3.0μg/kg,线性范围:0~20 ng/mL。加标回收率为90.7%~98.9%。该方法操作简单高效,重现性较好,适用于奶粉中地塞米松含量的测定。  相似文献   

5.
超高效液相色谱测定鱼体中的苯佐卡因残留量研究   总被引:1,自引:0,他引:1  
建立超高效液相色谱法(UPLC)快速测定鱼体中苯佐卡因的方法。通过乙腈提取,固相萃取柱净化,采用超高效液相色谱分离检测。苯佐卡因在0.010~0.300μg/mL范围内呈良好线性关性,相关系数可达0.999 2,选用乙腈-0.1%甲酸水(4∶6)作流动相,Waters Acquity BEH C18色谱柱(50 mm×2.1 mm,1.7μm),波长290 nm,流速0.4 mL/min,定量限达0.010 mg/kg,对0.010,0.025和0.100 mg/kg 3个浓度水平进行添加回收试验,回收率在85.5%~93.1%,相对标准偏差(n=6)均小于10%。  相似文献   

6.
建立一种同位素内标-超高效液相色谱串联质谱快速测定含乳饮料中三聚氰胺残留的分析方法。样品经乙腈提取,Generik DBX固相萃取柱净化,快速离心蒸发系统浓缩,通过MN Nucleoshell Hilic色谱柱梯度洗脱,采用电喷雾离子源(ESI~+)电离,多反应监测模式(MRM)采集信号,同位素内标法定性和定量。结果表明,三聚氰胺在2~200 ng/mL浓度范围内线性关系良好(r=0.9998),方法定量限为2μg/kg;10、25、50μg/kg三个添加水平时回收率为82.37%~103.15%,相对标准偏差6%。该方法处理简单、准确度好、灵敏度高,适合含乳饮料中三聚氰胺残留的快速检测。  相似文献   

7.
经过三氯乙酸、乙腈超声震荡离心提取,混合型阳离子交换固相萃取柱净化后的样品采用HPLC法测定。色谱条件:AgilentEclipseXDB-C_8柱(4.6×250mm),流动相为乙腈—离子对缓冲液(pH=3.0),体积比16︰84,流速为1.0mL/min;检测波长为240nm;柱温40℃;进样量为20μL。本法相对标准偏差为0.34%,最低检出限为0.05μg/mL,回收率为90%-105%。本法操作简便,样品出峰快,经济省时,准确可靠,适用于液态奶中三聚氰胺的含量测定。  相似文献   

8.
研究建立了禽蛋中五氯酚及其钠盐的液相色谱-串联三重四极杆质谱测定方法。样品经体积分数5%三乙胺的乙腈-水溶液(7:3,V/V)提取,混合型阴离子固相萃取柱净化,经ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱分离,以5 mmol/L乙酸铵(含0.1%甲酸)溶液和乙腈作为流动相,进行梯度洗脱,采用多反应监测负离子模式监测,基质匹配标准曲线外标法定量。在该优化条件下,五氯酚及其钠盐在1.0~20 ng/mL浓度范围内线性关系良好,相关系数均大于0.998,检出限为0.5μg/kg,定量限为1.0μg/kg。在不同浓度添加水平下(1.0、2.0、5.0μg/kg),平均回收率为74.0%~101.3%,相对标准偏差为0.78%~6.56%(n=6)。该方法简单、高效、准确,提取液经冷冻处理后避免了净化时固相萃取柱堵塞情况出现,缩短实验时间,优化后的实验方法适用于禽蛋中五氯酚及其钠盐的残留检测。  相似文献   

9.
杨嘉  丁娟芳  周元元  徐秋  朱姜  王帅 《食品科学》2014,35(6):172-175
建立高效液相色谱-二极管阵列检测器同时检测乳粉中三聚氰胺和双氰胺的分析方法。采用1%三氯乙酸溶液提取样品中的三聚氰胺和双氰胺,氨基柱为分析柱,流动相为乙腈-水(75∶25,V/V),流速1.0 mL/min,检测波长233 nm。2 种物质在0.005~60 mg/L范围内与其峰面积线性关系良好,不同添加水平的回收率在83.2%~102.6%,三聚氰胺和双氰胺的方法定量限分别为0.17、0.15 mg/kg,方法变异系数为2.3%~7.2%(n=6)。此方法操作简便、快速、成本低,适用于乳粉中三聚氰胺和双氰胺的同时检测。  相似文献   

10.
建立了猪肝中大环内酯类抗生素螺旋霉素(SPI)、北里霉素(KIT)、替米卡星(TILM)和泰乐菌素(TYL)的高效液相色谱(二极管阵列检测器)检测方法。样品经甲醇提取,Bond Elut SCX固相萃取柱(500 mg,3 mL)净化,液相色谱分析采用Waters Atlantis~(TM)dC_(18)柱(4.6 mm×250 mm,5μm),流动相为0.025 mol/L磷酸缓冲液-乙腈(pH 2.5)梯度洗脱,流速为1.0 mL/min。方法的检出限为0.01~0.037μg/mL,在0.2~20μg/ mL范围内峰面积与质量浓度成良好线性关系,相关系数大于0.998。在2、0.5、0.2μg/mL 3个添加水平下,回收率范围为69.2%~93.2%,精密度<12。方法灵敏,实用性强。  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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This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.  相似文献   

18.
<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of the  相似文献   

19.
《印刷工业》2014,(11):95-95
According to Printing and Printing Equipment Industries Association of China(PEIAC)'s statistics to the plate manufucturer in China, in 2013, the actual offset plate production has reached 346 million square meters in China. Among them, the CTP production volume was 245 million square meters, up by 11% than that of last year; the total sales of the CTP plate was 239 million square meters, up by 13%.  相似文献   

20.
《印刷工业》2014,(8):103-103
正Held at Guangdong Modern International Exhibition Center,Print China 2015 will cover 7exhibition halls,besides the original Hall No.3,4,5,6,7,the newly built F zone of Hall 3 will be used too.The total area will be140,000 square meters.Hall 3:Offset and large printing equipment,package printing equipment,post press  相似文献   

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