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1.
目的通过在线净化/固相萃取-高效液相色谱技术建立测定柑橘中痕量多菌灵的方法。方法 样品在固相萃取小柱Cyclone-MCX中进行净化和富集后,通过阀将固相萃取小柱切换至分析流路,使待测物从富集柱冲洗至分析柱PAⅡC18中,采用梯度洗脱方式完成多菌灵的分离和检测。结果 多菌灵在1~20μg/L范围内呈线性相关,线性方程为Y=0.0921X-0.0016,相关系数r=0.9995;检出限为0.1μg/L(S/N=3);柑橘中3个水平添加回收率(n=6)在86.5%~96.7%;6次加标回收相对标准偏差为2.34%~3.21%。结论 所建方法简便、快速、准确、重现性好,能够满足柑橘中多菌灵痕量残留量的测定。  相似文献   

2.
建立了固相萃取-高效液相色谱同时测定果蔬中吡虫啉和多菌灵含量的方法。试样用乙腈提取,经Cleanert-NH2固相萃取小柱净化,流动相定容后,采用高效液相色谱法测定。以甲醇-水(32∶68)为流动相,流速1.0 m L/min,于270 nm波长下检测。结果表明,吡虫啉和多菌灵分别在0.02μg/m L~1.0μg/m L和0.05μg/m L~5.0μg/m L范围内线性良好,相关系数均0.999 9以上;回收率在85.1%~100.5%之间,相对标准偏差为1.6%~6.6%(n=6)。该方法简便、高效,适用于果蔬中吡虫啉和多菌灵含量的同时测定。  相似文献   

3.
黄锋 《饮料工业》2009,12(12):32-34
基于固相萃取分离技术结合分光光度法,建立了一种测定水中痕量磷酸盐的分析方法。磷钼蓝(PMB)与十六烷基三甲基溴化铵(CTMAB)可生成疏水性的PMB-CTMAB离子缔合物,被Sep-Pak C18固相萃取小柱富集,用丙酮和硫酸混合液洗脱以后用分光光度法测定,固相萃取柱不被破坏且可重新处理使用。同时研究了固相萃取条件,讨论了共存离子的干扰及消除。该方法测定饮用水中痕量磷酸盐含量灵敏度高,选择性好,检测限为0.14μg/L(n=7),其相对标准偏差RSD为3.1%~6.7%(n=7),标准加入回收率为95%~102%,其结果令人满意。  相似文献   

4.
李志刚 《纺织学报》2015,36(5):69-73
采用液相色谱/质谱联用法测定由Fenton法降解含偶氮染料的印染废水中的痕量苯胺。降解反应溶液中的苯胺通过HLB固相萃取小柱净化、富集后,在XR-ODS II 柱上,以乙腈/5 mmol/L乙酸铵+0.05%甲酸为流动相进行梯度洗脱,采用电喷雾(ESI)电离正离子多反应监测模式(MRM)测定。结果表明,实验采用的固相萃取小柱能有效地去除溶液中的Fe2+和干扰苯胺测定的化合物,苯胺在10.0–1000.0 μg/L范围内具有良好的线性,相关系数0.9993,回收率在93.0%–98.8% 范围,日内相对标准偏差(RSDs)在3.2%–6.9%之间,日间RSDs在4.8%–6.3%之间,最低定量检出限为2.0 μg/L。建立的方法简便、干扰少、特异性强,应用此法测定Fenton反应液中的痕量苯胺取得了满意的结果。  相似文献   

5.
为稳定可靠地分析油茶籽油中多环芳烃,建立了分子印迹固相萃取-气相色谱-串联质谱测定油茶籽油中16种多环芳烃方法。样品经正己烷溶解后,分别采用反相固相萃取HLB小柱、弗罗里硅土小柱和分子印迹固相萃取小柱对16种多环芳烃进行净化。以回收率和基质效应为考察指标评估3种固相萃取柱的净化,在此基础上,对净化液进行低温低速氮吹浓缩,多反应监测扫描模式下进行气相色谱-串联质谱检测,外标法定量。结果表明:分子印迹固相萃取小柱对16种多环芳烃的净化效果最佳;16种多环芳烃在质量浓度1~50μg/L范围内线性关系良好(R2≥0.995 1),检出限为0.01~0.20μg/kg,在2、10μg/kg和20μg/kg加标水平下的回收率为71.5%~116.3%,相对标准偏差为1.5%~13.8%。该方法具有灵敏度高、检出限低、重复性好等特点,适用于油茶籽油中16种多环烃的测定。  相似文献   

6.
建立高效液相色谱-串联质谱法同时测定大米中敌瘟磷、莠去津和多菌灵的方法。大米采用C18固相萃取小柱净化,以C18色谱柱为分离柱,以水-乙腈为流动相进行梯度洗脱,用高效液相色谱-串联质谱,电喷雾电离,多反应监测模式检测,外标法同时定量测定敌瘟磷、莠去津和多菌灵。该方法的线性范围敌瘟磷、莠去津、多菌灵2~200ng/ml,线性相关系数均≥0.999,检出限为4μg/kg,定量限10μg/kg;平均加标回收率61.7%~90.2%;相对标准偏差均小于8.0%。该方法可应用于同时定量检测大米中敌瘟磷、莠去津和多菌灵,操作简单、快速、准确可靠。  相似文献   

7.
目的 基于全自动固相萃取-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mss spectrometry ,UPLC-MS/MS)建立果酒中14种有机酸的检测方法。方法 采用MAX固相萃取小柱净化,Agilent Eclipse Plus RRHD C18柱(3.0 mm×150 mm,1.8 μm)分离,0.4%甲酸溶液-乙腈为流动相梯度洗脱,电喷雾离子源负离子(ESI-)模式下,结合动态多反应监测模式,外标法定量。结果 14种有机酸在各自的线性范围内相关系数均大于0.991,方法的检出限为0.7~50 μg/L ,方法的定量限为2~150 μg/L,回收率为82.6%~117.1% ,相对标准偏差为0.6%~8.7%(n=6)。结论:该方法操作简单,灵敏,重现性好,适用于果酒中有机酸的定性定量测定。  相似文献   

8.
建立了分子印迹固相萃取-高效液相色谱法测定果汁中展青霉素的方法。浓缩果汁样品经酶解,乙酸-水溶液稀释,分子印迹固相萃取小柱净化后(澄清果汁样品经乙酸-水溶液稀释后,直接进行SPE净化),以Waters XSELECT HSS T3色谱柱为分离柱,以水和乙腈作为流动相,二极管阵列检测器高效液相色谱进行检测,外标法定量。展青霉素在20~1000μg/L质量浓度范围内线性关系良好,相关系数为0.9994,方法的定量限为10.0μg/kg;添加水平为10.0、20.0μg/kg和40.0μg/kg时,加标回收率为83.0%~91.5%,相对标准偏差为2.8%~7.6%。结果表明:该方法准确、高效、特异性好、重现性高,适用于果汁中展青霉素的测定。  相似文献   

9.
建立一种用高效液相色谱-PDA检测法测定运动饮料中甜菊糖苷的检测方法。样品前处理采用硅胶固相萃取小柱进行富集和净化,氮气吹干后用流动相复溶上机检测。采用Waters RP C18色谱柱(4.6 mm×250 mm,5μm)分离,以乙腈∶水=30∶70(体积比)作为流动相,用PDA检测器检测,外标法峰面积定量。结果表明,9种甜菊糖苷组分在20.0μg/m L~200.00μg/m L浓度范围内线性良好,相关系数r2为0.991~0.999,检出限在1.0μg/m L~3.0μg/m L,定量限为3.0μg/m L~9.0μg/m L,加标回收率达到81.4%~90.5%。  相似文献   

10.
采用固相萃取-高效液相色谱法对保健品中的枸橼酸西地那非进行测定。样品经Strata X-C固相萃取小柱净化,用Phenomenex Kinetex C18柱分离,乙腈-10mM醋酸铵(V/V=35/65)为流动相,经液相色谱检测。结果表明,枸橼酸西地那非在0.5~80μg/mL的浓度范围之间具有良好的线性关系(R2=0.9995),加标回收率大于90%。该方法简单,快速,精密度和准确度高,适用于保健品中枸橼酸西地那非的测定。  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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