文献读书报告.ppt

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1、Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee beanAnalytica Chimica ActaImpact Factor:4.517lPhloxine Ban insecticide gastric toxicity and cell toxicity detect：HPLC CZE SPElMI

2、Ps high selectivity and specific recognition physicochemical stability and applicabilityIntroductionMISPE MISPE monolithic column higher chemical stability,selectivity more facile preparation Preparation:in situ polymerization using nanostructured imprinted materialsGOGO-MIPs higher loading capacity

3、 faster association/dissociation kinetics improving the accessibility and sensitivity to target species Preparation of the GO-MISPE monolithic capillary columnGOporogenmethanol toluene dodecanol 30minultrasonicationphloxine B(template)MAA(functional monomer)mechanically stirred 1h,room temperatureED

4、MA(crosslinker)AIBN(initiator)purged with N2 fill 5min(capillary tube)polymerization,5h60 oC in a water-bath wash甲醇甲醇-乙酸乙酸(90:10,v/v)washmethanolthe GO-MISPE monolithic capillary columnPreparation of the GO-MISPE monolithic capillary columnThe correspondingnGO-NIPs monolithic capillary column-withou

5、t template nMIPs monolithic capillary column-without GOPreparation of phloxine B coffee bean samplesuThe sample solutions咖啡豆研磨后过 20 目筛，转移至广口瓶于5 0C保存。咖啡豆粉末(1.0 g)2.0mL 甲醇萃取 离心phloxine B 标准溶液 超声15 min 10,000 rpm,10 min重复两次。萃取液合并，用甲醇稀释至4.0 mL。溶液过0.45m滤膜备用。加标浓度为1.0 和20 ng/mLuthe GO-MISPE monolithic capi

6、llary column1.分别用100l甲醇和水活化活化活化2.样品溶液以0.02ml/min流速通过毛细管整体柱进样进样3.用40l甲苯以0.02ml/min流速洗涤去除杂质去除杂质4.用40l 甲醇-乙酸(90:10,v/v)0.1 mL/min洗脱洗脱洗脱收集洗脱液，氮气吹干，残留物溶解于0.2ml甲醇 HPLCLIFProcedure for determination of phloxine B coffee bean samplesFig.1.The chemical structure of phloxine B.Results and discussionFig.2.SEM

7、images of(a)the column prepared with AM,(b)the column prepared with MAA,(c)MIPs,(d)GO-MIPs and(e)the magnification is 20,000 folds for dSynthesis and morphologyFig.3.FT-IR spectra of(a)GO and(b)GO-MIPs.methanoltoluenedodecanol permeable,the flow rate of 0.15 ml/min toluene and dodecanol 3040%keep th

8、e pore size voidless structure Methanol augmented the solubility of GO and phloxine BporogenT:M:CCapacity of the columnFig.4.Breakthrough curves of phloxine B on GO-NIPs,MIPs and GO-MIPs columnand breakthrough curves of rose bengal on GO-MIPs column.Loading concentration:1.0mg/mL;Sample flow rate:0.

9、02 mL/mincapacity0.006g/mg0.029g/mg0.040g/mg0.012g/mgSelection of eluent and washing solventMethod validationA=1.620107C+262792 over 0.0012.0mg/mL R2=0.9995the method had good precision even at low concentrationsLOD=0.075 ng/mL(S/N=3);LOQ=0.25 ng/mL(S/N=10)LOD(0.3 ng/g)HPLC(7.5 ng/g)and CZE(10 ng/g)

10、coupled with traditional SPE this method was more sensitiveEnrichments and impurity removalFig.5.Illustrative chromatograms for the sample enrichment and impurities removal.(a)1.0 ng/mL.phloxine B sample before loaded onto the column and(b)1.0 ng/mL.phloxine B sample after loaded onto the column.Con

11、clusionIn summary,a novel phloxine B molecularly imprinted monolithic capillary column was prepared using GO as the support matrix.GO-MIPs presented higher capacity and affinity than those of traditional MIPs.The GO-MISPE monolithic capillary column as extraction approach was used for effectively extracting phloxine B from coffee bean and showed good selectivity and affinity for phloxine B while being capable of enrichment and impurity removing.谢谢