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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 bean,Analytica Chimica Acta,Impact Factor:4.517,Phloxine Ban insecticide gastric toxicity and cell toxicity detect：HPLC CZE SPE
2、MIPs high selectivity and specific recognition physicochemical stability and applicability,Introduction,MISPE,MISPE monolithic column higher chemical stability,selectivity more facile preparation Preparation:in situ polymerization using nanostructured imprinted materialsGOGO-MIPs higher loading capa
3、city faster association/dissociation kinetics improving the accessibility and sensitivity to target species,Preparation of the GO-MISPE monolithic capillary column,GO,porogenmethanol toluene dodecanol,30min,ultrasonication,phloxine B(template)MAA(functional monomer),mechanically stirred 1h,room temp
4、erature,EDMA(crosslinker)AIBN(initiator),purged with N2 fill 5min,(capillary tube),polymerization,5h60 oC in a water-bath,wash甲醇-乙酸(90:10,v/v),washmethanol,the GO-MISPE monolithic capillary column,Preparation of the GO-MISPE monolithic capillary column,The correspondingGO-NIPs monolithic capillary c
5、olumn-without template MIPs monolithic capillary column-without GO,Preparation of phloxine B coffee bean samples,The 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/mL,the GO-MISPE mon
6、olithic capillary column1.分别用100l甲醇和水活化活化2.样品溶液以0.02ml/min流速通过毛细管整体柱进样3.用40l甲苯以0.02ml/min流速洗涤去除杂质4.用40l 甲醇-乙酸(90:10,v/v)0.1 mL/min洗脱洗脱收集洗脱液，氮气吹干，残留物溶解于0.2ml甲醇 HPLCLIF,Procedure for determination of phloxine B coffee bean samples,Fig.1.The chemical structure of phloxine B.,Results and discussion,Fig.
7、2.SEM 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 d,Synthesis and morphology,Fig.3.FT-IR spectra of(a)GO and(b)GO-MIPs.,methanoltoluenedodecanol permeable,the flow rate of 0.15 ml/min toluene and dodecanol 304
8、0%keep the pore size voidless structure Methanol augmented the solubility of GO and phloxine B,porogen,T:M:C,Capacity of the column,Fig.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
9、 flow rate:0.02 mL/min,capacity,0.006g/mg0.029g/mg0.040g/mg0.012g/mg,Selection of eluent and washing solvent,Method validation,A=1.620107C+262792 over 0.0012.0mg/mL R2=0.9995,the 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
10、/g)and CZE(10 ng/g)coupled with traditional SPE this method was more sensitive,Enrichments and impurity removal,Fig.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 loade
11、d onto the column.,Conclusion,In 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,
