Covalent organic nanospheres(CONs)were explored as a fiber coating for solid-phase microextraction of genotoxic impurities(GTIs)from active ingredients(AIs).CONs were synthesized by an easy solution-phase procedure at 25℃.The obtained nanospheres exhibited a high specific surface area,good ther-mostability,high acid and alkali resistance,and favorable crystallinity and porosity.Two types of GTIs,alkyl halides(1-iodooctane,1-chlorobenzene,1-bromododecane,1,2-dichlorobenzene,1-bromooctane,1-chlorohexane,and 1,8-dibromooctane)and sulfonate esters(methyl p-toluenesulfonate and ethyl p-toluenesulfonate),were chosen as target molecules for assessing the performance of the coating.The prepared coating achieved high enhancement factors(5097-9799)for the selected GTIs.The strong affinity between CONs and GTIs was tentatively attributed to T-T and hydrophobicity interactions,large surface area of the CONs,and size-matching of the materials.Combined with gas chromatography-mass spectrometry(GC-MS),the established analytical method detected the GTIs in capecitabine and imatinib mesylate samples over a wide linear range(0.2-200 ng/g)with a low detection limit(0.04-2.0 ng/g),satisfactory recovery(80.03％-109.5％),and high repeatability(6.20％-14.8％)and reproducibility(6.20％-14.1％).Therefore,the CON-coated fibers are promising alternatives for the sensitive detection of GTIs in AI samples.

Yanfang Zhao;Jingkun Li;Hanyi Xie;Huijuan Li;Xiangfeng Chen

School of Pharmaceutical Sciences,Qilu University of Technology(Shandong Academy of Sciences),Jinan,250014,China;Shandong Analysis and Test Center,Qilu University of Technology(Shandong Academy of Sciences),Jinan,250014,China

药物分析学报（英文）

[1]Yanfang Zhao;Jingkun Li;Hanyi Xie;Huijuan Li;Xiangfeng Chen-.Covalent organic nanospheres as a fiber coating for solid-phase microextraction of genotoxic impurities followed by analysis using GC-MS)[J].药物分析学报（英文）,2022(04):583-589

CONs,GTIs,AIs,mostability,iodooctane,bromododecane,dichlorobenzene,bromooctane,chlorohexane,dibromooctane,toluenesulfonate

Covalent,organic,nanospheres,coating,solid,phase,microextraction,genotoxic,impurities,followed,by,analysis,using,were,explored,from,active,ingredients,synthesized,easy,solution,procedure,obtained,exhibited,high,specific,surface,area,good,ther,acid,alkali,resistance,favorable,crystallinity,porosity,Two,types,alkyl,halides,esters,methyl,chosen,target,molecules,assessing,performance,prepared,achieved,enhancement,factors,selected,strong,affinity,between,was,tentatively,attributed,hydrophobicity,interactions,large,matching,materials,Combined,gas,chromatography,mass,spectrometry,established,analytical,method,detected,capecitabine,imatinib,mesylate,samples,wide,linear,range,detection,limit,satisfactory,recovery,repeatability,reproducibility,Therefore,coated,fibers,promising,alternatives,sensitive

0.484335