资源描述:
《辛烯基琥珀酸菊粉酯的制备及其结构分析》由会员上传分享,免费在线阅读,更多相关内容在学术论文-天天文库。
1、现代食品科技ModernFoodScienceandTechnology2014,Vol.30,No.8辛烯基琥珀酸菊粉酯的制备及其结构分析张晓云,闫晓静,施金,朱益,郑焰,丁文慧(江苏大学食品与生物工程学院,江苏镇江212013)摘要:以取代度(DS)为指标,利用单因素试验研究了菊粉浓度、反应温度、pH值、OSA添加量等因素对制备辛烯基琥珀酸菊粉酯的影响,通过正交试验确定了适宜制备工艺条件为:菊粉浓度为25%,OSA/AFU摩尔比为0.35,pH8.5~9.0,反应温度30℃,13在该工艺条件下所得产品取代度为0.0342。对制备产品的结构采用扫描电镜(SEM)、红外光
2、谱仪(FT-IR)、核磁共振光谱仪(CNMR1和HNMR)等进行表征分析,结果表明:菊粉经过辛烯基琥珀酸酐(OSA)修饰后,其颗粒表面受到侵蚀,出现凹槽、破损孔纹。-1-1红外光谱图显示菊粉酯化后在1733.72cm、1569.80cm处分别出现酯键中羰基(C=O)振动和OSA上的烯基(C=C)伸缩振动的13特征吸收峰。CNMR谱图中在化学位移175.6ppm和176.5ppm处出现羰基碳和羧基碳的特征峰;1HNMR谱图中在化学位移1.2ppm、0.8ppm附近出现OSA分子亚甲基和甲基质子峰。这均证实了OSA基团以酯键形式连接到菊粉分子上。关键词:辛烯基琥珀酸菊粉酯;制
3、备;扫描电镜;核磁共振光谱仪;结构特征文章篇号:1673-9078(2014)8-125-130PreparationandStructuralCharacterizationofOctenylSuccinicAnhydrideModifiedInulinZHANGXiao-yun,YANXiao-jing,SHIJin,ZHUYi,ZHENGYan,DINGWen-hui(SchoolofFoodandBiologicalEngineering,JiangsuUniversity,Zhenjiang212013,China)Abstract:Thepreparation
4、ofoctenylsuccinicanhydrid(OSA)modifiedinulininaqueousmediumwasstudied.Theeffectsoftheinulinconcentration,reactiontemperature,pHvalue,theadditiveamountofOSAwereinvestigatedbysinglefactorexperimentswiththedegreeofsubstitution(DS)asmeasurementindex.ThesyntheticconditionsofOSAmodifiedinulinwh
5、ichwereoptimizedbyorthogonalanalysiswereasfollows:OSA/AFUmolarratioof0.35,temperature30℃,pH8.5~9.0,25%(m/m)concentrationofinulin.Thestructuresoftheproductweredeterminedbymeansofscanningelectronmicroscopy(SEM),fouriertransforminfraredspectroscopy(FT-IR),carbon-13andprotonnuclear131magnetic
6、resonancespectroscopy(CNMRandHNMR).TheresultsshowedthatthesurfacestructureofOSAmodifiedinulinparticlesweredamagedandlosttheiroriginalsmoothsurfacestructure.Infrareddatasshowedthatcarbonylabsorptionpeakofesterbondappearedat1733.72-1-1cmandalkenylabsorptionpeakofoctenylsuccinicanhydrideappe
7、aredat1569.80cm.Characteristicabsorptionpeaksofthecarbonylcarbon13andcarboxylcarbonwereappearedat175.6ppmand176.5ppmintheCNMRdiagram.Theabsorptionpeaksofmethyleneprotonsand1methylprotonsinthechainofOSAmoleculewerediscoveredabout1.2ppm,0.8ppmchemicalshiftintheHNMRdia