谷胱甘肽-铬-烟酸螯合物的制备与表征

Preparation and Characterization of Glutathiose-Cr3^(+)-Nicotinic Acid Chelate

以烟酸(NA)、谷胱甘肽(GSH)和CrCl3·6H2O为原料,制备高纯度GSH-Cr3+-NA2螯合物,分析影响合成螯合物的主要因素,获得最佳合成工艺,并对获得的螯合物进行表征,确定其螯合比例。结果表明,在Cr3+/NA/GSH(mol/mol/mol)=1∶2∶4,pH 5.0、温度60℃下反应3h,制备出Cr3+/NA/GSH(mol/mol/mol)=1∶2∶1的GSH-Cr3+-NA2螯合物;红外分析显示,与GSH相比,螯合物的-NH2、-NH-特征吸收峰发生蓝移,-NHC=O中-C=O的特征吸收峰红移,-SH的伸缩振动峰消失,说明GSH上的-NH-、NHC=O中-C=O、-SH均参与相互作用;与NA相比,螯合物的-C=O的伸缩振动峰发生红移,-OH的特征吸收峰消失了,说明NA上的-C=O和-OH参与相互作用。原子力显微镜形貌分析结果指出,由两分子NA和一分子GSH链围绕一Cr3+形成GSH-Cr3+-NA2螯合物。

The high purity GSH-Cr3+-NA2 chelate was prepared with CrCl3 ·6H2O,nicotinic acid and glutathione.The main factors that affect the synthesis of chelate were analyzed to get the best synthesis process,and characterization of obtained chelate to determine the proportion of its chelating.Experimental results showed that the GSHCr3+-NA2 chelate was obtained,of which molar ratio of Cr3+to NA and GSH was 1∶2∶1when the reaction continued for 3h,the Cr3+to NA and GSH was 1∶2∶4,pH was equal to 5.0and temperature was 60℃.Compared with GSH,the-NH2and-NH had a blue shift,the stretch vibration peak of-C=O had a red shift and the stretch vibration peak of-SH disappeared for chelate.These changes indicate that-NH、-C=O、-SH take part in coordination.Compared with NA,the stretch vibration peak of-C=O had a red shift and characteristic absorption peaks of-OH disappeared for chelate.The changes indicate that-C=O and-OH take part in coordination.AFM topography analysis results indicate that two molecules of NA and single molecule of GSH chain revolve about one Cr3+to form GSH-Cr3+-NA2 chelate.