摘要
基于盐酸氨基葡萄糖(GSM)与镍(Ⅱ)在碱性介质中生成配合物,在波长219nm处有其最大吸收的现象作了进一步验证。将此反应用于紫外-可见分光光度法测定其药物胶囊中GSM含量。测定时,将一颗GSM胶囊中的药物颗粒取出称重后(每颗药物中GSM的质量的标示量为0.24g)溶于水中并定容至250mL。取此溶液5.00mL置于50mL容量瓶中,相继顺序加入0.10mol·L^-1氢氧化钠溶液10mL和1.0×10^-2 mol·L^-1硫酸镍溶液2.00mL,用0.10mol·L^-1氢氧化钠溶液定容,在20℃水浴中反应15min。在波长219nm处测量其吸光度。GSM的浓度在6.00×10^-4~4.00×10^-3 mol·L^-1内与其相应的吸光度呈线性关系,其检出限(3S/N)为4.10×10^-5 mol·L^-1。以GSM胶囊样品溶液为基体,按标准加入法在4个浓度水平上进行回收试验,测得回收率为80.0%~110%。测定值的相对标准偏差(n=5)均小于0.2%。按此方法对药物实样进行分析,测得其GSM浓度为7.26×10^-4 mol·L^-1,换算成胶囊中GSM的质量为0.2386g,与其标示值相符。
Based on the phenomenon of coordination of glucosamine hydrochloride(GSM)with Ni 2+in alkaline medium to form a coordination complex having its absorption maximum at 219nm,further research was done to work out a method for UV-spectrophotometric determination of GSM in its drug capsule.In the determination,the drug particles of GSM in a capsule were taken,weighed(ca.0.24g as labelled),dissolved and made its volume to 250mL with water.An aliquot of 5.00mL of this solution was taken and placed in a 50mL volumetric flask,10mL of 0.10mol·L^-1 sodium hydroxide solution and 2.00mL of 1.0×10^-2 mol·L^-1 nickel sulfate solution were added successively and volume of the solution was made up to 50mL with 0.10mol·L^-1 sodium hydroxide solution.Then the solution was placed into a water bath keeping at constant temperature of 20℃for 15min for completion of the coordination reaction.Absorbance of the solution was then measured at 219nm.Linear relationship between values of absorbance measured and the respective concentrations of GSM was obtained in the range from 6.00×10^-4 to 4.00×10^-3 mol·L^-1;the detection limit(3S/N)found was 4.10×10^-5 mol·L^-1.On the base of GSM taken from a capsule,recovery was tested by addition of GSM standard solution at 4 concentration levels,giving results of recovery in the range of 80.0%-110%and values of RSDs(n=5)less than 0.2%.A substantial drug capsule was analyzed by this method,the concentration of GSM found was 7.26×10^-4 mol·L^-1,which was equivalent to a mass of 0.2386g in the capsule by conversion calculation.This value was found in consistency with the labelled value.
作者
刘欣
王誉清
李咏歌
刘春雨
LIU Xin;WANG Yuqing;LI Yongge;LIU Chunyu(Department of Chemistry,Tangshan Teachers′College,Tangshan 063000,China;Department of Life Science,Tangshan Teachers′College,Tangshan 063000,China)
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2020年第3期340-343,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)