自动消解-原子荧光法测定有机锗和总锗

Determination of Organic Germanium and Total Germanium Through Automatic Digestion and Fluorescence Spectrometry

以药材中有机锗和总锗为综合考察指标,利用GeCl_(4)沸点低的性质,设计程序使用全自动石墨消解仪对药材中有机锗和无机锗进行消解和分离,并采用原子荧光法检测药材中锗含量.结果表明,样品用质量分数为1%的HNO_(3)溶液处理后在50℃下振荡40 min,再将溶液倒入6 mol/L HCl溶液中于100℃下加热60 min,可实现无机锗和有机锗的分离.方法检出限为0.16μg/L,加标回收率为92.5%~104.0%,RSD为2.01%~3.77%,符合检测要求.

With organic germanium and total germanium as indexes in herbal medicine,and with the property of GeCl_(4)low boiling point,the organic germanium and inorganic germanium are separated and extracted by fully automated sample digestion system,and determined by atomic fluorescence spectrometry.We found that inorganic germanium could be extracted at 50℃,vibrating for 40 min in mass fraction of 1%HNO_(3).In 6 mol/L HCl heated at 100℃for 60 min,the inorganic germanium and organic germanium can be separated.The LOD of Ge was 0.16μg/L,the recoveries of germanium was 92.5%~104.0%,and the RSD was 2.01%~3.77%,which accords with the demand of analysis.