空心明胶胶囊中铬含量的快速测定

Rapid Determination of Chromium in Capsule Shells

通过对空心明胶胶囊进行热重分析确定样品马弗炉预处理温度为350℃,使用微波消解法,以7mL硝酸为消解试剂,实现在50mL小罐体下将空心明胶胶囊的消解。对消解液进行电感耦合等离子体-质谱法分析,以103Rh为内标,的到52Cr元素校准曲线方程为y=2.684x+5.121(R2=0.9995),方法的组内精密度0.86%,组间精密度为1.02%,回收率在97%—100%之间,显示方法稳定可靠;12批次实际样品检测表明本方法可以实现明胶胶囊中铬含量的检测,检出值均低于药典限定值2mg/kg,该方法快速、安全、可靠,能够满足实际工作需求。

Through the thermogravimetric analysis of capsule shells,the heat treatment method was decided to be 350℃ in muffle.Samples were prepared by microwave digestion with 7mL HNO3 after heat treatment,the method was proved to be availability for microwave systems with small vessel volume of 50mL.The solutions were determined by ICP-MS and the method was verified by precision,accuracy and real samples determination.The linear regression equation of 52Cr is y=2.684x＋5.121（R2=0.9995）with 103Rh as internal standard substance,the precision within groups and between groups of 52Cr are 0.86% and 1.02%,the recovery is 97%—100%.The method is proved to be convenient and reliable for determination of chromium in twelve batchs of capsule shell.