电感耦合等离子体发射光谱法同时测定奥贝胆酸中硼和钯的含量

Determination of B and Pd in obeticholic acid by ICP-AES

建立电感耦合等离子体发射光谱法同时测定奥贝胆酸中硼和钯含量的方法。奥贝胆酸样品经过微波消解处理后,采用电感耦合等离子体发射光谱法测定。通过实验确定硼的分析谱线为249.77 nm,钯的分析谱线为340.46 nm。方法学验证的结果表明,测定奥贝胆酸中硼和钯的检出限分别为0.02 mg/kg和0.09 mg/kg,线性良好,相关系数分别为0.999 9和0.999 8,RSD分别为0.68%和0.52%,加标回收率分别为100.7%~110.6%和96.7%~110.6%。该方法简化样品的前处理过程,具有快速、准确、灵敏度高及两种元素可同时测定的优点,可用于奥贝胆酸样品中残留硼和钯的测定。

This work proposed an ICP-AES method for simultaneous determination of trace amounts of B and Pd in obeticholic acid. The obeticholic acid was treated by microwave digestion,the B and Pd were analyzed by inductively coupled plasma atomic emission spectrometry. The analysis spectral lines of B and Pb were respectively determined by experiments,249.77nm for B and 340.46nm for Pb. The limit of detection was 0.02 mg/kg and 0.09 mg/kg. The method had a good linear correlation,with the correlation coefficient being 0.9999 and 0.9998 for B and Pd determination in obeticholic acid. The relative standard deviation was 0.68% and 0.52%, and recovery rate was100.7%-110.6% and 96.7%-110.6%. This method was proved to be rapid,accurate and reliable with high efficiency and multi elements analysis. It is suitable for the detection of B and Pd inobeticholic acid.