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目的:建立石墨炉原子吸收光谱法测定中草药中痕量元素锗的含量。方法:通过程序控温、控压的分步微波消化方式消化样品,优化石墨炉升温程序,采用Ni(NO3)2为基体改进剂,以氘灯扣除背景,在265.2nm波长下对中草药中痕量元素锗进行测定。结果:在选定分析条件下,锗的检出限为0.46μg.L-1,RSD分别为1.8%～2.8%,回收率为92.5%～103.4%。结论:该方法利用基体改进剂稳定锗,减少了测定时锗的挥发损失;再加上优化的石墨炉升温程序,测定结果准确、可靠。
Objective: To establish a method for the determination of trace element germanium in Chinese herbal medicine by graphite furnace atomic absorption spectrometry. Methods: Samples were digested by temperature-controlled and pressure-controlled step-by-step microwave digestion to optimize the temperature program of graphite furnace. Ni (NO3) 2 was used as the matrix modifier and deuterium lamp was used to deduct the background. The amount of elemental germanium was measured. Results: Under the selected conditions, the detection limit of germanium was 0.46μg.L-1, RSD was 1.8% -2.8%, the recovery was 92.5% -103.4%. Conclusion: This method uses matrix modifier to stabilize germanium and reduces the volatilization loss of germanium during the measurement. In addition, with the optimized program of graphite furnace heating, the determination result is accurate and reliable.