石墨炉原子吸收光谱法测定阿法替尼中镍的残留量

Determination of residual nickel in afatinib by graphite furnace atomic absorption spectrometry

目的建立微波消解-石墨炉原子吸收光谱法测定阿法替尼中镍残留量的方法。方法采用MARS 6微波消解仪和HNO3消化体系设置快速彻底消化样品,采用Zeenit650P石墨炉原子吸收光谱仪建立了阿法替尼中镍的残留量分析方法。结果镍含量在0.01μg/ml^0.10μg/ml时具有良好的线性关系,其相关系数(r)为0.998 6。仪器检出限与定量限分别为0.001 7μg/ml和0.005 7μg/ml。称样量在0.25 g时,该方法检出限为0.068 mg/kg,定量限为0.228 mg/kg。相对标准偏差为1.76%~7.10%,回收率为91.2%~107.0%。结论该法灵敏度高、干扰少,具有较强实用性,便于推广应用。

Objective To establish a method for the determination of residual nickel in afatinib with microwave digestion-graphite furnace atomic absorption spectrometry. Methods After the procedure set by MARS 6 microwave digestion instrument and HNO3 in digestive system,the samples were analyzed for the detection of residual nickel by Zeenit650 P graphite furnace atomic absorption spectrometry. Results The calibration curve was linear when the concentration of nickel was among 0. 01 μg / ml-0. 10 μg / ml（ r = 0. 998 6）. The limit of detection was 0. 001 7 μg / ml,and the limit of quantification was 0. 005 7 μg / ml. LOD and LOQ of the method was 0. 068 mg / kg and 0. 228 mg / kg when the sample weight was 0. 25 g. Recoveries of spiked samples were among 91. 2%- 107. 0% with RSD of 1. 76%- 7. 10%）. Conclusion This method is of high sensitivity,less interference,strong practicability,convenient popularization and application.