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    电感耦合等离子体质谱法测定醋酸阿比特龙原料药中钯的残留量

    ICP-MS Determination of Residual Amount of Palladium in Zytiga Bulk Drugs

    • 摘要: 0.500 0 g醋酸阿比特龙原料药样品经5.0 mL硝酸和1.0 mL高氯酸微波消解后,加热至近干,将消解液用水定容至25 mL,采用电感耦合等离子体质谱法测定其中钯的残留量。采用带有碰撞反应池的氦调谐模式,以相对丰度较高、抗干扰更强的105Pd作为同位素,以115In作为内标。钯的线性范围在80.0 μg·L-1以内,检出限(3.3s/k)为0.020 8 μg·L-1。方法用于醋酸阿比特龙原料药样品的分析,测定值的相对标准偏差(n=6)为1.2%,加标回收率为94.0%~100%。

       

      Abstract: The sample (0.500 0 g) of Zytiga bulk drug was dissolved with 5.0 mL of HNO3 and 1.0 mL of HClO4 with microwave digestion. The above solution was heated to near dryness, and then the digestion solution was diluted to 25 mL with water. ICP-MS was applied to the determination of residual amount of palladium in the solution. He tuned mode with collision pool was used, and 105Pd with higher abundance and stronger anti-interference was used as isotope. 115In was used as internal standard. Linearity range of palladium was found in the range within 80.0 μg·L-1 with detection limit (3.3s/k) of 0.020 8 μg·L-1. The proposed method was applied to the analysis of the sample of Zytiga bulk drug, giving value of RSD (n=6) of 1.2%. Values of recovery found by standard addition method were in the range of 94.0%-100%.

       

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