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阿嗪米特中潜在基因毒性杂质马来酰肼的含量测定
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| 篇名： | 阿嗪米特中潜在基因毒性杂质马来酰肼的含量测定 |
| TITLE： | Content Determination of Potential Genotoxic Impurity Maleic Hydrazide in Azintamide |
| 摘要： | 目的：建立阿嗪米特原料药中潜在基因毒性杂质马来酰肼含量测定的方法。方法：采用高效液相色谱-荧光检测器法。以ThermoSyncronisC18为色谱柱，以0.2mol/L乙酸溶液-甲醇为流动相进行梯度洗脱；柱温为30℃；激发波长为315nm，发射波长为389nm；流速为1mL/min；进样量为20μL。结果：空白溶剂和阿嗪米特均不干扰马来酰肼的测定；马来酰肼检测质量浓度的线性范围为19.5～300ng/mL（r＝0.9999）；检测限为4.5ng/mL，定量限为19.5ng/mL；加样回收率为98.79％～103.76％（RSD均小于3.00％，n＝9）；精密度、稳定性（24h）试验的RSD均不大于5.63％，且耐用性试验的RSD均小于2.00％（n＝6）。3批阿嗪米特原料药中均未检出马来酰肼。结论：该方法专属性好、灵敏度高、定量准确，可用于阿嗪米特或其他基质中马来酰肼的痕量测定。 |
| ABSTRACT： | OBJECTIVE：To establish a method for the content determination of potential genotoxic impurity maleic hydrazide in azintamide raw material. METHODS ：HPLC-FLD method was adopted. The determination was performed on Thermo Syncronis C18 column with mobile phase consisted of 0.2 mol/L acetic acid-methanol （gradient elution ）. The column temperature was set at 30 ℃，the excitation wavelength was 315 nm and emission wavelength was 389 nm. The flow rate was 1 mL/min，and the sample size was 20 μL. RESULTS：The blank solvent and azintamide did not interfere with the determination of maleic hydrazide. The linear range of maleic hydrazide was 19.5-300 ng/mL（r＝0.999 9）. The limit of detection was 4.5 ng/mL and the limit of quantification was 19.5 ng/mL. The recovery ranged from 98.79％ to 103.76％（RSDs were lower than 3.00％，n＝9）. RSDs of precision and stability （24 h）tests were no more than 5.63％，and those of durability tests were less than 2.00％（n＝6）. Maleic hydrazide was not detected in 3 batches of azinamide raw material. CONCLUSIONS ：The method is specific ，sensitive and accurate. It can be used for the trace determination of maleic hydrazide in azintamide or other matrix. |
| 期刊： | 2021年第32卷第18期 |
| 作者： | 赵钰馨，孙秉喆，倪卫星，梁然植，狄斌，苏梦翔 |
| AUTHORS： | ZHAO Yuxin，SUN Bingzhe ，NI Weixing ，LIANG Ranzhi ，DI Bin，SU Mengxiang |
| 关键字： | 马来酰肼；阿嗪米特原料药；高效液相色谱-荧光检测器法；基因毒性杂质 |
| KEYWORDS： | Maleic hydrazide ；Azintamide；HPLC-FLD；Genotoxic impurity |
| 阅读数： | 204 次 |
| 本月下载数： | 7 次 |
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