浏览全部资源
扫码关注微信
纸质出版日期:2021,
扫 描 看 全 文
赵钰馨, 孙秉喆, 倪卫星, 等. 阿嗪米特中潜在基因毒性杂质马来酰肼的含量测定[J]. 中国药房, 2021,32(18).
ZHAO Yuxin, SUN Bingzhe, NI Weixing, et al. Content Determination of Potential Genotoxic Impurity Maleic Hydrazide in Azintamide[J]. China Pharmacy, 2021,32(18).
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。
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.
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
Maleic hydrazideAzintamideHPLC-FLDGenotoxic impurity
0
浏览量
7
下载量
0
CSCD
关联资源
相关文章
相关作者
相关机构