摘要
目的:建立替格瑞洛原料药中的基因毒性杂质盐酸羟胺的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法:采用反相色谱,以水-乙腈(0.1%甲酸)为流动相,梯度洗脱,流速0.3 mL·min^(-1),以ESI正离子多反应监测(MRM)模式进行检测。结果:盐酸羟胺的检测限和定量限可分别达到0.2和0.4 ng·mL^(-1),在线性范围内有良好的线性关系(r=0.9987),准确度实验低、中、高浓度回收率均在95.1%~109.2%,RSD为2.2%~6.4%,重复性实验6份加标样品溶液回收率的RSD为5.7%。在3批次替格瑞洛原料药中均未检出盐酸羟胺。结论:该方法可用于检测替格瑞洛中的盐酸羟胺。
Objective:To establish an HPLC-MS/MS detection method of hydroxylamine hydrochloride in Ticagrelor API.Methods:Hydroxylamine hydrochloride and API sample were separated by reverse chromatography,with water-acetonitrile(0.1%formic acid)as mobile phase using gradient elution at a flow rate of 0.3 mL·min^(-1).Mass was performed with multi-reaction monitoring(MRM)in positive ESI mode.Results:The detection and quantitative limits of hydroxylamine hydrochloride reached 0.2,0.4 ng·mL^(-1),respectively,and good linear relationship(r=0.9987)was acquired.The recoveries of low,medium and high level in the accuracy experiment ranged from 95.1%to 109.2%,with RSD of 2.2%~6.4%.The RSD of the recovery of 6 spiked sample solution was 5.7%for the repeatability experiment.No hydroxylamine hydrochloride was detected in 3 batches of Ticagrelor API.Conclusion:The method can be used to detect hydroxylamine hydrochloride in Ticagrelor.
作者
樊华军
FAN Hua-jun(ICAS Testing Technology Service(Shanghai)Co.,Ltd.,Shanghai 201100,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2022年第4期709-713,共5页
Chinese Journal of Pharmaceutical Analysis
