气相色谱-质谱联用法用于测定盐酸普罗帕酮原料药中基因毒性杂质环氧氯丙烷的可行性
Feasibility of Using Gas Chromatography-mass Spectrometry to Determine the Genotoxic Impurity Epichlorohydrin in Propafenone Hydrochloride Raw Material
付金凤 1蒋晓勤1
作者信息
- 1. 常州市食品药品纤维质量监督检验中心,江苏常州 213101
- 折叠
摘要
目的 探讨气相色谱-质谱联用法(GC-MS)测定盐酸普罗帕酮原料药中基因毒性杂质环氧氯丙烷的可行性.方法 选用VF-624 ms(Agilent,30 m×0.25 mm,1.4 μm)毛细管色谱柱,以高纯氦为载气,柱流量为1.5 ml/min,分流比为5∶1,程序升温法;离子源温度为230℃,接口温度260℃,溶剂延迟时间2.0 min;选择离子监测(SIM),定量离子质荷比(m/z)为57.结果 环氧氯丙烷在4～128 ng/ml范围内线性关系良好,相关系数为0.9998;检测限为0.4 ng/ml;定量限为1.1 ng/ml;进样精密度的相对标准偏差(RSD)值为 1.9%;低、中、高 3 个浓度水平平均加样回收率为 88%～95%.结论 该方法简便高效,专属性好,灵敏度高,实用性强,适用于测定盐酸普罗帕酮中环氧氯丙烷的残留量.
Abstract
Objective To explore the feasibility of using gas chromatography-mass spectrometry(GC-MS)to determine the genotoxic impurity epichlorohydrin(ECH)in propafenone hydrochloride raw material.Methods The ECH was detected by VF-624 ms capillary column(Agilent,30 m×0.25 mm×1.4 μm)with temperature program,high purity helium as carrier gas.The flow rate was 1.5 ml/min,and the split ratio was 5∶1.The ion source temperatrue was 230℃and the inlet temperature was 260℃.Solvent delay time was 2.0 min.Selected ion monitoring was used to detect the quantitative ion(m/z 57).Results The linear calibration curves of ECH was obtained over the range of 4～128 ng/ml,the correlation coefficients was 0.9998.The limit of detection was 0.4 ng/ml,and the limit of quantitation was 1.1 ng/ml.The RSD of injection precision was 1.9%.The average recoveries at three spiked levels ranged from 88%to 95%.Conclusion The present method is simple and efficient,and proved to be specific,sensitive and practical.It is suitable for the residue quantity of ECH in propafenone hydrochloride.
关键词
盐酸普罗帕酮/环氧氯丙烷/气相色谱-质谱联用法Key words
Propafenone hydrochloride/Epichlorohydrin/Gas chromatography-mass spectrometry引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据