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,1.4μm)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0.999 8;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。
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 0.999 8.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.
作者
付金凤
蒋晓勤
FU Jin-Feng;JIANG Xiao-Qin(Changzhou Center For Food,Drug And Fiber Quality Supervision And Inspection,Changzhou 213101,China)
出处
《中国药物经济学》
2024年第2期104-106,111,共4页
China Journal of Pharmaceutical Economics
关键词
盐酸普罗帕酮
环氧氯丙烷
气相色谱-质谱联用法
Propafenone hydrochloride
Epichlorohydrin
Gas chromatography-mass spectrometry
