气相色谱-质谱联用测定盐酸多奈哌齐片中基因毒性杂质溴化苄的含量
Determination of Benzyl Bromide in Donepezil Hydrochloride Tablets by GC-MS
赵峰园 1杨艳芳 1许晓蒙 1侯亚平 1石燕丽 1刘双双 1刘志通 1马玉峰 2刘苗苗1
作者信息
- 1. 山东丹红制药有限公司,山东菏泽 274000
- 2. 山东步长制药股份有限公司,山东菏泽 274000
- 折叠
摘要
目的 建立气相色谱-质谱联用法测定盐酸多奈哌齐片中基因毒性杂质溴化苄的含量.方法 采用6%氰丙基苯-94%二甲基硅氧烷(Agilent DB-624,60 m×0.25 mm,1.40 μm)色谱柱,程序升温,进样口温度:210℃,进样体积:1 μl,色谱柱流量:1.1 ml/min.质谱条件:EI源,离子源温度220 C;溶剂延时:8.0 min,电子能量:70 eV.结果 溴化苄浓度在 10.11～505.48 ng/ml 范围内,线性关系良好(r2＞0.99).加样回收率(n=3)的范围为 86.53%～111.66%,检测限为3.03 ng/ml,定量限为10.11 ng/ml.结论 本方法专属性较强,灵敏度高,稳定性好,可准确对盐酸多奈哌齐片中基因毒性杂质溴化苄进行定量,为盐酸多奈哌齐片中基因毒性杂质溴化苄的含量检测提供了方法支持.
Abstract
Objective To establish a GC-MS method for the determination of benzyl bromide in Donepezil Hydrochloride Tablets.Methods An Agilent DB-624(6%cyanide propylbenzene-94%dimethylsiloxane copolymer,60 m×0.25 mm,1.40 μm)was used for separating the analytes by programmed heating.Injection port temperature:210℃;Injection volume:1 μl.The flow rate of the chromatographic column is 1.1 ml/min.Mass spectrometry conditions:EI source;ion source temperature:220 C;Solvent delay:8.0 min,electron energy:70 eV.Results The concentration of Benzyl bromide is 10.11～505.48 ng/ml,and the linear relationship is good(r2＞0.99).The range of sample recovery rate(n=3)is 86.53%～111.66%,with a detection limit of 3.03 ng/ml and a quantification limit of 10.11 ng/ml.Conclusion This method has strong specificity,high sensitivity and good stability,and can accurately quantify the genotoxic impurity benzyl bromide in Donepezil hydrochloride tablets,providing method support for the determination of genotoxic impurity benzyl bromide in Donepezil hydrochloride tablets.
关键词
气相色谱-串联质谱法/盐酸多奈哌齐片/溴化苄/方法学验证Key words
GC-MS/Donepezil Hydrochloride Tablets/Benzyl bromide/Methodology validation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