摘要
建立了高效液相色谱-四极杆/线性离子阱质谱仪（HPLC-QTRAP-MS/MS）测定盐酸决奈达隆药物中两种基因毒性杂质（杂质C和D）痕量残留的分析方法。盐酸决奈达隆药物以0.1%甲酸水溶液-乙腈（20∶80）溶解后，分别采用Agilent Extend-C18色谱柱（1.8 μm，2.1 mm×50 mm）或YMC Pack-CN色谱柱（5 μm，4.6 mm×250 mm）进行分离，以0.1%甲酸水和乙腈作为流动相分别进行梯度洗脱，电喷雾正离子（ESI＋）扫描方式下选择离子监测（SRM）模式对样品进行检测。结果表明，杂质C和D在1.0~50 μg/L范围内线性关系良好，检出限（S/N=3）分别为0.20 μg/L和0.30 μg/L，定量下限（S/N=10）分别为0.80 μg/L和1.0 μg/L。该方法操作简单、灵敏度高、重现性好，可用于盐酸决奈达隆药物中两种基因毒性杂质痕量残留的测定。
A high performance liquid chromatography-quadrupole ion mass spectrometric（HPLC-QTRAP-MS/MS） method was developed for the determination of two potential genotoxic impurities（impurity C and impurity D） residues in dronedarone hydrochloride.After extracted with 0.1% formic acid-acetonitrile（20∶80），the dronedarone hydrochloride samples were separated on an Agilent Extend-C18 column（1.8 μm,2.1 mm×50 mm） or a YMC Pack-CN column（5 μm,46 mm× 250 mm） with two mobile phases of 0.1% formic acid and acetonitrile.The detection of analytes was performed in the positive mode and selective reaction monitoring（SRM） mode.As a result，the calibration curves of impurity C and impurity D showed good linearity in the range of 1.0-50 μg/L.The limits of detection（S/N=3） were 0.20 μg/L and 0.30 μg/L,respectively.The limits of quantitation（S/N=10）were 0.80 μg/L and 1.0 μg/L，respectively.The method has the advantages of simple operation，high sensitivity，good reproducibility，and could be used for the detection of two genotoxic impurities residues in dronedarone hydrochloride.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第9期1111-1115,共5页
Journal of Instrumental Analysis
关键词
高效液相色谱-四极杆/线性离子阱质谱仪
基因毒性杂质
盐酸决奈达隆
残留
high performance liquid chromatography-quadrupole ion mass spectrometry（HPLC-QTRAP-MS/MS）
potential genotoxic impuritie
dronedarone hydrochloride
residues
