摘要
利用高效液相色谱-二极管阵列检测器-质谱联用方法对洛伐他丁及其杂质成分进行分离分析和结构鉴定。实验采用D iamonsil C18(5μm,4.6 mm×250 mm)为分离柱,乙腈-水(含0.1%乙酸)(65∶35)为流动相,分离并检测了洛伐他丁及其杂质;通过与DAD检测器和离子阱质谱联用,获得了它们的紫外光谱和质谱数据;紫外光谱表明除氢化洛伐他丁外其余杂质与洛伐他丁基本结构相同,利用MS和MS2数据确定了杂质的分子量和侧链结构,由此鉴定了其中10个杂质的结构。实验结果表明,高效液相色谱-二极管阵列检测器-质谱联用技术可以快速鉴定洛伐他丁中的杂质化学成分。
A high performance liquid chromatography-diode array detection-electrospray ionization tandem mass spectrometry method was developed for analysis and identification of impurities in lovastatin. Lovastatin and impurities were separated on a Diamonsil C18 column（5μm,4.6 mm × 250 mm）using acetonitrile-water （containing 0.1% acetic acid） （65：35） as mobile phase. The elutes were detected with diode array detector and ion trap mass spectrometer in positive mode. The ultraviolet （ UV）, MS and MS2 spectra of each chromatographic peak were obtained. The UV spectra of the impurities are similar with those of lovastatin except for dihydrolovastatin. It indicated that they have the same basic structures. Then the [ M ＋ H ]^＋ ions and their MS2 spectra were used for determining the molecule mass and side-chain. According to analyses of the UV, MS and MS2 as well as the comparison with the published hterature, the structures of ten impurities were identified. The results indicated that the described of impurities in lovastatin. method could be effectively applied to perform identification of impurities in lovastatin.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2006年第1期115-118,共4页
Chinese Journal of Analytical Chemistry
关键词
洛伐他丁
杂质
高效液相色谱
二极管阵列检测
质谱
鉴别
Lovastatin, impurity, high performance liquid chromatography, diode array detection, mass spectrometry, identification
