高效液相色谱-线性离子阱质谱鉴定瑞舒伐他汀中间体中相关杂质
发布时间：2018-11-11 20:20
【摘要】：目的:建立高效液相色谱-线性离子阱质谱法分离鉴定瑞舒伐他汀药物中间体N-[5-腈基-4-(4-氟苯基)-6异丙基嘧啶-2-]-N-甲基甲磺酰胺中的有关杂质,并探讨这些杂质的质谱裂解规律。方法:采用Cortecs C18色谱柱(100 mm×2.1 mm,2.7μm),以乙腈-0.1%甲酸溶液为流动相,进行梯度洗脱,流速为0.25 m L·min-1,柱温35℃,检测波长为242 nm,电喷雾离子化正负2种离子模式扫描。结果:中间体与各已知杂质均分离良好,根据一级和多级质谱信息,共鉴定出7种杂质,包括对甲基苯磺酸、4-(4-氟苯基)-2-羟基-6-异丙基-5-氰基-嘧啶、4-(4-氟苯基)-2-氨基-6-异丙基-5-氰基-嘧啶、5-氰基-6-(4-氟苯基)-4-异丙基-2-N-甲磺酰胺嘧啶-1-N-氧化物、4-(4-氟苯基)-2-甲氨基-6-异丙基-5-氰基-嘧啶、中间体的氯代产物和5-甲酸内酯化产物。杂质类型主要为氧化、降解产物及合成副产物。结论:本法分析结果为有关杂质确证提供分析方法,为瑞舒伐他汀合成中的质量控制提供指导。
[Abstract]:Objective: to establish a high performance liquid chromatography-linear ion trap mass spectrometry for the separation and identification of the drug intermediate N- [5- nitrilyl-4- (4-fluorophenyl) -6-isopropylpyrimidine-2-] -N-methylmethanesulfonyl Related impurities in amine, The law of mass spectrometry cracking of these impurities was discussed. Methods: a Cortecs C18 column (100 mm 脳 2. 1 mm,2.7 渭 m),) with acetonitrile-0.1% formic acid solution as mobile phase was used for gradient elution. The flow rate was 0.25 mL min-1, at 35 鈩，
本文编号：2326034
[Abstract]:Objective: to establish a high performance liquid chromatography-linear ion trap mass spectrometry for the separation and identification of the drug intermediate N- [5- nitrilyl-4- (4-fluorophenyl) -6-isopropylpyrimidine-2-] -N-methylmethanesulfonyl Related impurities in amine, The law of mass spectrometry cracking of these impurities was discussed. Methods: a Cortecs C18 column (100 mm 脳 2. 1 mm,2.7 渭 m),) with acetonitrile-0.1% formic acid solution as mobile phase was used for gradient elution. The flow rate was 0.25 mL min-1, at 35 鈩，
本文编号：2326034
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