摘要
建立了Y101中间体N-(N-苯甲酰基-O-苯甲酰基-L-酪氨酰基)-L-苯丙氨醇(M057)及其已知杂质的含量测定方法。采用液相色谱质谱联用技术(HPLC/MS),正离子扫描模式指认杂质峰;采用高效液相色谱(HPLC)外标法,以甲醇-水(v∶v=75∶25)洗脱,测定M057含量,以甲醇-0.01%磷酸水溶液梯度洗脱,测定3个已知杂质含量。测定结果:M057含量不低于77%,已知杂质总量未超过4.5%。本法已作为该中间体质量内控方法。
N-（N-Benzoyl-O-benzoyl-L-tyrosyl）-L-phenylalaninol （M057）, an intermediate for dipeptide Y101, and three impurities co-existed with M057 were determined with HPLC/MS. The positive ion scanning was used for the identification of the impurities and their contents were determined using methanol -0.01% phosphoric acid as the gradient elution. An external standard was used for the analysis of M057 with methanol-water （v：v=75：25） as the mobile phase. This method has been used as a standard for the quality control of M057.
出处
《精细化工中间体》
CAS
2014年第2期65-69,共5页
Fine Chemical Intermediates
基金
"十二五"国家重大新药创制科技重大专项(2011ZX09102-009-002)
贵州省中药现代化科技产业研究开发专项(黔科合中药字[2012]5054)
