Determination of the Synthesized Intermediates Residual of Cinepazide Maleate by LC-MS/MS

OBJECTIVE To determine the content of chloroacetyl pyrrolidine and 1-piperazine acetyl pyrrolidine which are the intermediates of cinepazide maleate synthesis in cinepazide maleate by LC-MS/MS. METHODS The LC-MS/MS method was established for determination of chloricacetyl pyrrolidine and 1-piperazine acetyl pyrrolidine. The residue of these two intermediates had been determined in cinepazide maleate. RESULTS The precision of the LC-MS/MS for chloroacetyl pyrrolidine and 1-piperazine acetyl pyrrolidine were 3.6% and 4.0%, the linear regression equation were Y=26 501X-6 034 (r=0.999 8, n=5) and Y=51 616X-10 434(r=0.999 9, n=5), the average recoveries were 98.2% and 97.3%. The contents of two intermediates in cinepazide maleate were both less than 0.05%. CONCLUSION The method is accurate, reliable with high sensitivity, and can provide the basic to quality control and the establishment of quality standard for cinepazide maleate.