| 引用本文: | 徐力昆,窦媛媛,王洪权.LC-MS/MS测定马来酸桂哌齐特原料合成中间体残留[J].中国现代应用药学,2013,30(4):421-424. |
| XU Likun,DOU Yuanyuan,WANG Hongquan.Determination of the Synthesized Intermediates Residual of Cinepazide Maleate by LC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2013,30(4):421-424. |
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| 摘要: |
| 目的 采用LC-MS/MS测定马来酸桂哌齐特原料中间体氯乙酰吡咯烷、1-哌嗪乙酰基吡咯烷的含量，考察马来酸桂哌齐特原料中两种中间体残留情况。方法 建立LC-MS/MS测定中间体氯乙酰吡咯烷、1-哌嗪乙酰基吡咯烷的方法，测定马来酸桂哌齐特原料样品中的中间体杂质残留。结果 LC-MS/MS测定中间体氯乙酰吡咯烷、1-哌嗪乙酰基吡咯方法精密度分别为3.6%和4.0%，线性回归方程分别为Y=26 501X-6 034(r=0.999 8，n=5)及Y=51 616X-10 434(r=0.999 9，n=5)，平均回收率分别为98.2%和97.3%，测定马来酸桂哌齐特原料中两中间体均<0.05%。结论 该方法准确可靠，灵敏度高，可为马来酸桂哌齐特原料质量控制及质量标准的建立提供依据。 |
| 关键词: 马来酸桂哌齐特 LC-MS/MS 中间体 氯乙酰吡咯烷 1-哌嗪乙酰基吡咯烷 质量控制 |
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| Determination of the Synthesized Intermediates Residual of Cinepazide Maleate by LC-MS/MS |
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XU Likun, DOU Yuanyuan, WANG Hongquan
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Institute of Microbiology and Epidemiology, Academy of Military Medical Sciences, Beijing 100071, China
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| Abstract: |
| 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. |
| Key words: cinepazide maleate LC-MS/MS intermediates chloroacetyl pyrrolidine 1-piperazine acetyl pyrrolidine quality control |
