投稿时间:2018-03-07  修订日期:2018-04-13  点此下载全文
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杜毅 上海交通大学医学院附属新华医院药学部, 上海 200092  
陈磊 上海长海医院药材科, 上海 200433  
李玲 第二军医大学药学院分析测试中心, 上海 200433  
周瑾 上海东方肝胆外科医院药材科, 上海 200438  
吕磊 上海东方肝胆外科医院药材科, 上海 200438 k_owen2002@126.com 
中文摘要:目的 采用GC-MS技术对多西他赛原料药中催化剂4-二甲氨基吡啶(DMAP)和脱水剂二环己基碳二亚胺(DCC)进行残留检测。方法 色谱柱为安捷伦的DB-5msUI(30 m×0.25 mm,0.25 μm)超高惰性毛细管气相色谱柱;采用程序升温方式,载气为高纯氦气,流速1.5 ml/min;进样量为1 μl。质谱采用EI源,选择离子监测模式:DMAP的定量离子为121,DCC的定量离子为163,内标龙脑的定量离子为95。多西他赛原料药采用甲醇超声提取。结果 DMAP和DCC的线性关系良好(r>0.999 2),其定量限分别为50.90和10.21 ng/ml,日内、日间精密度RSD均小于5.0%,回收率大于90%,符合方法学要求。3批样品中均未检测到DMAP和DCC的残留。结论 该方法灵敏度高,专属性好,可用于多西他赛原料药中微量杂质的残留检测。
中文关键词:气相色谱-质谱联用  多西他赛  4-二甲氨基吡啶  二环己基碳二亚胺  残留检测
Residue detection of DMAP and DCC in docetaxel by GC-MS
Abstract:Objective To establish a GC-MS method for residue detection of 4-Dimethylaminopyridine (DMAP) and Dicyclohexyl Carbodiimide (DCC) in docetaxel. Methods The separation was performed on an Agilent DB-5msUI capillary column (30 m×0.25 mm, 0.25 μm) with programmed temperature. The carrier gas was high purity helium, the flow rate was 1.5 ml/min and the injection volume was 1 μl. Electron impact ion source (EI) and selection monitoring mode (SIM) were applied for quantitative analysis. The quantitative ion of DMAP, DCC and internal standard (IS) was 121, 163 and 95 respectively. Docetaxel was ultrasonically extracted with methanol. Results The calibration of DMAP and DCC showed good linear relationship (r>0.999 2), the limits of quantification (LOQ) were 50.90 ng/ml and 10.21 ng/ml separately. Intra-day and inter-day precision were all less than 5% and recoveries were more than 90%, which conformed with the requirement of methodology validation. No residues of DMAP and DCC were detected in three batches of samples. Conclusion The method was sensitive and selective which can be used for the detection of trace impurities in docetaxel.
keywords:GC-MS  docetaxel  DMAP  DCC  residue detection
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