摘要
应用高效液相色谱方法研究了以2,6二氯苯酚和苯胺为起始原料合成药物中间体1(2,6二氯苯基)2吲哚酮(DCI)过程中,DCI及相关物质在不同色谱条件下的分离情况。结果表明,以CLCCN(150mm×6.0mmi.d.,7μm)为分离柱,以MeOHH2O(体积比为6∶4)为流动相,在流速为1mLmin的情况下,DCI及相关物质可以达到基线分离。建立了快速准确测定DCI纯度和检验杂质种类的高效液相色谱分析方法,方法准确可靠。对两个精品和两个粗品分别进行测定,结果表明精品中的杂质主要为N(2,6二氯二苯胺基)氯乙酰胺,粗品中的杂质主要为N(2,6二氯二苯胺基)氯乙酰胺和2,6二氯二苯胺。
The separation of 1 (2,6 dichlorophenyl) 2 indolone (DCI) and related materials in the synthesis of medical intermediate DCI from 2,6 dichlorophenol and phenylamine was investigated with high performance liquid chromatography under different chromatographic conditions.The results showed that DCI and related materials were in baseline separation by using CLC CN(150 mm×6.0 mm i.d.,7 μm) as column,MeOH H 2O(6∶4,V/V) as mobile phase and a flow rate at 1 mL/min. A rapid, accurate and reproducible HPLC method for determining DCI was developed. Fine and crude DCI samples were detected, results showed that N (2,6 dichlorodiphenyl) chloracetyl amide (CBCC) was the main impurity in fine sample, and CBCC and 2,6 dichlorodiphenylamine were the main impurities in the crude one.
出处
《色谱》
CAS
CSCD
北大核心
2000年第1期55-56,共2页
Chinese Journal of Chromatography
关键词
高效液相色谱法
吲哚酮
DCI
分离分析
high performance liquid chromatography
1 (2,6 dichlorophenyl) 2 indolone and related compounds
impurity
