[Isolation and purification of the process impurity in losartan by reversed-phase column chromatography].
A process impurity (approximately 4%, w/w) was isolated from losartan crude by low-pressure reversed-phase column chromatography. At first the elution portions containing the target compound were collected. After evaporation and recrystallization, the purity of the target compound was found to be over 99% based on high performance liquid chromatography with ultraviolet absorption. The electrospray ionization-mass spectrometry result showed that it was an isomeric compound of losartan, which had same fragmentation pattern with its parent compound. And at last the compound was further characterized by nuclear magnetic resonance. This research demonstrates that the low-pressure reversed-phase column chromatography can raise separation efficiency and recovery comparing with other conventional column chromatography, and the technique can be applied as an effective means for the enrichment and extraction of impurities in pharmaceutical separation.
Nie
Jing
J
Center for Instrumental Analysis, China Pharmaceutical University, Nanjing 210009, China.
Wen
Yi
Y
Yu
Qiongwei
Q
Xiang
Bingren
B
Feng
Yuqi
Y
D000327:Adsorption; D016588:Anticarcinogenic Agents / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D003377:Countercurrent Distribution / Q000379:methods; D004340:Drug Contamination; D004355:Drug Stability; D004365:Drugs, Chinese Herbal / Q000737:chemistry*; D019808:Losartan / Q000302:isolation & purification*; D021241:Spectrometry, Mass, Electrospray Ionization
D016588:Anticarcinogenic Agents; D004365:Drugs, Chinese Herbal; D019808:Losartan