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作 者:郭文敏[1] 白晓雪[1] 梁亚丽[1] 樊俊红[1] 赵岩[1]
机构地区:[1]石药集团中奇制药技术(石家庄)有限公司,石家庄050051
出 处:《中国药师》2011年第11期1570-1572,共3页China Pharmacist
基 金:科技部"十一五"重大新药创制项目(编号:2011ZX09401-306)
摘 要:目的:建立帕罗醇中反式帕罗醇和顺式帕罗醇的含量测定方法。方法:色谱柱为Phenomenex硅胶柱(250mm×4.6mm,5μm),以正己烷-乙醇-二乙胺(68:32:0.5)为流动相,流速为1.0ml·min^(-1),检测波长为267nm,柱温30℃。结果:反式帕罗醇、顺式帕罗醇与其他杂质之间能够达到良好分离;反式帕罗醇在5.0~4000.0μg·ml^(-1)浓度范围内线性关系良好(r=0.9999);顺式帕罗醇在2.0~800.0μg·ml^(-1)浓度范围内线性关系良好(r=0.999 9);反式帕罗醇和顺式帕罗醇平均加样回收率分别为99.60%、98.73%,RSD分别为0.61%、0.94%。结论:该法能够分别同时准确测定帕罗醇中两个异构体的含量,而且简便、准确、快速,可用于样品的质量控制。Objective: To establish a method for the determination of ( +/- )-trans-paroxol and ( -/+ )-cis-paroxol in paroxol by HPLC. Method : ( + / - ) -Trans-paroxol and ( - / + ) -cis-paroxol were separated on a Phenomenex silica column (250 mm × 4. 6 mm,5μm). The mobile phase consisted of hexane, ethanol and diethylamine ( 68: 32: 0. 5 ) at a flow rate of 1.0 ml. min ^-1 and the col- umn temperature was at 30℃ with detection wavelength of 267 nm. Result: The resolution of ( +/- )-trans-paroxol, ( -/+ )-cis- paroxol and other ingredients was promising. The linear calibration cmwe was obtained over the range of 5.0-4 000.0 μg· ml ^- 1tor( + / - ) -trans-paroxol ( r = 0. 999 9) and 2. 0-800. 0 μg·ml^- 1 for ( - / + ) -cis-paroxol ( r = 0. 999 9), respectively. The mean recovery, of ( +/- )-trans-paroxol and ( -/+ )-cis-paroxol was 99.60% with RSD of 0. 61% and 98.73% with RSD of 0. 94% ,respectively. Conclusion: This method is simple, rapid and accurate, and suitable for the quality control of samples.
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