Görög S, Babják M, Balogh G, Brlik J, Csehi A, Dravecz F, Gasdag M, Horváth P, Laukó A, Varga K
Chemical Works of Gedeon Richter Ltd., P.O.B. 27, H-1475 Budapest, Hungary.
Talanta. 1997 Sep;44(9):1517-26.
A general scheme is set up for the estimation of the impurity profile of bulk drug substances by the complex use of chromatographic, spectroscopic and hyphenated techniques. Several examples are presented as illustrations to the scheme from the authors' laboratory involving the use of chromatographic methods such as thin-layer-(TLC), gas-(GC), analytical and preparative high-performance liquid chromatography (HPLC), spectroscopic methods such as mass spectrometry (MS) and NMR spectroscopy as well as hyphenated techniques (HPLC/diode-array UV, GC/MS and HPLC/MS). In addition to summarizing earlier work, new examples are also presented: identification of an impurity (propyl 4-[diethylcarbamoyl(methoxy)]-3-methoxy phenylglyoxylate, II) in propanidid (I) and two unsaturated impurities in allylstrenol (VII) by GC/MS and HPLC/diode-array UV as well as estimation of the impurity profile of mazipredone (III) by HPLC/MS and HPLC/diode-array UV.
通过综合运用色谱、光谱和联用技术，建立了一种用于估算原料药杂质分布的通用方案。本文给出了几个示例，以说明作者实验室中该方案的应用，其中涉及使用多种色谱方法，如薄层色谱（TLC）、气相色谱（GC）、分析型和制备型高效液相色谱（HPLC），光谱方法如质谱（MS）和核磁共振光谱（NMR），以及联用技术（HPLC/二极管阵列紫外检测器、GC/MS和HPLC/MS）。除了总结早期工作外，还给出了新的示例：通过GC/MS和HPLC/二极管阵列紫外检测器鉴定丙泮尼地（I）中的一种杂质（4-[二乙氨基甲酰基（甲氧基）]-3-甲氧基苯甲酰乙酸丙酯，II）以及烯丙孕醇（VII）中的两种不饱和杂质，以及通过HPLC/MS和HPLC/二极管阵列紫外检测器估算马唑泼尼松（III）的杂质分布。
