5-氨基水杨酸锌及相关物质的高效液相色谱分析研究

Study on the Analysis of Zinc 5 Aminosalicylate and Related Compounds by High Performance Liquid Chromatography

对５－氨基水杨酸锌及相关物质５－氨基水杨酸、水杨酸、对氨基苯酚和５－苯偶氮基水杨酸的高效液相色谱法（ＨＰＬＣ）的分离条件进行了优化研究，结果表明，采用ＣＬＣ－ＯＤＳ（１５０ｍｍ×６．０ｍｍｉ．ｄ．，１０μｍ）作为分离柱，１％（Ｖ／Ｖ）ＨＡｃ－ＭｅＯＨ（４∶６）作为流动相，在流速为１ｍＬ／ｍｉｎ的情况下，上述５种物质在１０ｍｉｎ内可以达到基线分离，保留时间的日内和日间的变异系数分别小于２％和５％，在一定浓度范围内，浓度与峰面积的线性关系良好。对５－氨基水杨酸锌原药含量测定表明，主要杂质为５－氨基水杨酸和水杨酸；对５－氨基水杨酸锌在酸和热强化条件下的浓度变化研究表明。

In this paper, the separation and determination conditions of zinc 5 aminosalicylate (ZASA) and related compoands by high performance liquid chromatography(HPLC) have been studied systematically. The baseline separation was achieved at 20℃ on a CLC ODS column(150mm×6 0mm i.d.,10μm) within 10 minutes by using 1%( V/V )HAc MeOH(4∶6) as mobile phase at a flow rate of 1mL/min. The RSDs of rention time within day and between days were less than 2% and 5% respectively. The injection volume was 20μL, and relationships between the peak area with 280nm detection and the analyte concentration were linear within certain ranges. This method was used for determination of ZASA, impurities and thermal decomposition compounds. The results showed that the impurities in the crude ZASA were 5 aminosalicylic acid and salicylic acid. The thermal decomposition compounds in acid medium were 5 aminosalicylic acid, 5 aminophenol and 5 benzeneazosalicylic acid.