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目的:建立5-氨基水杨酸灌肠液的含量及其有关物质的测定方法。方法:采用高效液相色谱梯度洗脱法测定,色谱柱为Hypersil,ODS C18(250 mm×4.6 mm,5.0μm),流动相为流动相A为pH 7.5磷酸缓冲液(PBS)∶四丁基氢氧化铵溶液(TBAH)∶甲醇∶水(600∶50∶50∶300);流动相B为pH7.5磷酸缓冲液∶TBAH∶甲醇∶水(200∶50∶300∶450)。检测波长为208 nm;柱温40℃,进样量20μl。结果:5-氨基水杨酸与其两种降解产物可完全分离。5-氨基水杨酸在1~250μg·ml-1的浓度范围内,浓度与峰面积具有良好的线性关系,r=0.999 5,平均回收率为99.44%,RSD为0.94%(n=9)。结论:方法简单、灵敏、重复性好,可用于本品的含量和有关物质检查。
Objective: To establish a method for the determination of 5-aminosalicylic acid enema and its related substances. Methods: The mobile phase consisted of Hypersil, ODS C18 (250 mm × 4.6 mm, 5.0 μm) and the mobile phase A was pH 7.5. Phosphate buffer solution (PBS) was obtained by gradient elution with high performance liquid chromatography Ammonium solution (TBAH): methanol: water (600:50:50:300); Mobile phase B was pH 7.5 phosphate buffer: TBAH: methanol: water (200: 50: 300: 450). The detection wavelength was 208 nm; the column temperature was 40 ℃, and the injection volume was 20μl. Results: 5-Aminosalicylic acid and its two degradation products can be completely separated. The concentration of 5-aminosalicylic acid in the concentration range of 1 ~ 250μg · ml-1 has a good linear relationship with the peak area, r = 0.999 5, the average recovery was 99.44% and the RSD was 0.94% (n = 9) . Conclusion: The method is simple, sensitive, reproducible, and can be used for the content of this product and related substances inspection.