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目的:建立HPLC法测定甲磺酸卡莫他特原料药的含量及其有关物质。方法:采用VenusilX BP-C18柱(250mm×4.6mm,5μm),以甲醇-0.01mol·L-1四丁基氢氧化铵溶液(25∶75,用磷酸调节pH至3.5)为流动相,流速1.0mL·min-1,紫外检测波长265nm,室温,进样量20μL。结果:主峰能与相邻杂质峰较好分离。甲磺酸卡莫他特浓度在5.0～81.3μg·mL-1范围内,与峰面积呈线性关系,r=0.9996。低、中、高浓度平均加样回收率(n=3)分别为99.7%,99.2%,100.1%;RSD分别为0.65%,0.51%,0.47%。结论:本法准确、方便,专属性强,可用于测定甲磺酸卡莫他特原料药含量及有关物质。
OBJECTIVE: To establish an HPLC method for the determination of the content of camomit mesylate and its related substances. Methods: VenusilX BP-C18 column (250 mm × 4.6 mm, 5 μm) was used with mobile phase of methanol-0.01 mol·L-1 tetrabutylammonium hydroxide (25:75, adjusted to pH 3.5 with phosphoric acid) Min-1, UV detection wavelength 265nm, room temperature, injection volume 20μL. Results: The main peak can be better separated from adjacent impurity peaks. The concentration of carbamates in methanesulfonic acid was in the range of 5.0 ~ 81.3μg · mL-1 with a linear relationship with the peak area, r = 0.9996. The average recoveries (n = 3) of low, medium and high concentrations were 99.7%, 99.2% and 100.1%, respectively. The RSDs were 0.65%, 0.51% and 0.47%, respectively. Conclusion: This method is accurate, convenient and specific, and can be used for the determination of the content and related substances of the raw materials of carbamates methanesulfonate.