HPLC测定枸橼酸莫沙必利胶囊中的有关物质

Determination of Related Substances of Mosapride Citrate in the Capsule Formulation by HPLC

关键词:  枸橼酸莫沙必利  高效液相色谱法  有关物质  胶囊剂

Key words:  mosapride citrate  HPLC  related substances  capsule

摘要:

目的 建立反相高效液相色谱法测定枸橼酸莫沙必利胶囊中有关物质的总量。方法 分析柱采用 Shimadzu C18 (150 mm×4. 6 mm, 5 μm)，流动相为0.02 mol·L^-1磷酸二氢钾缓冲液(用磷酸调pH至4.0)-甲醇(50∶50)，流速为1 mL·min^-1，检测波长为274 nm。结果 该法能将枸橼酸莫沙必利与其有关物质有效分离。供试溶液的浓度确定为500 mg·mL^-1，室温下稳定，有关物质的峰面积重复性良好。莫沙必利浓度在3.0~15.0 mg·mL^-1与峰面积线性关系良好(r=0. 999 7，n=6)，精密度RSD<1.5%，回收率为100.5%~101.4%。而且，该法能用作稳定性试验的分析方法。结论 该法简单、快速、灵敏，适合用于枸橼酸莫沙必利胶囊中有关物质的检查。

Abstract:

OBJECTIVE To establish an HPLC method for the assay of mosapride citrate related substances in the capsule that might originate from synthesis processes or degradation. METHODS The related substances in mosapride citrate capsules were analyzed by a chromatographic system comprising a reverse phase C18 analytical column, a mobile phase of methanol-0.02 mol·L^-1 potassium dihydrogen phosphate buffer (pH adjusted to 4.0 with o-phosphoric acid) (50∶50), a flow rate of 1 mL·min^-1 and a UV detector set at 274 nm. RESULTS The HPLC method had shown good chromatographic resolution for mosapride citrate and its related substances. The analyte concentration was found to be 500 mg·mL^-1, and RSD of peak area responses of the related substances was 1.3%. The sample and standard solutions were stable for 24 hours at room temperature. The calibration curve was linear in the range from 3.0 to 15.0 mg·mL^-1 (r=0.999 7, n=6). The precision RSD at three different concentration levels (3, 5, 10 mg·mL^-1) were less than 1.5%. The recovery was between 100.5% and 101.4%. In addition, analysis of samples subjected to accelerated stability conditions showed that all degradants were resolved from the active component, resulting in a stability-indicating assay. CONCLUSION The HPLC method is simple, rapid, selective and suitable for quantitative determination of mosapride citrate related substances in the capsule.