枸橼酸莫沙必利片质量标准中含量及其均匀度检测方法修订探讨

Discussion on Revision of Detection Methods for Content and Content Uniformity in Quality Standard of Mosapride Citrate Tablets

目的 探讨高效液相色谱法(HPLC)用于枸橼酸莫沙必利片含量及含量均匀度检测的可行性。方法 色谱柱:Agilent ZORBAX SB-C18(250 mm×4.6 mm,5μm);流动相:枸橼酸盐溶液(取枸橼酸钠8.82 g,加水至1 000 ml,用稀盐酸调节p H值至4.0)-乙腈(60∶40);检测波长:274 nm;流速:1.0 ml/min;柱温:30℃;进样量:20μl。结果 枸橼酸莫沙必利片在0.020 06~0.802 4 mg/ml范围内线性关系良好(r=0.999 5),平均回收率为99.02%(相对标准偏差(RSD)=0.60%,n=6)。6批样品HPLC测定结果与紫外分光光度法比较,含量分别是99.10%、98.51%、98.72%、98.83%、99.75%、99.62%与98.71%、99.02%、99.53%、98.41%、99.43%、98.90%;A+2.2S分别是5.92、7.03、4.74、5.24、7.91、5.42与6.83、7.41、5.90、5.62、8.73、5.94。结论 所建立的HPLC符合方法学评价要求,可用于枸橼酸莫沙必利片中含量及含量均匀度的检测,可为该药品质量标准修订提供参考。

Objective To explore the feasibility of a high-performance liquid chromatography( HPLC) method for content and content uniformity of Mosapride Citrate Tablets.Methods HPLC was performed on a Agilent ZORBAX SB-C18 column(250mm×4.6 mm,5 μm) and the detection wavelength was 274 nm.The mobile phase consisted of citrate buffer(8.82 g of trisodium citrate dihydrate were dissolved in 1 000 mL of water,adjusted with dilute hydrochloric acid to a pH of 4.0)/acetonitrile(60:40),the flow rate was 1.0 ml/min,the column temperature was 35 ℃,and the injection volume was 20 μl.Results The linear range was 0.020 06~0.802 4 mg/ml(r=0.999 5).The average recovery was 99.02%(RSD=0.60%,n=6).The average contents of mosapride citrate in the six batches of samples by HPLC were 99.10%,98.51%,98.72%,98.83%,99.75% and 99.62%,respectively,and the contents of A+2.2S were 5.92,7.03,4.74,5.24,7.91 and 5.42,respectively.The average contents by ultraviolet spectrophotometry were 98.71%,99.02%,99.53%,98.41%,99.43% and 98.90%,respectively,and the contents of A+2.2S were 6.83,7.41,5.90,5.62,8.73 and 5.94 respectively.Conclusion The HPLC method meets the requirements of methodology,hence it can be used for the detection of the content and content unifority of Mosapride Citrate Tablets and may provide a reference for the modification of pharmaceutical quality standards.