摘要
目的开发一种高效液相色谱法(HPLC)用于检测普瑞巴林口崩片中的有关物质。方法使用Inertsil ODS-3V色谱柱(尺寸为4.6 mm×250 mm,粒径为5μm),以乙腈和磷酸二氢钾溶液(将1.2 g磷酸二氢钾溶解于1000 mL水中,并用稀氢氧化钾溶液将pH调至6.9)作为流动相A,乙腈和水作为流动相B,进行梯度洗脱;流速设定为1.0 mL/min;色谱柱温度保持在30℃;检测波长选择210 nm。结果经酸、碱、氧化、高温、光照及还原等强制降解处理后,主峰与各杂质均实现有效分离。普瑞巴林、普瑞巴林内酰胺、普瑞巴林葡萄糖加合杂质以及普瑞巴林二聚体在不同浓度范围内,其峰面积与浓度之间表现出良好的线性关系;供试品溶液与对照品溶液48 h内稳定性良好;普瑞巴林内酰胺的加样回收率平均值为99.93%,相对标准偏差(RSD)为1.25%;普瑞巴林葡萄糖加合杂质的加样回收率平均值为96.49%,RSD为3.33%;普瑞巴林二聚体的加样回收率平均值为104.60%,RSD为1.43%。结论本方法简洁、准确度高,适用于普瑞巴林口崩片中有关物质的控制。
Objective To develop a high-performance liquid chromatography(HPLC)technique for assessing impurities in pregabalin orally disintegrating tablets.Methods An Inertsil ODS-3V chromatographic column(4.6 mm×250 mm,5μm)served as the column,with a mobile phase A consisting of acetonitrile and a potassium dihydrogen phosphate solution(prepared by dissolving 1.2 g of potassium dihydrogen phosphate in 1000 mL of water and adjusting the pH to 6.9 using a dilute potassium hydroxide solution),and a mobile phase B consisting of acetonitrile and water.The flow rate was maintained at 1.0 mL/min,the column temperature was set at 30℃,and the detection wavelength was 210 nm.Results Under conditions of acid,alkali,oxida-tion,high temperature,light,and reduction damage,the separation degree between the impurities and the main peak was good.The peak areas of pregabalin,pregabalin lactam,pregabalin glucose adduct impurities,and pregabalin dimer were linear with concentration in each concentration range;The stability of the test solution and the reference solution was good within 48 hours;The average recovery rate of pregabalin lactam was 99.93%and relative standard deviation(RSD)was 1.25%.The mean re-covery rate for the pregabalin glucose adduct impurity was 96.49%,and the RSD was 3.33%.For the pregabalin dimer,the av-erage recovery was 104.60%,and the RSD was 1.43%.Conclusion The method is straightforward,precise,and appropriate for managing related substances in pregabalin orally disintegrating tablets.
作者
范平
夏雪琴
艾阳文
FAN Ping;XIA Xueqin;AI Yangwen(Jiangxi Center for Drug Certification and Evaluation,Nanchang Jiangxi 330029,China;Jiangxi Health Industry Institute of Traditional Chinese Medicine,Nanchang Jiangxi 330115,China)
出处
《天津药学》
2025年第7期769-773,837,共6页
Tianjin Pharmacy
基金
江西省药品监督管理局科研项目(2024GL19)。
关键词
高效液相色谱法
普瑞巴林口崩片
普瑞巴林内酰胺
普瑞巴林葡萄糖加合杂质
普瑞巴林二聚体
质量控制
High-performance liquid chromatography
Pregabalin orally disintegrating tablets
Pregabalin lactam impurity
Pegabalin glucose adduct impurity
Pegabalin dimer
Quality control
