普瑞巴林胃滞留缓释片含量测定及高黏性辅料对测定结果的影响
Determination of the content of pregabalin gastric retention sustained-release tablets and influence of high viscosity excipients on the determination results
刘娟 1庞跃成 2陈艳敏 2左淑航 2高永吉1
作者信息
- 1. 潍坊医学院,潍坊 261053
- 2. 华润双鹤利民药业(济南)有限公司,济南 250200
- 折叠
摘要
建立普瑞巴林胃滞留缓释片含量测定的高效液相色谱法(HPLC),采用一种特殊的样品前处理方式成功解决了普瑞巴林回收率低的难题.通过比较盐析法和辅料分散法,建立了克服供试品溶液黏稠的前处理方法.两种前处理方法均可用于本品的含量测定,但盐析法简便易行.采用的HPLC条件为Inertsil ODS-3(4.6 mm×0.25 m,5µm)色谱柱,流动相3.4 g/L磷酸二氢钾(氨水调pH至 6.3)-甲醇(85︰15),柱温 30℃,流速 1.0 mL/min,进样量 50µL,检测波长 210 nm.盐析法方法学验证结果显示,制剂中普瑞巴林平均回收率为 99.74%,RSD为 0.43%;精密度试验的RSD为 0.77%;供试品溶液 12h内稳定,色谱系统耐用性良好,辅料不干扰含量检测.本研究建立的测定方法稳定、可靠,适用于普瑞巴林胃滞留缓释片的含量测定.
Abstract
A high-performance liquid chromatographic(HPLC)method for the assay of pregabalin gastric retention sustained-release tablets was established,successfully solving the problem of low recovery of pregabalin through a special sample pretreatment method.By comparing salting-out and excipient dispersion,the pretreatment methods to overcome the viscosity of the test solution were established.Both methods can be used for the determination of the product content,but the salting-out method is easier to operate.The HPLC conditions were Inertsil ODS-3(4.6 mm×0.25 m,5 µm)column with mobile phase of 3.4 g/L potassium dihydrogen phosphate(pH adjusted to 6.3 by ammonia)and methanol(85︰15);the column temperature was 30℃;the flow rate was 1.0 mL/min;the sample size was 50 µL;and the detection wavelength was 210 nm.Through the validation of the salting-out method,the average recovery of the drug was 99.74%and the RSD was 0.43%;the precision test RSD was 0.77%;the test solution was stable within 12 h;the chromatographic system had good durability;and the excipient did not interfere with the content detection.The method is stable,reliable and suitable for the assay of pregabalin gastric retention sustained release tablets.
关键词
普瑞巴林/胃滞留缓释片/含量测定/高效液相色谱/盐析/辅料分散Key words
pregabalin/gastric retention sustained-release tablets/content determination/high performance liquid chromatography/salting-out/excipient dispersion引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据