Development and validation of a stability indicating HPLC method to determine diltiazem hydrochloride in tablets and compounded capsules

ABSTRACT A stability indicating HPLC method to determine diltiazem hydrochloride (DTZ) in tablets and compounded capsules was developed and validated according to Brazilian and the International Conference on Harmonization (ICH) guidelines. The separation was carried out on a Purospher Star® C18 (150 x 4.6 mm i.d., 5 µm particle size, Merck Millipore) analytical column. The mobile phase consisted of a 0.05% (v/v) trifluoroacetic acid aqueous solution and a 0.05% trifluoroacetic acid methanolic solution (44:56, v/v). The flow rate was 1.0 mL.min-1 with a run time of 14 minutes. The detection of DTZ and degradation products (DP) was performed at 240 nm, using a diode array detector. The method proved to be linear, precise, accurate, selective, and robust, and was adequate for stability studies and routine quality control analyses of DTZ in tablets and compounded capsules.

摘要 本研究开发并验证了一种稳定性指示型高效液相色谱（HPLC）法，用于测定片剂与复方胶囊中的盐酸地尔硫卓（diltiazem hydrochloride，DTZ），验证工作依照巴西相关指南及国际人用药品注册技术要求协调会（ICH）指南开展。色谱分离采用Purospher Star® C18分析色谱柱，规格为150×4.6 mm内径、5 μm粒径，生产商为默克密理博（Merck Millipore）。流动相由0.05%（体积比）三氟乙酸水溶液与0.05%三氟乙酸甲醇溶液按44:56的体积比混合而成，流动相流速为1.0 mL·min⁻¹，分析运行时长为14分钟。采用二极管阵列检测器，在240 nm波长下对盐酸地尔硫卓（DTZ）及其降解产物（DP）进行检测。结果证实，该方法具备线性、精密度、准确度、选择性与耐用性，可适用于片剂及复方胶囊中盐酸地尔硫卓的稳定性研究与常规质量控制分析。