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目的建立替米沙坦-羟丙甲纤维素(HPMC)固体分散体中替米沙坦含量测定的反相高效液相色谱(RP-HPLC)法,并对其进行理化性质表征。方法以HPMC为载体,采用冷冻干燥法,制备替米坦固体分散体。色谱分析方法为Phenomenex C_(18)(4.6 mm×250 mm,5μm)色谱柱,流动相0.01 moL/L KH_2PO_4(磷酸调pH至3.7)-乙腈(40:60),流速1.0 ml/min,检测波长298 nm,柱温35℃,进样量20μl。以X-射线衍射法(XRD)和差示扫描量热法(DSC)分析药物在载体中的存在状态。结果在本色谱条件下替米沙坦与辅料及溶剂峰分离良好,替米沙坦在1.0～100.0μg/ml质量浓度范围内与峰面积呈良好的线性关系(r=0.9999,n=8),日内精密度试验的相对标准偏差(RSD)为0.52%～0.72%(n=5),日间精密度试验的RSD为0.67%～1.79%(n=5),回收率为98.79%～100.20%(n=3)。主药在固体分散体中是以无定型或分子状态存在。结论以HPMC为载体可以成功制备出替米沙坦固体分散体。RP-HPLC色谱分析简便、易行,可用于替米沙坦-HPMC固体分散体中替米沙坦的含量测定。
Objective To establish an RP-HPLC method for the determination of telmisartan in solid dispersions of telmisartan-hypromellose (HPMC) and to characterize its physico-chemical properties. Methods HPMC as a carrier, using freeze-drying method, preparation of solid dispersion of telmisartan. The chromatographic method was Phenomenex C 18 column (4.6 mm × 250 mm, 5 μm). The mobile phase consisted of 0.01 mol / L KH 2 PO 4 (adjusted to pH 3.7 with phosphoric acid) -acetonitrile (40:60) and the flow rate was 1.0 ml / min. Wavelength 298 nm, column temperature 35 ℃, injection volume 20μl. The presence of the drug in the carrier was analyzed by X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Results Telmisartan was separated well from the excipients and solvent peaks under the chromatographic conditions. Telmisartan showed a good linear relationship with the peak area (r = 0.9999, n = 8) in the range of 1.0 ~ 100.0μg / ml. RSD was 0.52% -0.72% (n = 5), day RSD was 0.67% -1.79% (n = 5), and the recoveries were 98.79% -100.20 % (n = 3). The main drug in the solid dispersion is amorphous or molecular state exists. Conclusion The solid dispersions of telmisartan were successfully prepared using HPMC as carrier. RP-HPLC chromatographic analysis is simple, easy, and can be used for determination of telmisartan in telmisartan-HPMC solid dispersion.