HPLC法测定复方氨氯地平缬沙坦氢氯噻嗪片剂溶出度

目的: 优化并建立复方氨氯地平缬沙坦氢氯噻嗪片剂溶出度的测定方法,同时检测氨氯地平、缬沙坦和氢氯噻嗪3个组分的溶出度. 方法: 采用Zorbax SB-C₁₈(3.0 mm×150 mm,5 μm)色谱柱,以0.1%三乙胺(pH 2.8)-甲醇-乙腈为流动相进行梯度洗脱,流速0.8 mL·min^-1,检测波长230 nm. 结果: 本方法系统适用性佳,3个组分分离度良好,空白辅料及强制降解产物不干扰3个组分的测定;氨氯地平、缬沙坦和氢氯噻嗪的线性范围分别为2.8~17.3 μg·mL^-1(r²=0.999 9)、32.0~200.2 μg·mL^-1(r²=0.999 4)和2.5~15.6 μg·mL^-1(r²=0.999 6);平均回收率(n=9)分别为100.6%(RSD=1.1%)、100.8%(RSD=0.62%)和101.0%(RSD=0.70%);定量限分别为0.33、0.13和0.12 μg·mL^-1;检测限分别为0.10、0.03和0.03 μg·mL^-1;供试品溶液在72 h内稳定;耐用性良好;该方法测得氨氯地平、缬沙坦和氢氯噻嗪在30 min溶出度分别为标示量的92%、94%和91%. 结论: 该方法适用于复方氨氯地平缬沙坦氢氯噻嗪片剂溶出度的检测.

Objective: To establish an optimized HPLC method to determine the dissolution of compound amlodipine,valsartan and hydrochlorothiazide tablets and simultaneously determine the dissolution of three components amlodipine,valsartan and hydrochlorothiazide. Methods: The method was carried on the Zorbax SB-C₁₈(3.0 mm×150 mm,5 μm)column,using gradient elution of the mobile phase of water containing 0.1% triethylamine(pH 2.8),methanol and acetonitrile.The flow rate was 0.8 mL·min^-1 at the detection wavelength of 230 nm. Results: The method was of good system suitability and the three components were separated completely.The blank excipients and degradation products did not interfere with the determination of the three components.The linearity and range were 2.8-17.3 μg·mL^-1 (r²=0.999 9)for amlodipine,32.0-200.2 μg·mL^-1 (r²=0.999 4)for valsartan,and 2.5-15.6 μg·mL^-1 (r²=0.999 6)for hydrochlorothiazide.The average recoveries(n=9)of amlodipine,valsartan and hydrochlorothiazide were 100.6%(RSD=1.1%),100.8%(RSD=0.62%)and 101.0%(RSD=0.70%);LOQs were 0.33,0.13 and 0.12 μg·mL^-1;LODs were 0.10,0.03 and 0.03 μg·mL^-1,respectively.The solution was stable within 72 h with good durability.The dissolutions were 92%,94% and 91% of labeled amount for amlodipine,valsartan and hydrochlorothiazide by the method. Conclusion: The method is suitable to determine the dissolution of compound amlodipine,valsartan and hydrochlorothiazide tablets.