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目的建立复方美托拉宗片中美托拉宗和缬沙坦相关物质的HPLC测定方法。方法采用Agilent Eclipse SBC18色谱柱(4.6 mm×250 mm,5μm),以0.01 mol/L磷酸二氢钾溶液(pH=3.5)-乙腈为流动相,梯度洗脱,流速:1.0 ml/min,柱温:30℃,检测波长:237 nm,进样量:20μl。结果美托拉宗、缬沙坦及其相关物质之间分离度良好;美托拉宗在3~30μg/ml、缬沙坦在0.1~2.0μg/ml、缬沙坦杂质B在0.08~2.0μg/ml范围内峰面积与浓度线性关系良好;其平均回收率分别为102.97%、100.81%和100.44%;该法的重复性及中间精密度均符合要求;检测用溶液在室温条件下放置24 h稳定。结论该法专属性强、灵敏度高、准确可靠,可用于复方美托拉宗片中美托拉宗和缬沙坦相关物质测定。
OBJECTIVE To establish a HPLC method for the determination of the related substances of melatonid and valsartan in compound metolazone. Methods The mobile phase was eluted with an Agilent Eclipse SBC18 column (4.6 mm × 250 mm, 5 μm) using 0.01 mol / L potassium dihydrogen phosphate solution (pH = 3.5) - acetonitrile as the mobile phase at a flow rate of 1.0 ml / min. Temperature: 30 ℃, detection wavelength: 237 nm, injection volume: 20μl. Results The separation between metolazone, valsartan and its related substances was good; metolazone at 3 ~ 30μg / ml, valsartan at 0.1 ~ 2.0μg / ml, valsartan impurity B at 0.08 ~ 2.0 μg / ml peak area and concentration of a good linear relationship; the average recovery rates were 102.97%, 100.81% and 100.44%, respectively; the repeatability and precision of the method are in line with the requirements; test solution at room temperature for 24 h stable. Conclusion The method is highly specific, sensitive, accurate and reliable and can be used for the determination of related substances of melatonin and valsartan in compound metolazone.