高效液相色谱法测定复方非洛地平缓释片的含量及有关物质

Determination of Contents and Related Substances of Felodipine and Metoprolol Tartrate in Compound Felodipine Sustained-Release Tablets by HPLC

目的建立复方非洛地平缓释片中非洛地平和酒石酸美托洛尔的含量及有关物质检测方法。方法采用高效液相色谱法,非洛地平的检测条件为：Agilent Eclipse XDB-C18色谱柱（4.6 mm×150 mm,5μm）,流动相为甲醇-乙腈-水（50∶20∶30）,流速1.0 mL·min^-1,检测波长238 nm,柱温25℃,进样量20μL;美托洛尔的检测条件为：Agela Venusil MP C18色谱柱（4.6mm×150 mm,5μm）,流动相为0.48%乙酸铵溶液（用三乙胺和冰醋酸调节p H至7.5）-乙腈-甲醇（65∶20∶15）,流速1.0 mL·min^-1,检测波长275 nm,柱温30℃,进样量20μL。结果非洛地平和酒石酸美托洛尔的线性范围分别为0.005～0.06 mg·mL^-1和0.05～0.60 mg·mL^-1,平均回收率分别为100.70%和99.62%,RSD分别为0.53%和0.85%（n=9）。结论本方法可用于测定该制剂中的含量及有关物质。

OBJECTIVE To establish an HPLC method for determining the contents and related substances of felodipine and metoprolol tartrate in compound felodipine sustained-release tablets. METHODS The analysis of felodipine was performed on an Agilent Eclipse XDB-C18column（ 4. 6 mm × 150 mm,5 μm）,using a mobile phase of methanol-acetonitrile-water（ 50 ∶ 20 ∶ 30） at the flow rate of 1. 0 mL·min^-1. The column temperature was maintained at 25 ℃. The detection wavelength was set at 238 nm and injection volume was 20 μL. The analysis of metoprolol tartrate was performed on an Agela Venusil MP C18column（ 4. 6 mm × 150 mm,5μm）,using a mobile phase of 0. 48% ammonium acetate（ p H adjusted to 7. 5 with triethylamine and glacial acetic acid）-acetonitrilemethanol（ 65∶ 20∶ 15） at the flow rate of 1. 0 mL·min^-1. The column temperature was maintained at 30 ℃. The detection wavelength was set at 275 nm and injection volume was 20 μL. RESULTS The linear ranges of felodipine and metoprolol tartrate were 0. 005-0. 06 mg · mL^-1and 0. 05- 0. 60 mg · mL^-1,respectively. The average recoveries of felodipine and metoprolol tartrate were100. 70% and 99. 62%,respectively. The RSDs of this method were all less than 2%（ n = 9）. CONCLUSION The method is applicable for the contents and related substances control of compound felodipine sustained-release tablets.