保泰松糖衣片剂中保泰松含量测定的高效液相色谱法改进

Content Determination of Phenylbutazone in Phenylbutazone Tablets by Improved HPLC

目的改进测定保泰松片剂中保泰松含量的高效液相色谱法。方法色谱柱采用Agilent Eclipse XDB-C_(18)柱(250 mm×4.6 mm,5μm),流动相为醋酸钠缓冲液(取醋酸钠2.72 g,加水700 mL溶解,用冰醋酸调节pH至4.1,加水至1000 mL,摇匀)-乙腈(30∶70,V/V),流速为1.0 mL/min,检测波长为240 nm,柱温为30℃,进样量为20μL。结果保泰松主峰能与已知杂质有效分离。保泰松检测质量浓度线性范围为0.01~0.30 g/L(r=0.9999),精密度、稳定性、重复性试验的RSD均小于2.0%(n=6);加样回收率为99.00%~101.66%,RSD为1.41%(n=9)。结论改进方法灵敏度更高,重复性更好,适用于测定保泰松片中保泰松的含量。

Objective To improve the method of content determination of phenylbutazone in Phenylbutazone Tablets. Methods The Agilent Eclipse XDB-C18 column（ 250 mm × 4. 6 mm,5 μm） was adopted,the mobile phase was sodium acetate buffer（ 2. 72 g sodium acetate was taken and dissolved with 700 mL of water,the p H was adjusted to 4. 1 with glacial acetic acid,the water was added to 1 000 mL and shaken well）-acetonitrile（ 30 ∶ 70, V/V）, the flow rate was 1. 0 mL/min, the detection wavelength was 240 nm, the column temperature was 30 ℃,and the injection volume was 20 μL. Results Phenylbutazone could effective separate from the known impurities.The linear range of phenylbutazone was 0. 01-0. 30 g/L（ r = 0. 9999）; RSDs of precision, stability and reproducibility tests were lower than 2. 0%（ n = 6）, the recovery was 99. 00%-101. 66%, RSD = 1. 41%（ n = 9）. Conclusion The improved method is more sensitive and reproducible,which is suitable for content determination of phenylbutazone in Phenylbutazone Tablets.