高效液相法测定复方磷酸哌喹片中磷酸哌喹的含量

 目的 建立高效液相色谱法测定复方磷酸哌喹片中磷酸哌喹含量的方法。方法 采用Luna C₁₈色谱柱（4.6 mm×250 mm，5 μm）；流动相为乙腈-水（13∶87，每100 mL水含三氟乙酸50 μL，磷酸40 μL，三乙胺50 μL）；柱温30 ℃；流速1.0 mL·min-1；检测波长345 nm。样品分析结果与药品标准中非水滴定法对照。结果 磷酸哌喹在0.08～0.80 g·L-1内呈现良好的线性关系，r=0.999 9；精密度RSD为0.79% （n=6）；低、中、高3种浓度的回收率分别为105.2%，100.6%，103.6%，RSD分别为0.52%，0.31%，0.28%。结论 与药品标准非水滴定法相比，高效液相色谱法操作简便，节省时间，利于卫生环保；而且专属性强，重现性好，准确度高。

Determination of Piperaquine Phosphate in Compound Piperaquine Phosphate Tablets by RP-HPLC

OBJECTIVE To establish a method for the determination the content of piperaquine phosphate in compound piperaquine phosphate tablets by high-performance liquid chromatography. METHODS The analytical column was packed with phenomenex-Luna C_l8 (4.6 mm×250 mm，5 μm) and performed at 30 ℃. The mobile phase consisted of acetonitrile-water (13∶87). To 100 mL of the water in mobile phase, 50 μL of trifluoroacetic acid, 40 μL of phosphoric acid and 50 μL of triethylamine were added. The flow rate was 1.0 mL·min-1. The detector was at 345 nm. The injection volume was 10 μL. The results were compared with those of original drug standard. RESULTS The calibration curve was linear over the range of 0.08-0.80 g·L-1 with the correlation coefficient of 0.999 9. The RSD of precision was 0.79% (n=6). The recoveries at low, middle and high concentration were 105.2%，100.6%，103.6%, and the corresponding RSDs were 0.52%, 0.31%, 0.28%, respectively.CONCLUSION Compared with non-aqueous titration assay, HPLC assay is simple, rapid, accurate and specific.