目的：建立青蒿素哌喹片中哌喹的含量测定及有关物质的检测方法，并建立哌喹有关物质限度。方法：采用高效液相色谱法，色谱柱为SHISEIDO CAPCELL PAK C18（4.6 mm×250 mm，5 μm），以乙腈∶0.1%三氯乙酸溶液∶三乙胺（18∶82∶0.2，磷酸调节pH至2.5）为流动相，柱温为30℃，流速为1.0 mL·min-1，检测波长为216 nm（有关物质测定）和237 nm（含量测定）。结果：哌喹与各主要杂质及强制破坏产生的降解产物的杂质峰均分离良好，哌喹在0.01-0.2 mg·mL-1范围内与峰面积线性关系良好，R2=0.999 9，回收率为98.14%（RSD=0.77%，n=9），最低检出限为0.06 μg·mL-1，供试品溶液在12 h内稳定。结论：该方法专属性强，准确、灵敏，可用于青蒿素哌喹片中哌喹含量测定和有关物质检测。

This study was aimed to establish determination method of content and related substances of piperaquine in Artemisinin and Piperaquine Tablets, and to set the limit of related substance. HPLC was adopted on a SHISEIDO CAPCELL PAK C18 (4.6 mm×250 mm, 5 μm) using an isocratic mobile phase consisted of acetonitrile∶0.1% trichloroaceticacid∶triethylamine (18∶82∶0.2, V∶V∶V, pH 2.5) with a flow rate of 1.0 mL/min. The column temperature was kept at 30℃ and the detection wavelength was set at 216 and 237 nm, separately for the determination of related substance and content. The results showed that piperaquine and its related impurity can be separated effectively. The concentration-response relationship was linear over the range of 0.01-0.2 mg/mL (R2=0.999 9). The average recovery rate was 98.14% (RSD=0.77%, n=9). The minimum detection limit was 0.06 μg/mL. The solution was stable for 12 h. It was concluded that the method was specific, accurate, sensitive and suitable for the determination of content and related substances of piperaquine in Artemisinin and Piperaquine Tablets.

国家药典委员会中国全球基金TB结核病项目（2010-2013）：卫生系统加强（HSS）药品质量标准提高项目，负责人：王平。