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目的:建立同时测定磷酸哌喹有关物质与含量的HPLC方法。方法:采用反相高效液相色谱法,测定磷酸哌喹有关物质与含量,并分别计算其杂质A~I的相对保留时间及校正因子。色谱条件:采用Welch Ultimate XBC18(100mm×4.6mm,3μm)柱,以0.1%三氟乙酸水溶液为流动相A,以乙腈为流动相B,线性梯度洗脱。流速1.5ml·min~(-1),柱温35℃,检测波长240nm。结果:磷酸哌喹与其各杂质峰分离度良好;磷酸哌喹与杂质A~I在各自线性范围内线性关系良好(r=0.9999);磷酸哌喹,杂质A~I的检测限分别为3.4 ng·ml~(-1)、1.0 ng·ml~(-1)、4.9 ng·ml~(-1)、3.1 ng·ml~(-1)、1.4 ng·ml~(-1)、3.8 ng·ml~(-1)、1.7 ng·ml~(-1)、2.8 ng·ml~(-1)、1.9 ng·ml~(-1)、2.0 ng·ml~(-1);杂质A~I加样回收率在95.5%~99.4%之间,RSD(n=9)分别为2.8%、2.7%、1.9%、3.5%、1.8%、1.8%、1.8%、2.5%、1.1%;3批样品含量测定结果分别为99.9%,99.6%和99.8%。供试品溶液在24小时内稳定。结论:本方法灵敏度好,操作简便,结果准确,可作为磷酸哌喹的质量控制。
Objective: To establish an HPLC method for simultaneous determination of related substances and contents of piperaquine phosphate. Methods: The related substances and contents of piperaquine phosphate were determined by reversed-phase high-performance liquid chromatography. The relative retention time and calibration factor of impurity A ~ I were calculated. Chromatographic conditions: A linear gradient was performed on a Welch Ultimate XBC18 (100 mm × 4.6 mm, 3 μm) column using 0.1% trifluoroacetic acid in water as mobile phase A and acetonitrile as mobile phase B. The flow rate was 1.5ml · min -1, the column temperature was 35 ℃ and the detection wavelength was 240nm. Results: The calibration curve of piperaquine phosphate and its impurity peaks was good. The linear relationship between piperaquine phosphate and impurity A ~ I was good (r = 0.9999). The detection limits of piperaquine phosphate and impurity A ~ I were 3.4 ng · Ml -1, 1.0 ng · ml -1, 4.9 ng · ml -1, 3.1 ng · ml -1, 1.4 ng · ml -1, 3.8 ng Ml -1, 1.7 ng · ml -1, 2.8 ng · ml -1, 1.9 ng · ml -1, 2.0 ng · ml -1, and impurity A ~ I recoveries ranged from 95.5% to 99.4%, RSD (n = 9) were 2.8%, 2.7%, 1.9%, 3.5%, 1.8%, 1.8%, 1.8%, 2.5% and 1.1%, respectively. The results of three batches of samples were 99.9%, 99.6% and 99.8%, respectively. The test solution is stable within 24 hours. Conclusion: The method has good sensitivity, simple operation and accurate results, which can be used as the quality control of piperaquine phosphate.