摘要
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 to determine piperaquine phosphate content and its related substances.Methods：Piperaquine phosphate content and its related substances were determined by RP-HPLC.The impurity A- I in piperaquine phosphate,the relative retention limes and the correction factors were determined respectively by HPLC.The chromatographic condition was as follows.The Welch Ultimate XB-C18 column（100mm x 4.6mm,3 u.m） was adopted,the mobile phase was 0.1%Trifluoroacetic Acid in water（A）- acetonitrile（B） with gradient elution at a flow rate of 1.5 ml · min^-1,the column temperature was 35℃,and the detection wavelength was 240 nm.Results：Piperaquine phosphate and the impurities were separated well.The calibration curves of nine impurities were linear in each concentration range（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^-1,3.8ng · ml^-1,1.7 ng · ml^-1,2.8 ng · ml^-1,1.9 ng · ml^-1,2.0 ng · ml^-1,respectively.All the average recoveries of the impurity A-I were 95.5%- 99.4%,and RSDs（n=9） were 2.8%,2.7%,1.9%,3.5%,1.8%,1.8%,1.8%,2.5%,1.1%.The content determination results for the 3 batches of samples were 99.9%,99.6%and 99.8%,respectively.The solution was stable for 24 h.Conclusion：The method is sensitive,easy,accurate and suitable for quality control of piperaquine phosphate.
作者
黄军
Huang Jun(Guilin Pharmaceutical Co.,Ltd, Guilin, Guangxi 541004, China)
出处
《生命科学仪器》
2016年第4期43-47,共5页
Life Science Instruments
关键词
磷酸哌喹
HPLC
有关物质
含量
Piperaquine phosphate
high performance liquid chromatography（HPLC）
related substances
content
