HPLC法同时测定磷酸哌喹有关物质与含量  

HPLC Determination of Piperaquine Phosphate Content and Its Related Substances

作　　者：黄军 Huang Jun(Guilin Pharmaceutical Co.,Ltd, Guilin, Guangxi 541004, China)

机构地区：[1]桂林南药股份有限公司,桂林541004

出　　处：《生命科学仪器》2016年第4期43-47,共5页Life Science Instruments

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.

关 键 词：磷酸哌喹 HPLC 有关物质 含量 

分 类 号：Q65[生物学—生物物理学]