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目的:建立同时测定磷酸萘酚喹中有关物质和含量的高效液相色谱方法,为该原料药的质量控制提供了有效的分析方法。方法:Agilent SB-C8柱(150 mm×4.6 mm,5μm);流动相组成A:0.1%三氟乙酸溶液(三乙胺调节pH=3.0),B:乙腈,有关物质梯度洗脱,流速为1.0 mL.min-1,含量测定等度洗脱,流速为0.5 mL.min-1;检测波长为275 nm,柱温为35℃。结果:合成中间体Ⅰ~Ⅳ分别在2.057~51.428,2.333~58.336,1.766~44.140和2.113~52.828μg.mL-1的浓度范围内均有良好的线性关系,平均回收率均在96.1%~99.6%,RSD均在0.8%~3.0%,最低检测限均在0.5~8.8 ng;磷酸萘酚喹的线性范围为114.16~266.38μg.mL-1(r=0.999 9),低、中、高3个浓度RSD为0.24%(n=9)。结论:该方法灵敏、准确、专属性高,可用于磷酸萘酚喹的质量控制。
OBJECTIVE: To establish a high performance liquid chromatography (HPLC) method for the simultaneous determination of related substances and their contents in naphthoquine phosphate, and to provide an effective analytical method for the quality control of this raw material drug. Methods: Agilent SB-C8 column (150 mm × 4.6 mm, 5 μm); mobile phase A: 0.1% trifluoroacetic acid solution (adjusted to pH 3.0 with triethylamine); B: acetonitrile, gradient elution of related substances 1.0 mL.min-1, the content of isocratic elution, the flow rate of 0.5 mL.min-1; detection wavelength was 275 nm, the column temperature was 35 ℃. Results: The synthetic intermediates Ⅰ ~ Ⅳ had good linearity in the range of 2.057 ~ 51.428, 2.333 ~ 58.336, 1.766 ~ 44.140 and 2.113 ~ 52.828μg.mL-1, respectively.The average recoveries ranged from 96.1% to 99.6 %, RSD 0.8% -3.0%, the lowest detection limits were 0.5 ~ 8.8 ng; naphthoquine phosphate linear range of 114.16 ~ 266.38μg.mL-1 (r = 0.999 9), low, medium and high 3 The concentration RSD was 0.24% (n = 9). Conclusion: The method is sensitive, accurate and specific and can be used for quality control of naphthoquine phosphate.