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目的:建立[4-(4-氟苯基)-6-异丙基-2-(N-甲基-N-甲磺酰基氨基)嘧啶-5-基]甲醇(瑞舒伐他汀中间体Ⅵ)含量及其有关物质的测定方法。方法:采用高效液相色谱法检测3批样品中主成分和有关物质的含量。色谱柱为Grace-Alltima C18;流动相为乙腈-0.025mo·lL-1磷酸二氢钠溶液(57∶43);检测波长235nm为主成分测定波长,220nm为有关物质测定波长;流速为1.0mL·min-1;柱温为25℃。结果:主成分与其有关物质均能完全分离;主成分检测浓度线性范围为65.20～391.18μg·mL-1(r=0.9999);低、中、高3个浓度回收率分别为99.16%、98.73%、100.59%(RSD分别为0.59%、0.67%、1.06%)。有关物质检测限为195.8ng·mL-1。3批样品中主成分含量分别为98.48%、99.32%、98.14%,有关物质含量分别为0.17%、0.13%、0.17%。结论:本方法准确、可靠、专属性强,可用于瑞舒伐他汀中间体Ⅵ的含量测定及质量控制。
OBJECTIVE: To establish a method for the preparation of [4- (4-fluorophenyl) -6- isopropyl-2- (N -methyl- N- methanesulfonylamino) pyrimidin- 5-yl] methanol (rosuvastatin intermediate VI ) Content and determination of related substances. Methods: The contents of main components and related substances in three batches of samples were determined by high performance liquid chromatography. The column was Grace-Alltima C18; the mobile phase was acetonitrile-0.025mo · L-1 sodium phosphate monobasic solution (57:43); the detection wavelength was 235nm, the wavelength was 220nm, the flow rate was 1.0mL Min -1; column temperature 25 ° C. Results: The main components and their related substances could be completely separated. The linear range of the principal components detection was 65.20-391.18μg · mL-1 (r = 0.9999). The recoveries of low, medium and high concentrations were 99.16% and 98.73% , 100.59% (RSD 0.59%, 0.67%, 1.06% respectively). The limit of detection of the relevant substances was 195.8ng · mL-1.3. The contents of the main components in the batch samples were 98.48%, 99.32% and 98.14% respectively, and the related substances were 0.17%, 0.13% and 0.17% respectively. Conclusion: The method is accurate, reliable and specific. It can be used for the determination and quality control of rosuvastatin intermediate Ⅵ.