[4-(4-氟苯基)-6-异丙基-2-(N-甲基-N-甲磺酰基氨基)嘧啶-5-基]甲醇含量测定和有关物质检查

Study of the Content Determination of [4-(4-fluorophenyl)-6-isopropyl-2-(N-methyl-N-methylsulfonyl-amino) pyriminl-5-yl]methanol and Its Related Substances

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 the method for the content determination of [4-（4-fluorophenyl）-6-isopropyl-2-（N-meth- yl-N-methylsulfonyl-amino） pyriminl-5-yl]methanol （Rosuvastatin intermediate VI ） and its related substances. METHODS： HPLC method was adopted to determine the contents of main component and related substance in 3 batches of samples. A Grace-alltima C18 column was used, the mobile phase was acetonitrile-0.025 mol-L-1 NaH2PO4（57：43）. The determination wavelength was 235 nm for main component and 220 nm for related substances. The flow rate was 1.0 mL. min-1 and the column temperature was 25 -2. RESULTS： Main component and related substance were separated completely; the linear range of main component was 65.20--391.18 μg. mL-1 （r=0.999 9）, and recoveries of low, medium and high concentrations were 99.16%, 98.73% and 100.59% （RSD=0.59%, 0.67%, 1.06% ）. The detection limit of related substances was 195.8 ng.mL-1. The contents of main component in 3 batches of samples were 98.48%, 99.32%, 98.14%. The contents of related substance were 0.17%, 0.13% and 0.17%. CONCLUSION： The established method is accurate, reliable and specific, and it could be used for quality control of Rosuvastatin intermediate VI.