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SIPI-4884是由本室自主研发的降血脂候选新药。本研究以其合成路线中的各中间体及可能的副产物或降解产物为对象,建立了高效液相色谱法检测有关物质。采用C18色谱柱,以四氢呋喃-甲醇-0.02 mol/L乙酸铵缓冲液(用乙酸调至pH 4.5)(13︰48︰39)为流动相,检测波长255 nm,以检测非手性有关物质。SIPI-4884对映异构体的色谱条件为:CHIRALCEL AS-H色谱柱,流动相为正己烷-乙醇-三氟乙酸(80︰20︰0.1),检测波长255 nm。3批样品的总杂质量都小于1%,其中最大杂质是5-羰基物。
SIPI-4884 is a hypoglycemic candidate developed by our laboratory. In this study, the synthesis of various intermediates and possible by-products or degradation products as the object, the establishment of high performance liquid chromatography detection of related substances. The mobile phase was C18 with tetrahydrofuran-methanol-0.02 mol / L ammonium acetate buffer (adjusted to pH 4.5 with acetic acid) (13: 48︰39). The detection wavelength was set at 255 nm to detect achiral related substances. The chromatographic conditions for the SIPI-4884 enantiomer were: CHIRALCEL AS-H with a mobile phase of n-hexane-ethanol-trifluoroacetic acid (80:20:0.1) at a detection wavelength of 255 nm. Three batches of samples had less than 1% total impurities, of which the largest impurity was 5-carbonyl.