RP-HPLC测定盐酸西布曲明中的有关物质

Determination of related substances in sibutramine hydrochloride by RP-HPLC

目的 建立盐酸西布曲明原料中有关物质的检查方法。方法 色谱柱为HPODShypersil (5 μm ,12. 5mm×4mm) ,流动相为甲醇-水-三乙胺(85∶15∶0 . 0 1) (含0 .0 0 1mol·L-1庚烷磺酸钠,醋酸调pH 7.8) ,检测波长2 2 2nm ,流速1.0ml·L-1。结果 合成反应中的两个重要中间体与破坏产生的降解产物均能有效地分离,中间体的最低检出量为0 .1ng,控制总杂质量不得过2 .0 %。结论 该方法简便、准确、有效。

OBJECTIVE To establish a method for the determination of related substances in sibutramine hydrochloride.METHODS RP-HPLC method was adopted.The column was HP ODS hypersil (5 μm,125 mm×4 mm),and mobile phase consisted of methanol-water-triethylamine (85∶15∶0.01)[(containing 0.001 mol·L -1 sodium heptanesulfonate )adjusted to pH 7.8 with acetic acid]. The detective wavelength was 222 nm with a flow rate of 1.0 ml·min -1.RESULTS A satisfactory separation among two related impurities was obtained and the LOD of intermediate was 0.1 ng.CONCLUSION The method was simple,accrate and available.