摘要
目的:建立高效液相色谱法控制原料药托拉塞米中起始原料4-羟基吡啶与间甲苯胺的残留量的分析方法。方法:采用AgilentC18柱,以0.02mol/L磷酸二氢钾溶液-甲醇(3∶2)为流动相,检测波长240nm,流速为1.5ml/min,柱温为室温。结果:两种物质4-羟基吡啶浓度为0.014～1.244μg/ml,间甲苯胺浓度为0.081～1.317μg/ml的溶液的峰面积与浓度成线性关系,相关系数r≥0.99;定量限和检测限试验中,信噪比符合规定,能够达到定量检测及检出的要求;各浓度下的4-羟基吡啶、间甲苯胺平均回收率均在90%～110%范围内,且9个回收率的RSD均小于5.0%。结论:该方法专属性好,精密度、准确度都符合要求,方法可靠,可用于原料药托拉塞米中起始原料4-羟基吡啶与间甲苯胺的残留量的控制。
Objective：To establish a HPLC method to determine the content of the residual starting materials, 4-hydrox- ypyridine and m-tuloidine, in torasemide drug substance. Methods：The Agilent ClS column （15 cmx4.6 mm×5.0 μm） was used. The mobile phase was methanol-dibasic potassium phosphate（2：3）. The detection wavelength was at 240 nm. The flow rate was 1.5 ml/min. Results：The calibration curves were linear within the range of 0.014-1.244 μg/ml （r=0.999 8） for 4- hydroxypyridine and 0.081-1.317 μg/ml （r=0.999 8） for m-tuloidine, respectively. The average recoveries were 90%-110% （n=9） for 4-hydroxypyridine and for m-tuloidine, respectively. Conclusion：The method is simple,sensitive, accurate and suitable for the quality control of this drug substance.
出处
《中国医药导报》
CAS
2008年第26期33-34,36,共3页
China Medical Herald
