【摘要】 目的:建立 HPLC 法测定国产甲磺酸多拉司琼的有关物质,并初步考察其稳定性。方法:Diamonsil C₈（4.6 mm×250mm,5μm）色谱性;线性梯度洗脱,流动相 A 为0.008 mol·L^-1磷酸氢二铵溶液（磷酸调 pH 至7.0）-乙腈（200:16）,流动相B为0.008 mol·L^-1磷酸氢二铵溶液（磷酸调 pH 至7.0）-乙腈（60:160）;流速为1.0 mL·min^-1;检测波长为210 nm;柱温为25℃;进样量为100 μL。结果:建立了 HPLC 法,可同时测定甲磺酸多拉司琼中甲磺酸多拉司琼有关物质 A 和其他杂质的含量。有关物质 A 浓度在0.36～14.4μg·mL^-1范围内与峰面积呈良好的线性关系,回归方程为 Y=1.169×10^-4X-1.491×10³,r=0.9993,最低检测限为120 ng,回收率（n=9）为100.0%。对甲磺酸多拉司琼的稳定性进行了初步考察,在光照条件下,有关物质稍有变化;高湿条件下,性状稍有变化;在其他影响因素试验、加速试验和长期试验中,甲磺酸多拉司琼的性状和有关物质均无明显变化,表明甲磺酸多拉司琼在贮藏过程中基本稳定。结论:该法方法简便、快速、准确,适合该药生产和制剂的质量控制。更多还原

【Abstract】 Objective:To establish an HPLC method for assay the related substances in domestic dolasetron mesylate and to study its stability,nethod:A Diamonsil C₈（4.6 mm×250 mm,5μm）column was used for the gradient elution.The mobile phase A was 0.008 mol·L^-1 dibasic ammonium phosphate solution（adjust to pH 7.0 with phosphoric acid）-acetonitrile（200:16）;The mobile phase B was 0.008 mol·L^-1 dibasic ammonium phos- phate solution（adjust to pH 7.0 with phosphoric acid）-acetonitrile（60:160）.The flow rate was 1.0 mL·min^-1, the detective wavelength was 210 nm,the column temperature was 25℃,the injection volume was 100μL.Re- suits:Dolasetron mesylate related compound A and other related substances were detected by the established meth- od.The calibration curve was linear in the concentration range of 0.36-14.4μg·mL^-1（r=0.9993）for dolase- tron mesylate related compound A and the regression equation being Y=1.169×10⁴X-1.491×10³,and the de- tection limit was 120 ng;The recovery（n=9）of assay was 100.0%.The stability of dolasetron mesylate was stud- ied.It can be concluded that:under light conditions,the content of related substances was slightly changed;under high humidity conditions its appearance was slightly changed;in other tests including accelerated test and long- term test,its appearance and content were not obviously changed.Conclusion:This method is simple,convenient, fast,accurate,and can be applied for manufacture and quality control of the preparation.更多还原