HPLC法测定盐酸氯卡色林原料药中的有关物质

摘要

OBJECTIVE:To establish a method for the determination of related substances in lorcaserin hydrochloride.METHODS:HPLC method was adopted.The determination was performed on Welch ultimate XB-ODS column with mobile phase consisted of Sodium dihydrogen phosphate (pH =6.5)-acetonitrile (gradient elution) at the flow rate of 1.0 mL/min.The detection wavelength was set at 220 nm,and column temperature was 35 ℃.The sample size was 20 μL.RESULTS:The linear ranges of impurity 1,2,3 were 0.075 60-7.560 μg/mL(r=0.999 9),0.081 40-8.140 μg/mL(r=0.999 9),0.099 24-9.924 μg/mL(r=0.999 9),respectively.The limits of quantification were 0.075 60,0.081 40,0.099 25 μg/mL.The limits of detection were 0.022 68,0.024 42,0.029 77 μg/mL.RSD of precision test was lower than 2.0％.Impurity 1 was found in stability test and reproducibility test,RSD＜2.0％.The recoveries were 98.53％-102.45％ (RSD=1.06％,n=9),98.26％-101.64％ (RSD=1.03 ％,n=9),100.08％-102.10％ (RSD=0.70％,n=9),respectively.CONCLUSIONS:The method is sensitive,rapid,accurate and reliable,which can be used to determine the related substances of lorcaserin hydrochloride.%目的:建立测定盐酸氯卡色林原料药中有关物质的方法.方法:采用高效液相色谱法.色谱柱为Welch ultimate XB-ODS,流动相为磷酸二氢钠溶液(pH为6.5)-乙腈(梯度洗脱),流速为1.0 mL/min,检测波长为220 nrn,柱温为35 ℃,进样量为20 μL.结果:杂质1、2、3检测质量浓度线性范围分别为0.075 60～7.560 μg/mL(r=0.999 9)、0.081 40～8.140 μg/mL(r=0.999 9)、0.099 24～9.924 μg/mL(r=0.999 9);定量限分别为0.075 60、0.081 40、0.099 25.μg/mL,检测限分别为0.022 68、0.024 42、0.029 77μg/mL;精密度试验的RSD＜2.0％,稳定性、重复性试验只检出杂质1,RSD＜2.0％;回收率分别为98.53％～102.45％ (RSD=1.06％,n=9)、98.26％～101.64％(RSD=1.03％,n=9)、100.08％～102.10％(RSD=0.70％,n=9).结论:该方法灵敏、快速、准确、可靠,可用于盐酸氯卡色林原料药中有关物质的测定.