摘要
目的建立了同时检测利鲁唑中9种杂质的超高效液相色谱-紫外检测法。方法采用Phenomenex Kinetex XB-C_(18)色谱柱(4.6×100mm,2.6μm),以0.05%三氟乙酸溶液(A)和甲醇(B)为流动相,梯度洗脱,流速0.7 m L·min^(-1),检测波长221 nm,柱温30℃。结果利鲁唑及9种杂质能完全分离;主物质及各杂质在测定浓度范围内线性关系良好(r>0.995);主物质及各杂质检测限为0.003~0.059μg·m L^(-1),定量限为0.010~0.176μg·m L^(-1),灵敏度较好;稳定性、重复性、精密度、耐用性良好;主物质及9种杂质加标回收率为93.804%~107.339%,准确度良好。结论该方法操作简单、选择性好、灵敏度高,可用于利鲁唑有关物质的测定,为利鲁唑质量控制提供参考。
OBJECTIVE To establish a method for the simultaneous determination of nine impurities of riluzole by UPLC.METHODS The separation was performed on a Phenomenex Kinetex XB-C_(18)(4.6×100 mm,2.6μm) at30℃with the mobile phase consisting of 0.05%trifluoroacetic acid (A) and methanol (B) by gradient elution at a flow rate of 0.7 m L·min^(-1).RESULTS The riluzole and nine impurities could be completely separated;the main substance and nine impurities had excellent linear relationships within the tested range (r>0.995);the detection limits of the main component and impurities were 0.003-0.059μg·m L^(-1),the quantitation limits were 0.010-0.176μg·m L^(-1);This method had good stability,repeatability,precision and durability with RSD value less than10%;the recovery rate were 93.804%-107.339%.CONCLUSION The method is simple and accurate with high specificity which could be used for the determination of the related substances of riluzole and provides a reference for the quality control of riluzole.
作者
左翠霞
孙建之
刘彩云
闫丽
张冲
周俊瑞
胡娅娅
刘思光
张贵民
ZUO Cui-xia;SUN Jian-zhi;LIU Cai-yun;YAN Li;ZHANG Chong;ZHOU Jun-rui;HU Ya-ya;LIU Si-guang;ZHANG Gui-min(Shandong New Time Pharmaceutical Co,Ltd,Linyi 273400,China;Lunan Pharmaceutical Group Co,Ltd,Linyi 276002,China;Nation Engineering and Technology Research Center of Chirality Pharmaceutical,Linyi 273400,China)
出处
《海峡药学》
2022年第10期40-44,共5页
Strait Pharmaceutical Journal
关键词
超高效液相色谱法
利鲁唑
有关物质
Ultra performance liquid chromatography
Riluzole
Related substances
