超高效液相色谱法测定利鲁唑有关物质  

Determination of the Related Substances in Riluzole by UPLC

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)

机构地区：[1]山东新时代药业有限公司,山东临沂273400 [2]鲁南制药集团股份有限公司,山东临沂276002 [3]国家手性制药工程技术研究中心,山东临沂273400

出　　处：《海峡药学》2022年第10期40-44,共5页Strait Pharmaceutical Journal

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.

关 键 词：超高效液相色谱法 利鲁唑 有关物质 

分 类 号：R927[医药卫生—药学]