摘要
目的建立同时测定富马酸伏诺拉生中活性成分含量的高效液相色谱法,并评估其成盐率。方法色谱柱为Agilent 5 TC-C_(18)(2)柱(250 mm×4.6 mm,2.5μm),流动相为0.05 mol/L磷酸盐缓冲液(p H 6.8)-乙腈-甲醇(17∶7∶6,V/V/V),流速为1.0 m L/min,检测波长为230 nm,柱温为30℃,进样量为10μL。结果伏诺拉生和富马酸质量浓度分别在100~300μg/m L和34~102μg/m L范围内与峰面积线性关系良好(r=1.0000,0.9999,n=5);检测限分别为0.4,0.5 ng,定量限分别为1.0,1.4 ng;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为100.40%,100.22%,RSD分别为0.39%,0.35%(n=9)。9批样品中伏诺拉生含量为74.16%~75.83%,富马酸含量为24.55%~25.81%,成盐率为98.17%~101.79%。结论该方法操作简便、重复性好、结果准确可靠,可用于富马酸伏诺拉生中活性成分及盐基的含量测定。
Objective To establish a high-performance liquid chromatography(HPLC)method for the simultaneous determination of the active ingredients in vonoprazan fumarate,and to evaluate its salt-forming rate.Methods The chromatographic column was Agilent 5 TC C_(18)(2)column(250 mm×4.6 mm,2.5μm),the mobile phase was 0.05 mol/L phosphate buffer(pH 6.8)-acetonitrile-methanol(17∶7∶6,V/V/V),the flow rate was 1.0 mL/min,the detection wavelength was 230 nm,the column temperature was 30℃,and the injection volume was 10μL.Results The linear ranges of vonoprazan and fumaric acid were 100-300μg/mL and 34-102μg/mL(r=1.0000,0.9999,n=5).The limits of detection were 0.4 ng and 0.5 ng,respectively.The limits of quantification were 1.0 ng and 1.4 ng,respectively.The RSDs of precision,stability,and repeatability test results were lower than 2.0%.The average recoveries of vonoprazan and fumaric acid were 100.40%and 100.22%with RSDs of 0.39%and 0.35%(n=9),respectively.Among the nine batches of samples,the content of vonoprazan was in the range of 74.16%-75.83%,the content of fumaric acid was in the range of 24.55%-25.81%,and the salt-forming rate of vonoprazan fumarate was in the range of 98.17%-101.79%.Conclusion This method is simple,reproducible,accurate,and reliable,which can be used for the simultaneous determination of the active ingredients and base in vonoprazan fumarate.
作者
王玲兰
龚翠云
朱跃芳
朱婧
陈莉
宿亮
WANG Linglan;GONG Cuiyun;ZHU Yuefang;ZHU Jing;CHEN Li;SU Liang(Zhuzhou Qianjin Pharmaceutical Co.,Ltd.,Zhuzhou,Hunan,China 412000;Zhuzhou Institute for Food and Drug Control,Zhuzhou,Hunan,China 412000)
出处
《中国药业》
CAS
2023年第11期63-67,共5页
China Pharmaceuticals
基金
湖南省自然科学基金[2022JJ80049]。
