HPLC法测定富马酸沃诺拉赞原料药中吡啶-3-磺酸的含量-今日药学

HPLC法测定富马酸沃诺拉赞原料药中吡啶-3-磺酸的含量

作者：乐志艳¹ 肖敏¹ 方潇颖²

单位：1. 江西省抚州市食品药品检验所, 江西抚州 344000;
2. 江西中医药大学, 江西南昌 330004

关键词：吡啶-3-磺酸富马酸沃诺拉赞有关物质方法学验证高效液相色谱法

中图分类号：R927.2

文献标志码：

出版年,卷(期):页码：2019,29(1):17-20,

收稿日期：2018-5-30

摘要：

目的建立测定富马酸沃诺拉赞原料药中吡啶-3-磺酸的高效液相色谱（HPLC）法。方法色谱柱为Inertsil ODS-3 C₁₈柱（4.6 mm×150 mm，5 μm），以0.025 mol·L^-1磷酸钠溶液（用磷酸调节pH值至6.8）-乙腈（98：2，V/V）为流动相A，乙腈为流动相B，进行线性梯度洗脱，检测波长为210 nm，柱温为25℃，流速1.0 mL·min^-1，进样量20 μL。结果在选定的色谱条件下，吡啶-3-磺酸与相邻色谱峰分离良好，在0.1974~1.9743 μg·mL^-1浓度范围内与峰面积呈良好的线性关系，线性方程为Y=41638X+1137.5，相关系数r=0.9998；平均回收率为103.6%，RSD%为1.34%（n=12）；6批样品中吡啶-3-磺酸的含量分别为0.0018%、0.0017%、0.0015%、0.001%、0.004%及0.004%。结论本方法精密度良好，灵敏度高，准确度好，适用于富马酸沃诺拉赞原料药中吡啶-3-磺酸的检测。

OBJECTIVE To establish an HPLC method for the determination of pyridine-3-sulfonic acid in vonoprazan fumarate. METHODS Inertsil ODS-3 C₁₈(4.6 mm×150 mm, 5 μm)column was used, 0.025 mol·L^-1 sodium phosphate solution(pH adjusted to 6.8 with phosphori acid)￣acetonitrile(98:2,V/V) as mobile phase A, acetonitrile as mobile phase B, using linear gradient elution. The detection wavelength was 210 nm, column temperature was 25℃, flow rate was 1.0 mL·min^-1 and the sample volume was 20 μL. RESULTS Under the selected chromatographic conditions, pyridine-3-sulfonic acid was separated from adjacent chromatographic peaks, the concentration in the range of 0.197 4 -1.974 3 μg·mL^-1 had good linear relationship with the peak area, the linear equation was Y=41 638X+1 137.5, the correlation coefficient was r=0.999 8. The average recovery rate was 103.6% and RSD% was 1.34% (n=12).The content of pyridine-3-sulfonic acid in 6 batches of samples were 0.001 8%, 0.001 7%, 0.001 5%, 0.001%, 0.004% and 0.004% respectively. CONCLUSION The method has been verified by methodology, and the method has good precision, high sensitivity and good accuracy. It is suitable for the detection of pyridine-3-sulfonic acid in the vonoprazan fumarate.

基金项目：

作者简介：

乐志艳,主管中药师,研究方向:食品药品检验及检验结果质量控制方面,E-mail:112177269@qq.com

通讯作者：肖敏,副主任药师,研究方向:食品药品检验及检验结果质量控制方面,Tel:0794:8211979,E-mail:709972742@qq.com

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