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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
参考文献:
[1] Kennedy B F, Loitsch S, McLaughlin R A, et al. Fibrinphantom for use in optical coherence tomography[J]. J Biomed Opt, 2010, 15(3):030507-1-030507-3.
[2] Matsukawa J, Hori Y, Nishida H, et al. A comparative study on the modes of action of TAK-438, a novel potassium-competitive acid blocker, and lansoprazole in primary cultured rabbit gastric glands[J]. Biochem Pharmacol, 2011, 81(9):1145-1151.
[3] 陈震. 有关物质的研究与新药注册[J]. 中国医药工业杂志, 2010, 41(11):872-876
[4] Sachs G, Shin J M, Munson K, et al. Gastric acid-dependent diseases:a twentieth-century revolution[J].Dig Dis Sci, 2014, 59(7):1358-1369.
[5] Takeda. Takecab (vonoprazan tablets):Japanese prescribing information. Japan Pharmaeutical and Medical Device Agency[EB/OL]. http://www.info.pmda.go.jp/downfiles/ph/PDF/400256_2329030F1020-1-04.pdf.
[6] Sachs G, Shin J M, Vagin O, et al. The gastric H, K ATPase as a drug target:past, present, and future[J]. J Clin Gastroenterol, 2007, 41(S2):S226-S242.
[7] 吕久安, 张凯, 张克军. 富马酸沃诺拉赞的合成研究[J].国际药学研究杂志, 2017, 9(44):890-893.
[8] 贲新琰.浅谈高效液相色谱法在药品检验中的体现[J].科技创新与应用, 2016(16):74.
[9] 国家药典委员会. 中华人民共和国药典[M].4部.2015:374-377.
[10] 郝文静, 张涛, 黄华, 等.HPLC法测定恩格列净片的有关物质[J].药物分析杂志, 2016, 36(5):902-910.
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