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高效液相色谱法测定匹伐他汀钙原料药中的有关物质

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  • 山东齐都药业有限公司,临淄 255400
第一作者 Tel:(0531)88998262;E-mail:qdrdkangle@163.com
*Tel:(0531)88998262;E-maill:qdrdliuyin@163.com

收稿日期: 2020-11-26

  网络出版日期: 2024-06-21

Determination of related substances of pitavastatin calcium by high performance liquid chromatography

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  • Shangdong Qidu Pharmaceutical Co., Ltd, Linzi 255400, China

Received date: 2020-11-26

  Online published: 2024-06-21

摘要

目的:建立高效液相色谱法测定匹伐他汀钙原料药中的11个有关物质。方法:采用ODS-3 C18色谱柱(250 mm×4.6 mm,5 μm),以乙酸-乙酸钠缓冲溶液(取超纯水1 000 mL,加冰乙酸0.6 mL,用0.1%乙酸钠溶液调节pH至2.5)为流动相A,乙腈为流动相B,梯度洗脱,流速1.0 mL·min-1,检测波长245 nm,柱温30 ℃。结果:匹伐他汀钙与各有关物质均在一定范围内线性关系良好且分离度均高于1.5;检测下限均不高于0.01 μg·mL-1;精密度试验中各有关物质含量回收率的RSD均不高于6%;各有关物质平均回收率在95.5%~110.2%,RSD均不高于5%;供试品溶液室温放置48 h内,除杂质A外,其他杂质均稳定;改变柱温、流速及更换色谱柱后,对有关物质的检测结果无影响。结论:本文所建立的高效液相色谱法简便、灵敏、准确,可用于匹伐他汀钙原料药中有关物质的检测,控制匹伐他汀钙原料药的质量。

本文引用格式

康乐, 林蒙, 孟凡领, 刘印 . 高效液相色谱法测定匹伐他汀钙原料药中的有关物质[J]. 药物分析杂志, 2021 , 41(10) : 1812 -1822 . DOI: 10.16155/j.0254-1793.2021.10.19

Abstract

Objective: To establish an HPLC method for simultaneous determination of the 11 related substances in pitavastatin calcium. Methods: ODS-3 C18 column (250 mm×4.6 mm, 5 μm) was adopted. The mobile phase A was composed of acetic acid-sodium acetate buffer (0.6 mL glacial acetic acid was added to 1 000 mL purified water, and pH was adjusted to 2.5 with 0.1% sodium acetate solution). And the mobile phase B was acetonitrile. The gradient elution was performed. The flow rate was 1.0 mL·min-1.The detection wavelength was 245 nm and the column temperature was 30 ℃. Results: Pitavastatin calcium and its related substances were separated well, the detection limits of pitavastatin calcium and impurities were all below 0.01 μg·mL-1. The RSD of the recoveries of relevant substances in precision tests were less than 6%. The recovery rates were between 95.5% and 110.2% and the RSD of each recovery rate was less than 5%. After the sample solution was placed at room temperature for 48 h, all impurities except impurity A were stable. Therefore, changing the column temperature, flow rate, and replacing the chromatographic column had no effect on the detection results of related substances. Conclusion: The established method is simple, sensitive and accurate, which can be used to determinate the related substances of pitavastatin calcium and to control the quality of pitavastatin calcium.

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