依折麦布片有关物质的 HPLC 法测定

刘清梁, 赵丕华, 杨 琰, 王文峰

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主办:上海医药工业研究院
   中国药学会
   中国化学制药工业协会
ISSN 1001-8255   CN 31-1243/R   ZYGZEA
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中国医药工业杂志 ›› 2016, Vol. 47 ›› Issue (12) : 1573. DOI: 10.16522/j.cnki.cjph.2016.12.018
药品分析与质控 Analysis & Quality Control

依折麦布片有关物质的 HPLC 法测定

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Determination of the Related Substances in Ezetimibe Tablets by HPLC

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摘要

建立了高效液相色谱法测定依折麦布片的有关物质。采用Hypersil Gold C8 色谱柱,以甲醇∶ 0.05%三氟乙酸溶液(50 ∶ 50) 为流动相,检测波长232 nm。依折麦布与其非对映异构体[6,(3R,4S)-1-(4- 氟苯基)-3-[(3R)-3-(4- 氟苯基)-3-羟基丙基] -4-(4- 羟基苯基) -2- 氮杂环丁酮] 的分离度为1.8;依折麦布及其有关物质2、非对映异构体和有关物质3 分别在12 ~ 820、9.6 ~ 640、12 ~ 780 和12 ~ 780 ng/ml 范围内线性关系良好。上述有关物质的相对校正因子分别为0.8、1.0 和1.2;平均回收率分别为102.5%、104.4%和97.9%,RSD 分别为1.3%、1.7%和2.4%。

Abstract

An HPLC method was established for the determination of related substances in ezetimibe (1) tablets. A Hypersil Gold C8 column was used, with the mobile phase of methanol∶0.05% TFA (50∶50), at the detection wavelength of 232 nm. The resolution between 1 and its diastereoisomer [6, (3R,4S)-1-(4-fluorophenyl)-3-[(3R)-3-(4-
fluorophenyl)-3-hydroxypropyl]-4-(4-hydroxyphenyl)azetidin-2-one] was 1.8. It was linear for 1, the related substance 2, diastereoisomer 6 and the related substance 3 in the ranges of 12—820, 9.6—640, 12—780 and 12—780 ng/ml, respectively. Their relative correction factors were 0.8, 1.0 and 1.2. Their average recoveries were 102.5%, 104.4% and 97.9%, with RSDs of 1.3%, 1.7% and 2.4%, respectively.

关键词

依折麦布 / 有关物质 / 高效液相色谱法 / 含量测定

Key words

ezetimibe / related substance / HPLC / content determination

引用本文

导出引用
刘清梁, 赵丕华, 杨 琰, 王文峰. 依折麦布片有关物质的 HPLC 法测定. 中国医药工业杂志. 2016, 47(12): 1573 https://doi.org/10.16522/j.cnki.cjph.2016.12.018
LIU Qingliang, ZHAO Pihua, YANG Yan, WANG Wenf. Determination of the Related Substances in Ezetimibe Tablets by HPLC. Chinese Journal of Pharmaceuticals. 2016, 47(12): 1573 https://doi.org/10.16522/j.cnki.cjph.2016.12.018

参考文献

[1] FDA. Ezetimibe 10 mg. [EB/OL]. http://www.accessdata.fda.gov/drugsatfda_docs/nda/2002/21445_Zetia.cfm

[2] PMDA. エゼチミブ10 mg [EB/OL] . http://www.pmda.go.jp/drugs/2007/P200700023/index.htm

[3] 于振鹏, 刘 石, 谭相端, 等. 依折麦布的合成[J]. 中国医药工业杂志, 2013, 44(5): 424—428.

[4] 国家食品药品监督管理局. 进口药品注册标准,JX20070201, 依折麦布片[S]. 2007.

[5] 高 妍, 蒋玲敏, 张 蕾, 等. 一种依折麦布药物组合物的制备方法: 中国, 103655453A [P]. 2014-03-26.
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