阿司匹林丁香酚酯颗粒剂有关物质检测方法的建立与验证

doi:10.11843/j.issn.0366-6964.2023.08.034

畜牧兽医学报 ›› 2023, Vol. 54 ›› Issue (8): 3500-3509.doi: 10.11843/j.issn.0366-6964.2023.08.034

阿司匹林丁香酚酯颗粒剂有关物质检测方法的建立与验证

王志霞, 白莉霞, 秦哲, 刘希望, 杨亚军, 李世宏, 葛闻博, 李剑勇*

中国农业科学院兰州畜牧与兽药研究所/农业农村部兽用药物创制重点实验室/甘肃省新兽药工程重点实验室, 兰州 730050

收稿日期:2022-11-23 出版日期:2023-08-23 发布日期:2023-08-22
通讯作者: 李剑勇,主要从事兽医药理学研究,E-mail:lijy1971@163.com
作者简介:王志霞(1992-),女,甘肃平凉人,硕士,主要从事新兽药开发研究,E-mail:wzx142893@163.com;白莉霞(1993-),女,甘肃兰州人,实习研究员,硕士,主要从事新兽药开发研究,E-mail:bailx552369@163.com。
基金资助:
中国农业科技创新工程（CAAS-25-LZIHPS-02）

Establishment and Validation of the Determination Method for the Related Substances in Aspirin Eugenol Ester Granules

WANG Zhixia, BAI Lixia, QIN Zhe, LIU Xiwang, YANG Yajun, LI Shihong, GE Wenbo, LI Jianyong*

Key Laboratory of New Animal Drug Project of Gansu Province, Key Laboratory of Veterinary Pharmaceutical Development of Ministry of Agriculture and Rural Affairs, Lanzhou Institute of Husbandry and Pharmaceutical Sciences, Chinese Academy of Agricultural Sciences, Lanzhou 730050, China

Received:2022-11-23 Online:2023-08-23 Published:2023-08-22

摘要/Abstract

摘要： 旨在建立阿司匹林丁香酚酯（aspirin eugenol ester，AEE）颗粒剂有关物质的测定方法。采用超高效液相色谱（ultra performance liquid chromatography，UPLC）法，色谱柱为Phenomenex luna C18（150 mm×4.6 mm，5 μm）；流动相为0.5%磷酸溶液-乙腈，梯度洗脱；流速为1.0 mL·min^-1；检测波长为279 nm；柱温为35℃；进样量为10 μL。结果显示：在选定的色谱条件下，AEE主峰与杂质峰分离良好；杂质A在0.25~60.0 μg·mL^-1浓度范围与峰面积线性关系良好，R²=0.999 2（n=8）；回收率为98.34%~100.15%（n=9，RSD=0.68%）；不同条件下耐用性良好，RSD值<3.33%。经方法学验证，该方法操作简单，专属性良好，适合于AEE颗粒剂有关物质测定。

关键词: 阿司匹林丁香酚酯, 超高效液相色谱, 有关物质, 方法学验证

Abstract: This study aims at establishing a method for the determination of related substances in aspirin eugenol ester(AEE) granules. Ultra performance liquid chromatography(UPLC) was used to detect the related substances of AEE granules, with the column was Phenomenex luna C18 (150 mm×4.6 mm, 5 μm), mobile phase was 0.5% phosphoric acid squeous solution and acetonitrile, flow rate was 1.0 mL·min^-1, wavelength was 279 nm, column temperature was 35℃, injection volume was 10 μL. Under the selected chromatographic conditions, the separation of the main peak of AEE and the impurity peak was well. Impurity A had a good linear relationship with the peak area in the concentration range of 0.25-60.0 μg·mL^-1, R²=0.999 2 (n=8). The material recoveries ranged from 98.34% to 100.15% (n=9, RSD=0.68%), and the robustness of the method under different conditions was well, the RSD value was less than 3.33%. The method is simple and specific, which suitable for the determination of related substances in AEE granules after methodological verification.

Key words: aspirin eugenol ester, UPLC, related substances, method validation

中图分类号:

S859.79

王志霞, 白莉霞, 秦哲, 刘希望, 杨亚军, 李世宏, 葛闻博, 李剑勇. 阿司匹林丁香酚酯颗粒剂有关物质检测方法的建立与验证[J]. 畜牧兽医学报, 2023, 54(8): 3500-3509.

WANG Zhixia, BAI Lixia, QIN Zhe, LIU Xiwang, YANG Yajun, LI Shihong, GE Wenbo, LI Jianyong. Establishment and Validation of the Determination Method for the Related Substances in Aspirin Eugenol Ester Granules[J]. Acta Veterinaria et Zootechnica Sinica, 2023, 54(8): 3500-3509.

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阿司匹林丁香酚酯颗粒剂有关物质检测方法的建立与验证

Establishment and Validation of the Determination Method for the Related Substances in Aspirin Eugenol Ester Granules

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