中国药师2024,Vol.27Issue(3) :382-387.DOI:10.12173/j.issn.1008-049X.202401122

HPLC法测定戊二酸酐中的有关物质

Determination of related substances in gluaric anhydride by HPLC

刘敏 廉贞霞 刘延新 王帆 李霞 杨海霞
中国药师2024,Vol.27Issue(3) :382-387.DOI:10.12173/j.issn.1008-049X.202401122

HPLC法测定戊二酸酐中的有关物质

Determination of related substances in gluaric anhydride by HPLC

刘敏 1廉贞霞 1刘延新 1王帆 1李霞 1杨海霞1
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作者信息

  • 1. 山东省药学科学院(济南 250101);山东省化学药物重点实验室(济南 250101)
  • 折叠

摘要

目的 建立HPLC法测定戊二酸酐中有关物质的方法.方法 采用HPLC法,色谱柱:Waters Symmetry C18 柱(250 mm×4.6 mm,5 µm);流动相:甲醇-0.1%磷酸溶液(3 ∶ 97);流速:0.9 mL/min;柱温:30℃;进样体积:20 µL;检测波长:210 nm.结果 戊二酸酐中丁二酸、己二酸及未知杂质均能有效检出,丁二酸、己二酸、戊二酸的线性范围分别为 5.925~59.251 μg/mL(r=0.999 6)、6.210~62.100 μg/mL(r=0.999 7)、5.110~8 516.000 μg/mL(r=0.999 9);丁二酸和己二酸的平均回收率分别为 100.92%(RSD=0.86%)和 105.89%(RSD=2.99%)(n=9).结论 该方法专属性强、灵敏度高、准确度好,可用于测定戊二酸酐的有关物质.

Abstract

Objective To establish a method for the determination of related substances in glutaric anhydride by HPLC.Methods The HPLC method was performed on a Waters Symmetry C18 column(250 mm×4.6 mm,5 µm)with mobile phase of methanol-0.1%phosphoric acid solution(3 ∶ 97)at a flow rate of 0.9 mL/min,the column temperature was 30℃,the injection volume was 20 μL,and the detection wavelength was set at 210 nm.Results Succinic acid,adipic acid and unknown impurities in glutaric anhydride can be effectively detected.The linear range was 5.925-59.251 μg/mL for succinic acid(r=0.999 6),6.210-62.100 μg/mL for adipic acid(r=0.999 7),and 5.110-8 516.000 μg/mL for glutaric acid(r=0.999 9).The average recoveries of succinic acid and adipic acid were 100.92%(RSD=0.86%)and 105.89%(RSD=2.99%)(n=9),respectively.Conclusion The method has strong specificity,high sensitivity and good accuracy,and can be used for the related substances determination of glutaric anhydride.

关键词

戊二酸酐/丁二酸/己二酸/有关物质/高效液相色谱法

Key words

Glutaric anhydride/Succinic acid/Adipic acid/Related substances/High performance liquid chromatography

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基金项目

医药绿色智能制造与新药评价关键技术研究项目(2021ZDSYS07)

出版年

2024
中国药师
国家药品监督管理局高级研修学院,武汉医药(集团)股份有限公司

中国药师

CSTPCD
影响因子:0.944
ISSN:1008-049X
参考文献量13
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