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 C_(18)柱(250 mm×4.6 mm,5μm);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:20μL;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5.925~59.251μg/mL(r=0.999 6)、6.210~62.100μg/mL(r=0.999 7)、5.110~8 516.000μg/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。
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,5µm)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 20μL,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 5.925-59.251μg/mL for succinic acid(r=0.9996),6.210-62.100μg/mL for adipic acid(r=0.9997),and 5.110-8516.000μg/mL for glutaric acid(r=0.9999).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.
作者
刘敏
廉贞霞
刘延新
王帆
李霞
杨海霞
LIU Min;LIAN Zhenxia;LIU Yanxin;WANG Fan;LI Xia;YANG Haixia(Shandong Academy of Pharmaceutical Sciences,Ji’nan 250101,China;Key Laboratory for Chemical Drug Research of Shandong Provincial,Ji’nan 250101,China)
出处
《中国药师》
CAS
2024年第3期382-387,共6页
China Pharmacist
基金
医药绿色智能制造与新药评价关键技术研究项目(2021ZDSYS07)。
关键词
戊二酸酐
丁二酸
己二酸
有关物质
高效液相色谱法
Glutaric anhydride
Succinic acid
Adipic acid
Related substances
High performance liquid chromatography
