超临界流体色谱法测定吲达帕胺及其对映异构体含量
Determination of Indapamide and Its Enantiomer by Supercritical Fluid Chromatography
林丽琴 1汪霞 1杨直 1高丽琼 1彭彦 1石云峰2
作者信息
- 1. 浙江省杭州市食品药品检验科学研究院,浙江 杭州 310022
- 2. 浙江省食品药品检验研究院,浙江 杭州 310052
- 折叠
摘要
目的 建立有效分离吲达帕胺对映异构体并测定其含量的超临界流体色谱法.方法 色谱柱为Daicel IB N-5 柱(250 mm×4.6 mm,5 μm),流动相为二氧化碳-0.1%二乙醇胺甲醇溶液(70∶30,V/V),背压为 150 bar,流速为 3.0 mL/min,检测波长为 243 nm,柱温为 40℃,进样量为 5 μL.结果 吲达帕胺及其对映异构体分离度良好,5 min内均已出峰完全.两者质量浓度均在 2.48～37.10 μg/mL范围内与峰面积线性关系良好(r=0.999 9,n=6);检测限均为 0.012 μg/mL,定量限均为 0.05 μg/mL;精密度、稳定性试验结果的RSD均小于 1.0%;耐用性良好;平均回收率分别为 100.75%和 100.90%,RSD分别为 1.00%和 0.72%(n=9).结论 建立的超临界流体色谱法结果准确、耐用性较好,能有效测定吲达帕胺片中吲达帕胺及其对映异构体的含量.
Abstract
Objective To establish a supercritical fluid chromatography(SFC)method for effectively separating the enantiomer of indapamide and determining its content.Methods The chromatographic column was the Daicel IB N-5 column(250 mm×4.6 mm,5 μm),the mobile phase was carbon dioxide-0.1%diethanolamine methanol solution(70∶30,V/V),the back pressure was 150 bar,the flow rate was 3.0 mL/min,the detection wavelength was 243 nm,the column temperature was 40℃,and the injection volume was 5 μL.Results Indapamide and its enantiomer were separated successfully in 5 min with a good resolution.The linear ranges of the two components were 2.48-37.10 μg/mL(r=0.999 9,n=6).The limits of detection for both were 0.012 μg/mL,and the limits of quantification for both were 0.05 μg/mL.The RSDs of precision and stability tests were lower than 1.0%.The durability was good.The average recovery rates of indapamide and its enantiomer were 100.75%and 100.90%,with RSDsof 1.00%and 0.72%respectively(n=9).Conclusion The established SFC method is accurate and durable,which can effectively determine the contents of indapamide and its enantiomer in Indapamide Tablets.
关键词
吲达帕胺/超临界流体色谱法/手性拆分/对映异构体/含量测定Key words
indapamide/supercritical fluid chromatography/chiral separation/enantiomer/content determination引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据