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

作　　者：林丽琴 汪霞 杨直 高丽琼 彭彦 石云峰 LIN Liqin;WANG Xia;YANG Zhi;GAO Liqiong;PENG Yan;SHI Yunfeng(Hangzhou Institute for Food and Drug Control,Hangzhou,Zhejiang,China 310022;Zhejiang Institute for Food and Drug Control,Hangzhou,Zhejiang,China 310052)

机构地区：[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

出　　处：《中国药业》2024年第12期75-78,共4页China Pharmaceuticals

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,5µm),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5µL。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2.48~37.10µg/mL范围内与峰面积线性关系良好(r=0.9999,n=6);检测限均为0.012µg/mL,定量限均为0.05µg/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。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,5µm),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 5µL.Results Indapamide and its enantiomer were separated successfully in 5 min with a good resolution.The linear ranges of the two components were 2.48-37.10µg/mL(r=0.9999,n=6).The limits of detection for both were 0.012µg/mL,and the limits of quantification for both were 0.05µg/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 RSDs of 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 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]