摘要
目的 建立手性高效液相色谱方法测定米拉贝隆中的对映异构体。方法 采用对照品法进行定性定量分析,使用Daicel Chiralpak AY-H(4.6 mm×250 mm,5 μm)色谱柱,流动相为正己烷-乙醇-二乙胺(650∶350∶1),流速为1.0 mL·min^(-1),检测波长为240 nm,柱温为35℃,进样体积为10 μL。结果 米拉贝隆与其对映异构体能有效分离,分离度大于1.5;米拉贝隆在0.461~5.975 μg·mL^(-1)与峰面积线性关系良好(r=0.9998);低、中、高质量浓度平均加样回收率分别为89.5%、94.8% 和92.8%,RSD分别为2.9%、2.9%和1.6%(n=3);供试品溶液在室温条件下24 h内基本稳定。经检测,6批米拉贝隆中均未检出对映异构体。结论 本方法经方法学验证,可用于米拉贝隆中对映异构体的测定。
Objective To develop an HPLC method to determine enantiomer in mirabegron.Methods Reference substance was used for the qualitative and quantitative determination.The separation was performed on a Daicel Chiralpak AY-H column (4.6 mm×250 mm,5 μm) with the mobile phase of hexane-ethanol-diethylamine (650∶350∶1) at 1.0 mL·min^(-1),the detective wavelength was 240 nm,the column temperature was 35℃and the injection volume was 10 μL.Results Mirabegron and enantiomer were effectively separated under the above conditions with the resolution higher than 1.5.The calibration curves were linear at 0.461~5.975 μg·mL^(-1)(r=0.9998).The recoveries were 89.5%,94.8%,and 92.8% at low,medium and high concentrations with the RSD of 2.9%,2.9% and 1.6%,respectively (n=3).The test solution was basically stable within 24 h at room temperature.No enantiomers were detected in the 6 batches of mirabegron.Conclusion The method is suitable for the determination of enantiomer in mirabegron by methodology validation.
作者
陈秋
樊梦妮
李国柱
兰公剑
CHEN Qiu;FAN Meng-ni;LI Guo-zhu;LAN Gong-jian(Nanjing Chia Tai Tianqing Pharmaceutical Co.,Ltd,Nanjing 210046)
出处
《中南药学》
CAS
2022年第11期2631-2634,共4页
Central South Pharmacy
关键词
米拉贝隆
对映异构体
手性药物检测
高效液相色谱法
mirabegron
enantiomer
chiral drug detection
high performance liquid chromatography
