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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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手性NACE法测定酒石酸美托洛尔片剂中对映体的含量

Determination of enantiomers of metoprolol tartrate in tablets by chiral NACE

作者(英文):
分类号:R917
出版年·卷·期(页码):2019,39 (1):127-132
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立手性非水毛细管电泳法(NACE法)测定酒石酸美托洛尔片剂中对映体的含量。方法:D-葡萄糖酸-硼酸络合酸为手性选择剂,在优化过的NACE手性分离条件下展开相关研究。优化的NACE手性分离条件:未涂层熔融石英毛细管( 55.0 cm×50 μm,有效长度为45.0 cm);背景缓冲液为含8 mmol·L-1 D-葡萄糖酸、120 mmol·L-1硼酸、43.2 mmol·L-1三乙胺的甲醇溶液;10 cm,5 s重力进样;运行电压20 kV;检测波长224 nm;柱温为室温。结果:酒石酸美托洛尔的2个对映体质量浓度在7.5~250.0 μg·mL-1范围内,与峰面积呈现良好的线性关系;对映体1的定量下限和检测下限分别为7.5 μg·mL-1和2.5 μg·mL-1;对映体2的定量下限和检测下限分别为25.0 μg·mL-1和7.5 μg·mL-1;对映体1和对映体2的加样回收率分别为99.7%、98.0%、97.2%和97.7%、98.0%、98.0%,均在95.0%~105.0%范围内。6个批次的酒石酸美托洛尔片剂中对映体1和对映体2的标示量百分含量均在96.6%~102.5%之间。结论:该方法经验证可用于酒石酸美托洛尔片剂中对映体含量的测定。  

-----英文摘要:---------------------------------------------------------------------------------------

Objective:To establish a method for the determination of enantiomers of metoprolol tartrate in tablets by nonaqueous capillary electrophoresis (NACE).Methods:D-Gluconic acid-boric acid complex was used as the chiral selector.The experiments were carried out under the optimized chiral NACE conditions.The optimized conditions were as follows:Enantiomeric sepraration was performed in an unmodified fused silica capillary of 50.0 μm with 55.0 cm of total length and 45.0 cm of effective length;the running buffer solution was a mixture of 8 mmol·L-1 D-gluconic acid,120 mmol·L-1 boric acid and 43.2 mmol·L-1 triethylamine in methanol;injection were performed hydrostatically for 5 s at a 10 cm height difference;the applied voltage was 20 kV;the detection wavelength was 224 nm;the experiments were performed at room temperature.Results:Good linearity for the two enantiomers of metoprolol tartrate were obtained in the range of 7.5-250.0 μg·mL-1.The limit of quantification (LOQ)and the limit of detection (LOD)for enantiomer 1 were 7.5 μg·mL-1 and 2.5 μg·mL-1,respectively,and for enantiomer 2,25.0 μg·mL-1 and 7.5 μg·mL-1,respectively. The recoveries for each enantiomer were 99.7%,98.0%,97.2% and 97.7%,98.0%,98.0%,respectively,with all in the range of 95.0%-105.0%.The contents of enantiomer 1 and enantiomer 2 in six batches of metoprolol tartrate tablets were all in the ranges of 96.6%-102.5%.Conclusion:The method validated by methodology is suitable for the determination of enantiomer contents in metoprolol tartrate tablets. 

-----参考文献:---------------------------------------------------------------------------------------

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