HPLC Determination of (E)-3-Ethyl-(2,3-Dihydro-1-Benzofuran-5-yl)-2-Propenoate and Its by-Products in the Process of Synthesis
摘 要
提出了一种测定(E)-3-乙基-(2,3-二氢苯并呋喃-5-基)-2-丙烯酸乙酯[(E)-EDHBFP]及其合成中的副产物含量的高效液相色谱分析方法.色谱条件:固定相为Diamonsil-C18色谱柱(250 mm×4.6 mm,5 μm),流动相为甲醇-水(72+28),流量0.8 mL·min-1,检测波长为319 nm.结果表明:在方法所建立的最佳条件下,目的产物即(E)-EDHBFP可达到与其异构体副产物,合成的反应物以及一种结构不明的副产物的完全分离,并同时定量测定.(E)-EDHBFP的质量浓度在10~80 mg·L-1范围与峰面积呈线性,检出限(3S/N)为35 μg·L-1.方法已用于(E)-EDHBFP的质量控制.
Abstract
A method for the determination of (E)-3-ethyl-(2,3-dihydro-1-benzofuran-5-yl)-2-propenoate [abbreviated as (E)-EDHBFP] and its by-products during synthesis by HPLC was proposed.The Diamonsil-C18 column (250 mm×4.6 mm,5 μm) was used as the stationary phase,and a mixture of methanol and water (72+28 by vol.) was used as the mobile phase,with its flow-rate at 0.8 mL·min-1.UV detection at the wavelength of 319 nm was adopted in the determination.It was found that under the optimum condition of the proposed method,the objective product (E)-EDHBFP was well separated from the reactant of synthesis (i.e.,2,3-dihydro-1-benzofuran-5-carbaldehyde),and the isomeric by-product (Z)-3-ethyl-(2,3-dihydro-1-benzofuran-5-yl)-2-propenoate as well as an unknown by-product as shown in the chromatogram.Linear relationship between values of peak area and concentration of (E)-EDHBFP was obtained in the range of 10-80 mg·L-1 with the value of detection limit (3S/N) of 35 μg·L-1.The proposed method was used for the quality control of synthesis of (E)-EDHBFP.
中图分类号 O652.63
所属栏目 工作简报
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收稿日期 2009/9/3
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备注刘芬(1984-),女,湖南人,硕士研究生,主要研究方向为药物分析.
引用该论文: LIU Fen,LI liang,FENG Li-hua. HPLC Determination of (E)-3-Ethyl-(2,3-Dihydro-1-Benzofuran-5-yl)-2-Propenoate and Its by-Products in the Process of Synthesis[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(4): 401~403
刘芬,李良,冯丽华. 高效液相色谱法测定(E)-3-乙基-(2,3-二氢苯并呋喃-5-基)-2-丙烯酸乙酯及其相关物质的含量[J]. 理化检验-化学分册, 2010, 46(4): 401~403
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参考文献
【1】SIMPSON D,CURRAN M P.Ramelteon : a review of its use in insomnia[J].Drugs,2008,68(13):1901-1919.
【2】PANDI-PERUMAL S R,SRINIVASAN V,SPENCE D W,et al.Ramelteon: a review of its therapeutic potential in sleep disorders[J].Adv Ther,2009,26(6):613-626.
【3】黄玉凤,唐丽娜.新型催眠药瑞美替昂及其临床研究[J].世界临床药物,2006,27(9):556-559.
【4】UCHIKAWA O,FUKASTSU K,TOKUNOH R,et al.Synthesis of a novel series of tricyclic indan derivatives as melatonon receptor agonists[J].J Med Chem,2002,45(19):4222-4239.
【5】徐克勋.精细有机化工原料及中间体手册[M].北京:化学工业出版社,2002:4.
【2】PANDI-PERUMAL S R,SRINIVASAN V,SPENCE D W,et al.Ramelteon: a review of its therapeutic potential in sleep disorders[J].Adv Ther,2009,26(6):613-626.
【3】黄玉凤,唐丽娜.新型催眠药瑞美替昂及其临床研究[J].世界临床药物,2006,27(9):556-559.
【4】UCHIKAWA O,FUKASTSU K,TOKUNOH R,et al.Synthesis of a novel series of tricyclic indan derivatives as melatonon receptor agonists[J].J Med Chem,2002,45(19):4222-4239.
【5】徐克勋.精细有机化工原料及中间体手册[M].北京:化学工业出版社,2002:4.
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