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
HPLC Determination of (E)-3-Ethyl-(2,3-Dihydro-1-Benzofuran-5-yl)-2-Propenoate and Its by-Products in the Process of Synthesis
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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.
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