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-C_(18)色谱柱(250 mm×4.6 mm,5μm),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35μg·L^(-1)。方法已用于(E)-EDHBFP的质量控制。
A method for the determination of（E）-3-ethyl-（2,3-dihydro-l-benzofuran-5-yl）-2-propenoate [abbreviated as（E）-EDHBFP]and its by-products during synthesis by HPLC was proposed.The Diamonsil-C_（18） column（250 mm×4.6 mm,5μm） 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-l-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 35μg·L^-1.The proposed method was used for the quality control of synthesis of（E）-EDHBFP.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2010年第4期401-403,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
