L. Fen
2010
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Journal
Physical Testing and Chemical Analysis
Abstract
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.