2-Bromoacetyl-6-metroxynaphthalene을 형광유도체화제로 HPLC와 SPE를 이용한 생약제제 중 Ursodeoxycholic acid의 정량

Determination of Ursodeoxycholic Acid in Crude Drug Formulations by HPLC and SPE Using Selective Pre-column Derivatization with 2-Bromoacetyl-6-methoxynaphthalene

A simple and sensitive high performance liquid chromatographic method to quantitate ursodeoxycholic acid in crude drug pharmaceuticals was investigated. Ursodeoxycholic acid react with 2-bromoacetyl-6-methoxynaphthalene (Br-AMN) in the presence of triethylamine to form highly fluorescent derivative. The derivatization procedure was performed at 70oC and completed within 30 min. The optima1 wavelength of the fluorescence detector are λex=300 nm and λex= 460 nm. The LOD of the ursodeoxycholic acid was 25 ng/ml based on the S/N=3, and the LOQ was 80 ng/ml based on S/N=10. Crude drug pharmaceuticals pretreated by solid phase extraction (Sep-pak C18 cartridge) which were shown very geod separation and recwery values for the compound.