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

진창화 (중앙대학교 약학대학)
임수희 (중앙대학교 약학대학)
이기진 (중앙대학교 약학대학)
심형섭 (중앙대학교 약학대학)
조의환 (삼진제약주식회사)
염정록 (중앙대학교 약학대학)
Publication Information
YAKHAK HOEJI / v.46, no.6, 2002 , pp. 392-397 More about this Journal
Abstract
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 7$0^{\circ}C$ and completed within 30 min. The optimal wavelength of the fluorescence detector are λ$_{ex}$=300 nm and λ$_{em}$ = 460 nm. The LOD of the ursodeoxycholic acid was 25 ng/mι based on the S/N =3, and the LOQ was 80 ng/mι based on S/N = 10. Crude drug pharmaceuticals pretreated by solid phase extraction (Sep-pak $C_{18}$ cartridge) which were shown very good separation and recovery values for the compound.d.
Keywords
Ursodeoxycholic acid; 2-bromoacetyl-6-methoxynaphthalene; HPLC; solid phase extraction; pre-column derivatization; crude drug formulations;
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