title: Analysis of synephrine in da-cheng-qi decoction by HPLC employing precolumn derivatization with 9-fluorenylmethyl chloroformate.
abstract: A sensitive and reliable method has been developed to determine synephrine in a famous purgative Chinese medicinal prescription, da-cheng-qi decoction. After purified by solid-phase extraction (SPE), the decoction was derivatized with 9-fluorenylmethyl chloroformate in borate buffer and analyzed by reversed-phase high-performance liquid chromatography equipped with a diode-array detector. The chromatographic separation was carried out on a Shimadzu shim-pack VP-ODS column using acetonitrile-water as mobile phase. This method was validated in terms of linearity, recovery, precision, accuracy, and repeatability. Calibration curves were linear (r(2) > 0.99) over the concentration range of 0.78-100 microg/mL, and the mean recovery was 93.28%. The intra- and inter-batch precisions were less than 2% in terms of relative standard deviations. The accuracy and repeatability were well within the acceptable range. The limit of detection was 0.25 microg/mL. This validated method also can be used for assays of herbal products, fruits, dietary supplements, and biological samples containing synephrine.
authors.affiliation: Key Laboratory of Drug Quality Control and Pharmacovigilance (China Pharmaceutical University), Ministry of Education, Nanjing 210009, PR China.
authors.forename: Ying
authors.initials: Y
authors.lastname: Liu
authors.forename: Fengguo
authors.initials: F
authors.lastname: Xu
authors.forename: Zunjian
authors.initials: Z
authors.lastname: Zhang
authors.forename: Cheng
authors.initials: C
authors.lastname: Yang
authors.forename: Rui
authors.initials: R
authors.lastname: Song
authors.forename: Yuan
authors.initials: Y
authors.lastname: Tian
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D004365:Drugs, Chinese Herbal / Q000032:analysis*; D005449:Fluorenes / Q000737:chemistry*; D013578:Synephrine / Q000032:analysis*
chemical_list: D004365:Drugs, Chinese Herbal; D005449:Fluorenes; C054007:1-(9-fluorenyl)methyl chloroformate; D013578:Synephrine