title: Development and validation of a subcritical fluid extraction and high performance liquid chromatography assay for medroxyprogesterone in aquatic products.
abstract: A simple, rapid and sensitive method was developed for the determination of medroxyprogesterone in aquatic products by extraction with subcritical 1,1,1,2-tetrafluoroethane (R134a) and high performance liquid chromatography (HPLC). A response surface methodology (RSM) was adopted to optimise extraction pressure, temperature and co-solvent volume. The optimum extraction conditions predicted within the experimental ranges were as follows: pressure, 3 MPa; temperature, 25 °C; and co-solvent volume, 6 ml. The analysis was carried out on Zorbax SB-C₁₈ column (4.6 mm × 150 mm, 5 μm) with the mobile phase acetonitrile-water (55:45, v/v), flow rate 1.0 ml/min, temperature 30 °C and wavelength 240 nm. Good linearity of detection was obtained for medroxyprogesterone between concentrations of 50-250 ng/ml, r²=0.999. The method was validated using samples fortified with medroxyprogesterone at levels of 10, 30 and 50 ng/g, the mean recovery exceeds 90%, and the RSD values were less than 10%.
authors.affiliation: Department of Food Science and Engineering, Ocean University of China, P.O. Box 266003, Qingdao, China. hanyuqian@ouc.edu.cn
authors.forename: Yuqian
authors.initials: Y
authors.lastname: Han
authors.forename: Qinchuan
authors.initials: Q
authors.lastname: Ma
authors.forename: Jie
authors.initials: J
authors.lastname: Lu
authors.forename: Yong
authors.initials: Y
authors.lastname: Xue
authors.forename: Jie
authors.initials: J
authors.lastname: Xu
authors.forename: Changhu
authors.initials: C
authors.lastname: Xue
mesh_terms: D000704:Analysis of Variance; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods* / Q000592:standards; D025924:Chromatography, Supercritical Fluid / Q000379:methods* / Q000592:standards; D004350:Drug Residues / Q000032:analysis / Q000302:isolation & purification; D008525:Medroxyprogesterone / Q000032:analysis* / Q000302:isolation & purification; D012044:Regression Analysis; D015203:Reproducibility of Results; D017747:Seafood / Q000032:analysis*; D017210:Tilapia
chemical_list: D008525:Medroxyprogesterone