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Development and validation of a subcritical fluid extraction and high performance liquid chromatography assay for medroxyprogesterone in aquatic products
- Han, Yuqian, Ma, Qinchuan, Lu, Jie, Xue, Yong, Xu, Jie, Xue, Changhu
- Journal of chromatography 2012 v.897 pp. 90-93
- high performance liquid chromatography, medroxyprogesterone, response surface methodology, temperature, wavelengths
- 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, 3MPa; temperature, 25°C; and co-solvent volume, 6ml. The analysis was carried out on Zorbax SB-C₁₈ column (4.6mm×150mm, 5μm) with the mobile phase acetonitrile–water (55:45, v/v), flow rate 1.0ml/min, temperature 30°C and wavelength 240nm. Good linearity of detection was obtained for medroxyprogesterone between concentrations of 50–250ng/ml, r²=0.999. The method was validated using samples fortified with medroxyprogesterone at levels of 10, 30 and 50ng/g, the mean recovery exceeds 90%, and the RSD values were less than 10%.