Development and validation of a subcritical fluid extraction and high performance liquid chromatography assay for medroxyprogesterone in aquatic products.

Yuqian Han, Qinchuan Ma, Jie Lu, Yong Xue, Jie Xu, Changhu Xue

Department of Food Science and Engineering, Ocean University of China, P.O. Box 266003, Qingdao, China. hanyuqian@ouc.edu.cn

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences 2012 May 15

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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%. Copyright © 2012 Elsevier B.V. All rights reserved.

Citation

Yuqian Han, Qinchuan Ma, Jie Lu, Yong Xue, Jie Xu, Changhu Xue. Development and validation of a subcritical fluid extraction and high performance liquid chromatography assay for medroxyprogesterone in aquatic products. Journal of chromatography. B, Analytical technologies in the biomedical and life sciences. 2012 May 15;897:90-3