title: Optimisation for subcritical fluid extraction of 17-methyltestosterone with 1,1,1,2-tetrafluoroethane for HPLC analysis.
abstract: A simple, rapid and sensitive method was developed for determination of 17α-methyltestosterone in aquatic products by extraction with subcritical 1,1,1,2-tetrafluoroethane (R134a) extraction and high performance liquid chromatography (HPLC). 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 5 MPa, temperature 31°C, and co-solvent volume 3.35ml. The analysis was carried out on XDB-C(18) column (4.6 mm × 250 mm, 5 μm) with the mobile phase acetonitrile-water (55:45, v/v), flow rate 0.8 ml/min, temperature 30°C and wavelength 245 nm. Good linearity of detection was obtained for 17α-methyltestosterone between concentrations of 50-250 ng/ml, r(2)=0.999. The method was validated using samples fortified with 17α-methyltestosterone 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: Changhu
authors.initials: C
authors.lastname: Xue
mesh_terms: D000728:Androgens / Q000032:analysis* / Q000302:isolation & purification; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D025924:Chromatography, Supercritical Fluid / Q000295:instrumentation / Q000379:methods*; D004350:Drug Residues / Q000032:analysis / Q000302:isolation & purification*; D005399:Fishes; D006845:Hydrocarbons, Fluorinated / Q000737:chemistry; D008460:Meat / Q000032:analysis*; D008777:Methyltestosterone / Q000032:analysis / Q000302:isolation & purification*; D004980:Ethane / Q000031:analogs & derivatives; D005466:Fluorocarbons
chemical_list: D000728:Androgens; D006845:Hydrocarbons, Fluorinated; D008777:Methyltestosterone; C063006:norflurane; D004980:Ethane; D005466:Fluorocarbons