Department of Food Science and Engineering, Ocean University of China, P.O. Box 266003, Qingdao, China.
Food Chem. 2012 Dec 15;135(4):2988-93. doi: 10.1016/j.foodchem.2012.07.081. Epub 2012 Jul 25.
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%.
建立了一种利用亚临界 1,1,1,2-四氟乙烷（R134a）萃取和高效液相色谱法（HPLC）测定水产品中 17α-甲基睾丸酮的简单、快速、灵敏的方法。采用响应面法优化了萃取压力、温度和共溶剂体积。在实验范围内预测的最佳萃取条件如下：压力 5 MPa，温度 31°C，共溶剂体积 3.35ml。分析在 XDB-C（18）柱（4.6mm×250mm，5μm）上进行，流动相为乙腈-水（55:45，v/v），流速 0.8ml/min，温度 30°C，波长 245nm。17α-甲基睾丸酮在 50-250ng/ml 浓度范围内检测线性良好，r（2）=0.999。该方法采用 10、30 和 50ng/g 水平添加 17α-甲基睾丸酮的样品进行验证，平均回收率超过 90%，RSD 值小于 10%。
