鳗鲡中甲基睾酮的二维液相色谱检测方法研究

Study on determination of methyltestosterone in eel by two-dimensional liquid chromatography

针对鳗鲡样品中油脂含量较多,采用常规液相色谱分析时易产生干扰的状况,建立了鳗鲡样品甲基睾酮的在线二维液相色谱检测方法。样品用乙醚提取、硅胶固相萃取柱净化后,用二维液相色谱进行检测。选择C_8柱和C_(18)柱分别作为一维和二维色谱柱,构建二维分离体系。通过中心切割技术将一维色谱柱上的目标馏分转移到二维色谱柱上进行进一步的分离。实验结果表明,构建的二维液相色谱系统稳定性良好,建立的二维液相色谱方法可以实现甲基睾酮和基质干扰物的充分分离,检测结果准确可靠,适合鳗鲡样品中甲基睾酮的测定。本研究解决了用常规液相色谱法检测高油脂含量的鳗鲡样品中甲基睾酮残留时经常出现的干扰问题,是对现有水产品中甲基睾酮残留的液相色谱检测方法的有益补充。

Eel products have high fat content. Since the conventional liquid chromatography would easily lead to interference in the analysis,it is necessary to establish on- line two- dimensional liquid chromatography inspection method for determination of methyltestosterone in eel products. Samples were extracted with ether and purified by silica gel solid phase extraction column,and then determined by two- dimensional liquid chromatography. C_8 and C18columns were selected as the first and second dimensional chromatographic columns to construct the two- dimensional separation system. The target fraction of the first- dimensional column was transferred to the second- dimensional column for further separation through heart- cutting technique. The results showed that the two- dimensional liquid chromatographic system had good stability,and the established method can realize the full separation of methyltestosterone and matrix interference. The method was accurate and reliable,and suitable for the determination of methyltestosterone in eel products. This study solved the interference problem which often appears in the determination of methyltestosterone residues in eel products with high fat by conventional liquid chromatography,and was a useful supplement to existing liquid chromatography method for determination of methyltestosterone residues in aquatic products.