Zhang Lan, Chen Jinfeng, He Yu, Chi Yuwu, Chen Guonan
Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fuzhou University, Fuzhou, Fujian, China.
Talanta. 2009 Jan 15;77(3):1002-8. doi: 10.1016/j.talanta.2008.07.060. Epub 2008 Aug 8.
A simple, rapid and low-costing new mixed surfactant MEKC method has been developed for the analysis of five neutral anabolic steroids in this paper. It was found that the bile salt coupling with Triton X-100 was a suitable bi-micellar surfactant for the separation of these anabolic steroids with similar structure. The separation conditions were optimized in detail. The five natural and synthetic anabolic steroids, such as androstenedione (AD), 19-norandrostenedione (NAD), 1,4-androstadiene-3,17-dione (ADD), methandrostenolone (MA) and methyltestosterone (MT) were separated and detected in an alkaline buffer system (pH 9.0) containing 15 mM Britton-Robinson (BR) buffer, 50mM sodium cholate (SC) and 0.1% (v/v) Triton X-100 with detection wavelength at 241 nm and 18 kV of separation voltage. Under the optimal conditions, five coexistence neutral steroids were completely separated within 12 min with the detection limits ranged from 0.20 to 0.51 microg/mL. This method was successfully used for detection and confirmation of the anabolic steroid methandrostenolone in methandrostenolone tablets and in the real human urine, GC-MS method was applied to confirm the free methandrostenolone existence in the urine sample in order to validate the reliability of MEKC method.
本文开发了一种简单、快速且低成本的新型混合表面活性剂胶束电动色谱法，用于分析五种中性合成代谢类固醇。研究发现，胆盐与 Triton X - 100 结合是一种适用于分离这些结构相似的合成代谢类固醇的双胶束表面活性剂。详细优化了分离条件。在含有 15 mM Britton - Robinson（BR）缓冲液、50 mM 胆酸钠（SC）和 0.1%（v/v）Triton X - 100 的碱性缓冲体系（pH 9.0）中，在检测波长为 241 nm 和分离电压为 18 kV 的条件下，分离并检测了五种天然和合成的合成代谢类固醇，如雄烯二酮（AD）、19 - 去甲雄烯二酮（NAD）、1,4 - 雄二烯 - 3,17 - 二酮（ADD）、美雄酮（MA）和甲基睾酮（MT）。在最佳条件下，五种共存的中性类固醇在 12 分钟内完全分离，检测限范围为 0.20 至 0.51 μg/mL。该方法成功用于检测和确证美雄酮片剂及实际人尿中的合成代谢类固醇美雄酮，应用气相色谱 - 质谱法确证尿样中游离美雄酮的存在，以验证胶束电动色谱法的可靠性。
