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睾丸酮是人体内主要的雄性激素,正确地测定其含量,对于某些疾病的诊断、治疗及研究具有重要的意义。人体内睾丸酮的含量较低,多采用放射免疫分析法及竞争性蛋白结合分析法进行测定,因此需制备[1,2-~3H]睾丸酮。采用催化加成法,以1,2脱氢睾丸酮(以下均写成Δ~1睾丸酮)为前体,5%Pd-C为催化剂,二氧六环为溶剂,在氚气压为95800 Pa左右条件下进行催化加成反应,氚化时间为1.5小时,其反应式见图1。氚化产物首先采用硅胶纸薄层层析法,继而采用高压液体色谱法进行纯化,所得产品比活度达1887 GBq/mmol(51 Ci/mmol),放化纯度99%以上,已用于放免分析,用户满意,产品稳定,一年后,放化纯度仍达95.0%。
Testosterone is the major androgen in the human body, and its content is correctly measured, which is of great significance for the diagnosis, treatment and research of certain diseases. Human testosterone content is low, more use of radioimmunoassay and competitive protein binding assay for determination, it is necessary to prepare [1,2 ~ 3H] testosterone. Adopting catalytic addition method, 1,2-dehydrogenation testosterone (hereinafter described as Δ1 testosterone) as a precursor, 5% Pd-C as a catalyst, dioxane as a solvent, at a tritium pressure of about 95800 Pa Catalytic addition reaction, tritiated time of 1.5 hours, the reaction shown in Figure 1. Tritiated products were first purified by silica gel thin-layer chromatography followed by high-pressure liquid chromatography. The specific activity was 1887 GBq / mmol (51 Ci / mmol) and the radiochemical purity was over 99% Analysis, customer satisfaction, product stability, one year later, the radiochemical purity still reached 95.0%.