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对小剂量己烯雌酚(Diethylstibestrol,下简称DES)进行含量测定需要特殊灵敏和精密的分析方法。通常可利用 DES 结构中酚羟基之反应活性发展不同测定方法如:乙酰化、亚硝化、亚硝化后极谱法、溴化法和紫外法,此外也可利用酚基与一些生色试剂如磷钼钨酸盐、铁、锑和钒盐反应后进行比色测定。这些方法专一性和灵敏度差。虽然紫外辐射法对 DES 测定专一性好,但手续冗长,费时,特别对 DES 二丙酸酯油剂的测定,手续更繁锁。鉴于三苯氯化四唑(Triphenyl tet-razolium chloride)(Ⅰ)能被不同二羟基苯衍生物还原成相应的有色甲(月替)(Formazan)衍生物,作者研究了DES 和它的二丙酸酯与三苯氯化四唑反应形成有色甲(月替),再用比色法测定。实验方法四唑溶液:取三苯氯化四唑用无醛醇稀释成0.5％溶液;标准液:准确秤取经80°真空干燥2小
Determination of small doses of diethylstibestrol (DES) requires a very sensitive and precise analytical method. The reactivity of phenolic hydroxyl groups in DES structures can often be exploited to develop different assays such as acetylation, nitrosation, post-nitrosation polarography, bromination and UV methods. It is also possible to utilize phenolic groups with some chromogenic reagents such as phosphorus Molybdenum tungstate, iron, antimony and vanadium salt reaction after the colorimetric determination. The specificity and sensitivity of these methods is poor. Although the ultraviolet radiation method for DES specificity, but the procedures lengthy, time-consuming, in particular, the determination of DES dipropionate oil, the procedure more complicated lock. Since Triphenyl tet-razolium chloride (I) can be reduced to the corresponding Formazan derivative by different dihydroxybenzene derivatives, the authors studied the effects of DES and its dipropylene The reaction of the ester with tetrakistriphenylchloride to form a colored armor (monthly), followed by colorimetric determination. Experimental method Tetrazole solution: Take tetraphenyl trichloride with no alcohol diluted to 0.5% solution; standard solution: accurately weighed 80 ° vacuum drying 2 small