雄甾-4-烯-3,17-二酮的浓硫酸乙酸酐分光光度测定

为建立一种雄甾-4-烯-3,17-二酮(4-AD)快速而简便的测定方法,用乙酸乙酯-浓硫酸(15︰1,v/v)溶液溶解4-AD标准品,配成标准溶液,并稀释为一定的浓度梯度后加乙酸酐反应15 min,测定吸光度,绘制标准曲线,进行稳定性试验、加样回收率试验和精密度试验,并通过分光光度法检测分支杆菌转化植物甾醇所得转化液中4-AD含量,与高效液相法进行了比较.结果表明:4-AD在0.08⁰.48 mg/m L的范围内呈良好线性关系,相关系数R2=0.9993,精密度RSD为0.672%,样品平均回收率为99.69%,分光光度法和高效液相方法检测结果差异不显著(p>0.05).故此法操作简单、快速,准确性高,重现性好.

The Determination of 4-Androstene-3,17-Dione by Spectrophotometry Using Concentrated Sulfuric Acid and Acetic Anhydride as Solvent

To develop a quick and convenient analysis method for 4-androstene-3,17-dione （ 4-AD）, standard was dissolved in concentrated sulfuric acid and acetic anhydride （volume ratio=15︰1）and diluted to different concentrations. Acetic anhydride was added to react 15 min, and the absorbency was measured.The stability, average recovery rate and precision of the experiment were evaluated based on the standard curve. The content of 4-AD in the broth by biotranformating phytosterols using Mycobacterium neoaurum were analyzed by our spectroscopic method and high pressure liquid chromatography （ HPLC） , respectively.The results indicated that when the concentration of 4-AD were in the range of 0.08~0.48 mg/mL, the linear correlation was excellent （R2 =0.9993）, and the average recovery rate and precision were 99.69% and 0.672% （ RSD）, respectively.There was no significant difference between the results of the spectroscopic and HPLC methods（p＆gt;0.05）.So this is an effective, simple, and rapid method with high accuracy and repeatability for the analysis of 4-AD.