中南民族大学学报(自然科学版)
中南民族大學學報(自然科學版)
중남민족대학학보(자연과학판)
JOURNAL OF SOUTH-CENTRAL UNIVERSITY FOR NATIONALITIES(NATURAL SCIENCE EDITION)
2014年
4期
43-46
,共4页
分光光度法%雄甾-4-烯-3,17-二酮%浓硫酸-乙酸酐%分支杆菌%植物甾醇
分光光度法%雄甾-4-烯-3,17-二酮%濃硫痠-乙痠酐%分支桿菌%植物甾醇
분광광도법%웅치-4-희-3,17-이동%농류산-을산항%분지간균%식물치순
spectrophotometry%4-androstene-3,17-dione%concentrated sulfuric acid%acetic anhydride%Mycobacterium neoaurum%phytosterol
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0.08~0.48 mg/mL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.
為建立一種雄甾-4-烯-3,17-二酮(4-AD)快速而簡便的測定方法,用乙痠乙酯-濃硫痠(15︰1, v/v)溶液溶解4-AD標準品,配成標準溶液,併稀釋為一定的濃度梯度後加乙痠酐反應15 min,測定吸光度,繪製標準麯線,進行穩定性試驗、加樣迴收率試驗和精密度試驗,併通過分光光度法檢測分支桿菌轉化植物甾醇所得轉化液中4-AD含量,與高效液相法進行瞭比較.結果錶明:4-AD在0.08~0.48 mg/mL的範圍內呈良好線性關繫,相關繫數R2=0.9993,精密度RSD為0.672%,樣品平均迴收率為99.69%,分光光度法和高效液相方法檢測結果差異不顯著(p>0.05).故此法操作簡單、快速,準確性高,重現性好.
위건립일충웅치-4-희-3,17-이동(4-AD)쾌속이간편적측정방법,용을산을지-농류산(15︰1, v/v)용액용해4-AD표준품,배성표준용액,병희석위일정적농도제도후가을산항반응15 min,측정흡광도,회제표준곡선,진행은정성시험、가양회수솔시험화정밀도시험,병통과분광광도법검측분지간균전화식물치순소득전화액중4-AD함량,여고효액상법진행료비교.결과표명:4-AD재0.08~0.48 mg/mL적범위내정량호선성관계,상관계수R2=0.9993,정밀도RSD위0.672%,양품평균회수솔위99.69%,분광광도법화고효액상방법검측결과차이불현저(p>0.05).고차법조작간단、쾌속,준학성고,중현성호.
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>0.05).So this is an effective, simple, and rapid method with high accuracy and repeatability for the analysis of 4-AD.