聚焦微波辅助提取-酸性染料分光光度法测定农吉利中总生物碱  

Determination of Total Alkaloids in Crotalaria Sessiliflora L.by Acidic Dye Spectrophotometry Combined with Focused Microwave-Assisted Extraction

作　　者：樊轻亚[1] 游国叶[1] 

机构地区：[1]信阳职业技术学院药学院,信阳464000

出　　处：《理化检验（化学分册）》2015年第3期289-292,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：广东省社会发展领域科技计划项目(73060)

摘　　要：采用聚焦微波辅助提取(FMAE)结合溴麝香草酚蓝分光光度法测定农吉利中总生物碱。粒径为0.180 mm的样品,以甲醇为溶剂,料液比为1比25,在微波功率中火条件下提取50min。在pH 7.2的磷酸二氢钾-氢氧化钠缓冲溶液中,提取得到的生物碱与溴麝香草酚蓝酸性染料形成缔合物,用三氯甲烷萃取后,在最大吸收波长417nm处测量其吸光度。总生物碱的质量浓度在0.25~250mg·L-1范围内呈线性,方法的检出限(3S/N)为1.5mg·L-1。应用该方法测定农吉利药材中总生物碱,加标回收率为105%,测定值的相对标准偏差(n=6)小于3.0%。A method of acidic dye spectrophotometry coupled with focused microwave assisted extraction was applied to determine the total alkaloids in Crotalaria sessiliflora L.The sample with particle sizes of 0.180 mm was extracted by microwave at middle power level for 50 min with methanol as extract and the material-solvent ratio of1∶25.The extracted obtained alkaloids were reacted with bromothymol blue to form ion-pair complexes in the buffer solution of KH2PO4-NaOH with pH of 7.2.The complexes were then extracted with chloroform and absorbance was measured at 417 nm.The linearity range of the mass concentration of alkaloids was 0.25-250mg·L-1 with detection limit of 1.5mg·L-1.The method was used to measure total alkaloids in Crotalaria sessiliflora L.,giving recovery rates in the range of 106%,with RSD(n=6)less than 3.0%.

关 键 词：分光光度法 酸性染料 聚焦微波辅助提取 农吉利 生物碱 

分 类 号：O657.3[理学—分析化学] R284.1[理学—化学]