摘要
在强碱性条件下,1.5×10^(-4)mol·L^(-1)高锰酸钾溶液氧化2.0×10-5mol·L^(-1)鲁米诺溶液发生化学发光反应,芦丁对该反应具有增敏作用,通过检测其化学发光强度来对芦丁进行定量,据此建立了化学发光分析与高效液相色谱联用检测芦丁的方法。将芦丁片剂研磨成粉末,用甲醇溶解后,经回流加热、0.45μm滤膜抽滤、超声振荡,制得待测样品溶液。改装BPCL型微弱发光测量仪,连接高效液相色谱仪和化学发光检测系统,调节化学发光条件中流量为4 cm·s^(-1),检测盘管长度为10 cm。采用C18色谱柱为固定相,体积比6∶4的甲醇-2%(体积分数)冰乙酸溶液的混合液为流动相,芦丁能够很好地分离。结果显示:在1.00~150.00μg·L^(-1)内,芦丁的质量浓度与其化学发光强度呈线性关系,检出限为1.00×10^(-6)g·L^(-1),测定值的相对标准偏差(n=11)为2.7%。
Luminol solution of 2.0×10-5mol·L^(-1)was oxidized by potassium permanganate solution of 1.5×10^(-4)mol·L^(-1)in strong alkaline condition to make chemiluminescence reaction,which could be sensitized by rutin,and the quantification of rutin was carried out by detecting its chemiluminescence intensity.Based on this fact,a method for the determination of rutin by high performance liquid chromatography coupled with chemiluminescence detection was established.Rutin tablets were grinded into powder and dissolved with methanol.The sample solution was prepared by reflux heating,0.45μm filter membrane filtration and ultrasonic oscillation.BPCL weak luminescence measuring instrument was modified,and coupled with high performance liquid chromatography and chemiluminescence detection system.In the chemiluminescence condition,the flow rate was adjusted to 4 cm·s^(-1),and the length of the detected coil was 10 cm.Using C18 column as stationary phase and a mixture of methanol and 2%(φ)glacial acetic acid solution at volume ratio of 1∶1 as mobile phase,rutin could be separated well.The results showed that linear relationship between mass concentration of rutin and its chemiluminescence intensity was found in the range of 1.00-150.00μg·L^(-1),with detection limit of 1.00×10^(-6)g·L^(-1).RSDs(n=11)of the determined values was 2.7%.
作者
吴华
闵媛婷
刘立明
石小涛
郑轩
胡飞跃
夏志刚
雷克亮
胡双修
WU Hua;MIN Yuanting;LIU Liming;SHI Xiaotao;ZHENG Xuan;HU Feiyue;XIA Zhigang;LEI Keliang;HU Shuangxiu(The Second Clinical Hospital,Three Gorges University,Yichang 443000,China;College of Biology and Pharmacy,Three Gorges University,Yichang 443002,China;College of Hydraulic and Environmental Engineer,Three Gorges University,Yichang 443002,China;Ecological Environmental Bureau of Hubei Huanggang Macheng,Macheng 438300,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2021年第8期709-713,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
化学发光分析
高效液相色谱
芦丁
chemiluminescence detection
high performance liquid chromatography
rutin
