溶剂诱导相变萃取-UPC^2快速测定中成药及原料药中的香豆素

Rapid Determination of Coumarin in Chinese Traditional Patent Medicine and Raw Materials by UPC^2 and Solvent Induced Extraction

使用溶剂诱导相变萃取对中成药及原料药进行预处理,建立了中成药中香豆素的超高效合相色谱(UPC2)检测方法。样品经粉碎(60目)、乙腈-水(7∶3,体积比)提取,二氯甲烷诱导分相后,使用UPC2对样品中的香豆素进行检测。以3倍信噪比(S/N)确定香豆素的检出限为0.1 mg/L;线性范围为0.3~10.0mg/L;加标回收率为89.8%~102.3%;相对标准偏差为0.31%~1.0%。同时与UPLC进行比较,结果表明该方法的选择性高,检测成本低,且分析时间仅为UPLC的1/4。该研究为高通量检测香豆素提供了一种全新的前处理及检测方法。

A method of solvent induced phase extraction and ultra performance convergence chroma- tography （ UPC2 ） was established for the determination of coumarin in Chinese traditional patent medi- cine and raw materials. Samples were crushed（60 mesh）, and extracted with acetonitrile -water（7 ： 3,by volume） using dichloromethane as induced separation solvent. The targeted compound was de- tected by UPC2 method. The limit of detection （LOD, S/N = 3 ） for coumarin was 0. 1 mg/L. The linear range of coumarin was in the range of 0. 3 - 10.0 mg/L. The spiked recoveries ranged from 89.8% to 102. 3% and the relative standard deviations were between 0. 31% and 1.0% . Compared with UPLC method, the method showed the advantages of high selectivity and low detection cost, and its analysis time is only 1/4 of the UPLC. This study provided a new pretreatment and detection method for the high throughput detection of the coumarin.