CAJ | 학술논문

建立分散液相微萃取(DLLME)与HPLC结合快速测定中药样品中呋喃香豆素类化学成分含量的方法.对影响萃取效率的因素进行了优化:在含2.5%(w/V) NaCl的1.5 mL样品溶液中加入50 μL CCl_4和300 μL乙腈,分散均匀后,以3500 r/min离心3 min,吸取CCl_4聚集相,用2倍于CCl_4体积的甲醇溶解后进行HPLC分析.补骨脂素、氧化前胡素在0.006～6.00 mg/L范围内,欧前胡素、异欧前胡素在0.006～12.0 mg/L范围内线性关系良好;检出限为1.0～3.0 μg/L(S/N=3);相对标准偏差在2.3%～5.4%(n=5);浓缩倍数为12.6～38.5倍;回收率97.5%～114.8%.将本方法应用于快速测定白芷及其制剂元胡止痛片中欧前胡素、异欧前胡素及微量成分补骨脂素、氧化前胡素的含量,结果令人满意.
건립분산액상미췌취(DLLME)여HPLC결합쾌속측정중약양품중부남향두소류화학성분함량적방법.대영향췌취효솔적인소진행료우화:재함2.5%(w/V) NaCl적1.5 mL양품용액중가입50 μL CCl_4화300 μL을정,분산균균후,이3500 r/min리심3 min,흡취CCl_4취집상,용2배우CCl_4체적적갑순용해후진행HPLC분석.보골지소、양화전호소재0.006～6.00 mg/L범위내,구전호소、이구전호소재0.006～12.0 mg/L범위내선성관계량호;검출한위1.0～3.0 μg/L(S/N=3);상대표준편차재2.3%～5.4%(n=5);농축배수위12.6～38.5배;회수솔97.5%～114.8%.장본방법응용우쾌속측정백지급기제제원호지통편중구전호소、이구전호소급미량성분보골지소、양화전호소적함량,결과령인만의.
A method was developed for the determination of furocoumarin compounds(psoralen, oxypeucedanin, imperatorin, isoimperatorin) in traditional Chinese medicine samples by dispersive liquid-liquid microextraction(DLLME) coupled with high performance liquid chromatography and the relation of sample solution volume, sediment phase volume with enrichment factors was deducted. Some important parameters that influenced the extraction efficiency were optimized: 50 μL carbon tetrachloride and 300 μL acetonitrile were rapidly injected into 1.5 mL sample solution containing 2.5%(w/V) NaCl. After centrifugation at 3500 r/min for 3 min, the sedimented CCl_4 phase was pumped and recorded the volume, then dissolved with methanol and injected into the HPLC for analysis. Under the optimum conditions, a good linear relationship was obtained in the range of 0.006 6.00 mg/L of both psoralen and oxypeucedanin and 0.006-12.0 mg/L of both imperatorin and isoimperatorin. The limits of detection were 1.0-3.0 μg/L(S/N=3). The relative standard deviations were 2.3%-5.4%(n=5). The enrichment factors ranged from 12.6 to 38.5 folds. The average recoveries ranged from 97.5% to 114.8%. The four kinds of furocoumarin compounds in Radix Angelicae dahuricae and Yuanhu Zhitong tablet were determined by the proposed method with satisfactory results.