分散液液微萃取快速测定中药中4种呋喃香豆素化合物

Rapid Determination of Four Kinds of Furocoumarin Compounds in Traditional Chinese Medicine by Dispersive Liquid-Liquid Microextraction

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50μL CCl4和300μL乙腈,分散均匀后,以3500 r/min离心3 min,吸取CCl4聚集相,用2倍于CCl4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1.0～3.0μg/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。

A method was developed for the determination of furocoumarin compounds（psoralen, oxypeuceda- nin, imperatorin, isoimperatorin） in traditional Chinese medicine samples by dispersive liquid-liquid microex-traction（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： 50μL carbon tetrachloride and 300μL acetonitrile were rapidly injected into 1.5 mL sample solution containing 2.5% （ω/V） NaCl. After centrifugation at 3500 r/min for 3 min, the sedimented CCl4 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 - 3.0μg/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.