非水液相微萃取-高效液相色谱法测定大黄中5种游离葸醌类化合物

目的利用非水液相微萃取-高效液相色谱法（HPLC）同时测定大黄中游离蒽醌类化合物的含量。方法利用自制的液相微萃取装置，以聚偏氟乙烯中空纤维为溶剂载体，正己醇为萃取溶剂，供相为甲醇，接受相为1mmol／L NaOH，搅拌速度为1500r／min，萃取时间为50min。萃取结束，接受相在434nm处进行HPLC分析。结果在优化的液相微萃取条件下，芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的线性范围、回收率、精密度和检测限分别为：0.015～13.2、0.075～11.2、0.085～12.8、0.096～14.4、0.117～17.6μg／ml；103.8％～106.1％；2.5％～5.2％和2.9.20.0ng／ml。结论本法选择性高，有机溶剂消耗少，能快速、准确地测定大黄药材中游离蒽醌类化合物。

Determination of five free anthraquinones in Rhubarb by nonaqueous Hquld-phase microextraction-high performance liquid chromatography

Objective To simultaneously determine the free anthraquinones in Rhubarb by nonaqueous liquidphase microextraction （NLPME） coupled with high performance liquid chromatography. Methods Using a self-made microextraction system, NLPME was carried out with polyvinylidene difluoride hollow fiber supporting the solvent, 1- hexanol as the organic solvent, methanol as the donor phase, 1 mmol/L NaOH as the acceptor phase, agitation at 1500 r/min for 50 min. After extraction, the acceptor phase was analyzed by HPLC at 434nm. Results Under optimal NLPME conditions, the linearity range, recovery rate, precision and detection limits for aloe-emodin, rhein, emodin, erysophanol and physcion were 0.0147～13.2, 0.0747～11.2, 0.0853-12.8, 0.096～14.4, 0.117～17,6 μg/ml; 103.8%- 106.1%; 2.5%～5.2% and 2.9～20.0 ng/ml, respectively. Conclusion With high selectivity and minimal use of organic solvent, nonaqueous liquid-phase microextraction could be applied to determine free anthraquinones in Rhubarb quickly and accurately.