目的采用高效液相色谱法对醋柳黄酮片中黄酮类化合物进行分析。对其中的山柰酚和异鼠李素进行直接定量;结合化学计量学方法对槲皮素与杂质的重叠峰进行分辨和定量。方法采用C18柱,流动相为甲醇-0.4%磷酸溶液(51:49),柱温30℃,检测波长368nm,测定山柰酚和异鼠李素的含量。在相同色谱条件下采用MCR-ALS方法对醋柳黄酮片中有效成分槲皮素的重叠色谱峰进行分辨和定量。结果槲皮素在1.92~19.2mg·L^-1(r=0.9993),山柰酚、异鼠李素在0.40~4.03mg·L^-1(r=0.9994),4.74~47.40mg·L^-1(r=0.9994)内线性关系良好,精密度分别为2.2%,2.38%,1.8%(n=6)。槲皮素、山柰酚、异鼠李素平均回收率为96.1%,101.8%,98.0%。结论HPLC-DAD检测结合MCR-ALS可以快速准确的测定醋柳黄酮片中有效成的含量。
OBJECTIVE To establish a HPLC method for the determination of kaempferoe and isorhamnetine in flavone hippophaes tablets. METHODS Chemmometric tools were used for the resolution of overlapping peaks of quercetin and impurity. The sepauation was performed on a diamonsil C18 column. The mobile phase consisted of methanol -0. 4% phosphoric acid, and column temperature was at 30 ℃, with DAD detection at 368 nm. Under the same chromatogram condition, multivariate curve resolution with alternating least square was used to analyze the overlapping peaks from quercetin and impurity. RESULTS The kaempferoe and isorhamnetine were linear in the ranges of 0. 403 - 4.03 mg·L^-1 ( r = 0. 999 4 ) and 4.74 - 47.4 mg·L^-1 ( r = 0. 999 4 ), respectively. CONCLUSION HPLC -DAD couple with MCR-ALS was a simple, rapid and accurate method to determine the content of flavone hippophaes tables.