HPLC高效液相色谱测定抗癌1号中异嗪皮啶的含量

Determination of isofraxidin content in anticancer NO. 1 by HPLC

目的 采用高效液相色谱（HPLC）测定抗癌1号中异嗪皮啶的含量,并与肿节风药材提取液进行对比分析.方法 采用Acclaim 120 C18 5um 120°A（4.6×250 mm） 柱,以乙腈为流动相A,以0.1%磷酸溶液为流动相B,乙腈-0.1%磷酸（20：80）梯度洗脱,检测波长为344 nm 波长,流速为1.5 mL/min,测定肿节风药材提取液中异嗪皮啶的含量.结果 肿节风样品用流动相定容与甲醇定容,抗癌1号（混合药材）用流动相定容与甲醇定容,测定异嗪皮啶含量分别为 （1.84±0.02）、（2.09±0.01）、（5.56±0.01）、（5.56±0.01）（mg/g）,除混合药材流动相定容与甲醇定容比较无差异外,其余比较,P〈0.01,差异均有统计学意义;加样回收试验平均为87.5%,进样20μl测定浓度在（0.004~0.064）mg/mL按峰高值计有良好线性关系,相关系数为R=0.9951.结论 该法测定准确,线性关系好,可用于抗癌1号的质量控制,单一提取液用甲醇定容所得异嗪皮啶含量高于流动相定容.

Objective Determination of isofraxidin content in anticancer NO.1 by HPLC,to comparative analysis with the herbs extract of sarcandrae liquid.Methods The contents of isofraxidin in anticancer NO.1 were assayed by HPLC.The column used of Acclaim120 C18 5um 120°A（4.6x250mm） column.The mobile phase was acetonitrile-0.1% phosphoric acid（20：80） at a flow rate of 1.5ml﹒min-1,the detection wavelength was set at 344nm.Results Sarcandrae sample with the mobile phase constant volume and constant volume of methanol,anticancer NO.1（mixed herbs） mobile phase capacity with methanol to volume,determination of different triazine leather pyridine contents were 1.84±0.02、2.09±0.01、5.56±0.01、5.56±0.01（mg/g）.In addition to mixed herbs capacity with constant volume of methanol mobile phase was no significant difference compared to the rest,P〈0.01,different were statistically significant,The average recovery of isofraxidin was 87.5%.And the linear range was 0.004-0.064 mg/mL（r=0.9951） on the injection 20ul.Conclusion The method was accurate,and the great linear relationship can be used for quality control of the anticancer NO.1 single extract was washed with to volume proceeds isofraxidin content highter than the mobile phase constant volume.