一测多评法同时测定清火抗毒丸中6种成分

Simultaneous determination of six components in Qinghuo Kangdu Pill by QAMS

目的建立一测多评法同时测定清火抗毒丸中绿原酸、咖啡酸、木犀草苷、3,5-O-二咖啡酰基奎宁酸、迷迭香酸、蒙花苷的含量。方法采用Thermo ODS C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈-体积分数为0.3%磷酸溶液,梯度洗脱;流速:1.0 mL·min^(-1);柱温:30℃;检测波长:320 nm。以绿原酸为内参物,计算其他5种成分的相对校正因子,测定其含量。结果绿原酸、咖啡酸、木犀草苷、3,5-O-二咖啡酰基奎宁酸、迷迭香酸、蒙花苷分别在质量浓度为3.188-102.0 mg·L^(-1)、0.3531-11.30 mg·L^(-1)、12.50-400.0 mg·L^(-1)、2.313-74.00 mg·L^(-1)、1.313-42.00 mg·L^(-1)、1.188-38.00 mg·L^(-1)内线性关系良好(r≥0.9996),平均加样回收率(RSD)分别为100.1%(0.57%)、95.9%(2.0%)、99.5%(0.33%)、98.7%(0.9%)、99.7%(0.46%)、100.5%(1.1%)。各成分相对校正因子重现性良好,采取一测多评法测得的含量与外标法实测值无显著性差异。结论该方法不但稳定而且可靠,可用于清火抗毒丸的质量评价。

Objective To establish a quantitative analysis of multi-components by single-marker(QAMS) method for the simultaneous content determination of chlorogenic acid, caffeic acid, luteoloside, 3,5-O-dicaffeoylquinic acid, rosmarinic acid and buddleoside in Qinghuo Kangdu Pills.Methods The analysis of methanol extract of the drug was performed on a 30 ℃ thermostatic Thermo ODS C_(18) column(250 mm×4.6 mm, 5 μm),with the mobile phase composition of acetonitrile-0.3% phosphoric acid at the flow rate of 1.0 mL·min^(-1) in a gradient elution manner, and the detection wavelength was set at 320 nm.With chlorogenic acid as an internal standard, the relative correction factors of the other five constituents were calculated, and the content determination was carried out.Results Chlorogenic acid, caffeic acid, luteoloside, 3,5-O-dicaffeoylquinic acid, rosmarinic acid and buddleoside showed good linear relationships within the ranges of 3.188-102.0 mg·L^(-1),0.353 1-11.30 mg·L^(-1),12.50-400.0 mg·L^(-1),2.313-74.00 mg·L^(-1),1.313-42.00 mg·L^(-1),1.188-38.00 mg·L^(-1)(r≥0.999 6),whose average recoveries(RSD) were 100.1%(0.57%),95.9%(2.0%),99.5%(0.33%),98.7%(0.9%),99.7%(0.46%) and 100.5%(1.1%),respectively.The reproducibilities of relative correction factors were good.The results obtained by QAMS and external standard method were similar.Conclusion This stable and reliable method can be used for the quality control of Qinghuo Kangdu Pills.