一测多评法同时测定小承气汤颗粒中9种成分的含量

Simultaneous Determination of the Contents of 9 Components in Xiao Chengqitang Granules by Quantitative Analysis of Multi-components by Single-marker

关键词:  一测多评法  小承气汤颗粒  含量测定  相对校正因子

Key words:  quantitative analysis of multi-components by single marker  Xiao Chengqitang granules  content determination  relative correction factor

摘要:

目的 建立一测多评(quantitative analysis of multi-components by single-marker，QAMS)法同时测定小承气汤颗粒中柚皮苷、新橙皮苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚、和厚朴酚、厚朴酚的含量。方法 采用HPLC，Waters Xbridge C₁₈色谱柱(250 mm×4.6 mm，5 μm)，柱温为30 ℃，检测波长为280 nm(柚皮苷、新橙皮苷)、254 nm(芦荟大黄素、大黄酸、大黄素、和厚朴酚、厚朴酚、大黄酚、大黄素甲醚)；以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱；流速为1.0 mL·min^-1；进样量为10 μL。以新橙皮苷为内参物，计算该成分与其他8种成分的相对校正因子，并计算各成分含量。将QAMS计算结果与外标法实测结果进行对比，验证所建立方法的可行性。结果 9种成分在各自规定的浓度范围内线性关系良好(r>0.999)，平均加样回收率为87.06%~98.08%，RSD为1.21%~2.83%，QAMS法与外标法测定结果无显著差异。结论 建立的方法准确可靠，QAMS法可用于小承气汤颗粒中9种成分含量的同时测定及质量控制。

Abstract:

OBJECTIVE To establish a quantitative analysis of multi-components by single-marker(QAMS) method for the simultaneous determination of naringin, neohesperidin, aloe-emodin, rhein, emodin, chrysophanol, emodin methyl ether, honokiol, magnolol in Xiao Chengqitang granules. METHODS HPLC was used with Waters Xbridge C₁₈ column (250 mm×4.6 mm, 5 μm). The column temperature was 30 ℃. The detection wavelength was 280 nm(naringin, neohesperidin), and 254 nm(aloe-emodin, rhein, emodin, chrysophanol, emodin methyl ether, honokiol, magnolol). The mobile phase was acetonitrile-0.1% phosphoric acid solution for gradient elution. The flow rate was 1.0 mL·min^-1. The sample volume was 10 μL. Taking neohesperidin as the internal reference, the relative correction factor of this component and the other 8 components was calculated, and the content of each component was calculated. The QAMS calculation results were compared with the measured results of the external standard method to verify the feasibility of the established method. RESULTS The 9 components had a good linear relationship within their specified concentration ranges(r>0.999), the average recovery rate was 87.06%-98.08%, and the RSD was 1.21%-2.83%. There was no significant difference between the calculated values by QAMS and the measured values by the external standard method. CONCLUSION The established method is accurate and reliable. The QAMS method can be used for the simultaneous determination and quality control of the content of 9 components in Xiao Chengqitang granules.