复方川脊片中3种活性成分的含量测定

摘要

目的 建立同时测定复方川脊片中原儿茶酸、原儿茶醛和芍药苷3种有效成分含量的高效液相色谱方法.方法 采用Thermo ODS-2 HYPERSIL C18色谱柱(250 mm× 4.6 mm,5 μm),流动相为10 mmol.结论 L-1 磷酸二氢钾-0.02%磷酸溶液(A)-甲醇(B),线性梯度洗脱(0～12 min,15% B;12～32 min,25% B),流速1.0 mL.结论 min-1;柱温38 ℃;检测波长分别为210 nm(原儿茶酸)、280 nm(原儿茶醛)、232 nm(芍药苷).结果 原儿茶酸、原儿茶醛和芍药苷的质量浓度分别在5.27～105.50,1.60～31.92,86.04～1 721.00 μg.结论 mL-1范围内呈良好线性关系(r≥0.999 9);日内、日间精密度良好,RSD均＜1.93%(n＝6);各组分低、中、高浓度的平均加样回收率均在98.39%～99.94%之间,RSD均＜1.78%(n＝6);复方川脊片中原儿茶酸、原儿茶醛和芍药苷的质量浓度分别为(120.70±1.94),(24.28±0.57 ),(3 439.00±60.18) μg.结论 g-1.结论 该方法简便可靠,重复性好,可全面反映复方川脊片中各味药的质量,适用于复方川脊片质量控制.%Objective To develop a HPLC method for the simultaneous determination of protocatechuic acid, protocate-chuic aldehyde and paeoniflorin in compound chuanji tablets. Methods A Thermo ODS-2 HYPERSIL C18 column ( 250 mmx 4. 6 mm,5 μm ) was used. The mobile phase consisted of 10 mmol · L-1 KH2PO4 ,0. 02% H3PO4 in water ( A ) and methanol ( B ) with linear gradient elution ( 0-12 min,15% B; 12-32 min,25% B ),The flow rate was 1. 0 mL · Min-1. DAD detection was used and detection wavelength was set at 210 nm for protocatechuic acid,280 nm for protocatechuic aldehyde and 232 nm for paeoniflorin,respectively. The temperature of column was 38 °C. Results Protocatechuic acid,protocatechuic aldehyde and paeoniflorin showed good linearity ( r≥ 0.999 9 ) in the range of 5. 27-105. 50,1. 60-31. 92 and 86.04-1 721.00 μg · mL-1 , respectively. The RSDs of intra-day and inter-day precision were no more than 1. 93% ( n = 6 ). The average recovery rate of three tested compounds at low,medium and high concentration levels were in the range of 98. 39% -99. 94% for all with RSDs less than 1.78% (n = 6). The contents of protocatechuic acid, protocatechuic aldehyde and paeoniflorin in compound chuanji tablets were ( 120.70±l. 94 ),( 24. 28±0. 57 ),( 3 439.00±60. 18 ) μg · G-1 .respectively. Conclusion The developed method is simple,accurate,reliable and can be used to control the quality of compound chuanji tablets.