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•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•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•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•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。

Simultaneous Determination of Protocatechuic Acid,Protocatechuic Aldehyde and Paeoniflorin in Compound Chuanji Tablets

Objective To develop a HPLC method for the simultaneous determination of protocatechuic acid,protocatechuic aldehyde and paeoniflorin in compound chuanji tablets.Methods A Thermo ODS-2 HYPERSIL C18 column(250 mm×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 ℃.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±1.94),(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.