天舒胶囊中9种活性成分的HPLC-CAD法含量测定及稳定性研究

目的：采用高效液相色谱仪-电喷雾检测器（HPLC-CAD），建立同时测定天舒胶囊中天麻素、巴利森苷B、巴利森苷C、巴利森苷A、阿魏酸、阿魏酸松柏酯、洋川芎内酯A、6，7-二羟基藁本内酯及Z-藁本内酯含量的检测方法，并对天舒胶囊稳定性进行考察。方法：采用GL Sciences Inertsil ODS-3色谱柱，以90%乙腈（A），20 mmol·L^-1甲酸铵（甲酸pH 3.5）-乙腈（90：10）（B）为流动相，梯度洗脱，流速1.0 mL·min^-1，柱温40℃；CAD雾化器温度35℃，采集频率10 Hz，气压59.6 psi。同时测定天舒胶囊在加速及长期试验下各成分含量的变化，为该品种稳定性及贮藏条件提供依据。结果：各成分分离度均良好，阴性无干扰；9种成分的线性关系良好（r≥0.999 1）；平均加样回收率（n=6）为96.44%~98.91%，RSD≤2.0%。稳定性考察结果表明，阿魏酸松柏酯、洋川芎内酯A及Z-藁本内酯在加速条件下含量显著下降，提示该品种不宜在高温下长时间放置；长期条件下稳定性良好。结论：经方法学验证，该方法具有良好的灵敏度及准确度，可为天舒胶囊的全面质量控制提供科学依据，该品可于室温贮藏。

Determination and stability research of nine active ingredients in Tianshu Capsule by HPLC-CAD

OBJECTIVE To develop an HPLC-CAD method for simultaneous determination of nine active ingredients of gastrodin, Parishin B, Parishin C, Parishin A, ferulic acid, coniferyl ferulate, senkyunolide A, 6, 7-dihydroxyligustilide and Z-ligustilide in Tianshu capsule, and the stability of Tianshu Capsule was studied.METHODS The chromatographic separation was performed on a GL Sciences Inertsil ODS-3 column with 90% acetonitrile(A)-20 mmol·L^-1 ammonium acetate(formic acid tone pH 3.5):acetonitrile(90:10)(B) as the mobile phase, gradient elution was adopted at a flow rate of 1.0 mL·min^-1, the column temperature was set at 40℃; For CAD, the nebulization temperature of detector was 35℃, the acquisition frequency was 10 Hz, and gas pressure was 59.6 psi.At the same time, the content changes of components in Tianshu Capsule were determined under accelerated and long-term test, which provided the basis for the stability and storage conditions of Tianshu Capsule.RESULTS The separation of all components was good, with no interference in the negative; the linearity of the nine components was good(r ≥ 0.999 1); The average recoveries were 96.44%-98.91%, and the RSDs ≤ 2.0%.The results of stability investigation showed that the contents of coniferyl ferulate, senkyunolide A and Z-ligustilide decreased rapidly under accelerated condition, implied that the storage time of Tianshu Capsule under high temperature condition should not be too long; the stability under long-term condition was good.CONCLUSION The method is sensitive and accurate by method validation, which can be used for the overall assessment of the quality of Tianshu Capsule, this variety should be stored at room temperature.