[关键词]
[摘要]
目的 建立HPLC法,同时测定不同炒制程度下决明子中决明子苷、决明子苷B2、决明子苷C、红链霉素-龙胆二糖苷、决明素、黄决明素、橙黄决明素、美决明子素、大黄素、大黄酚、大黄素甲醚11种主要活性成分的含量,并探寻在不同炒制程度下决明子中11种成分的变化规律。方法 将决明子在140℃、160℃及180℃下分别炒制3 min、5 min、8 min、10 min、12 min及15 min,采用YMC-PackODS-A C18(250 mm×4.6 mm,5 μm)色谱柱,流动相A为乙腈,流动相B为0.1%甲酸水溶液,梯度洗脱,流速为0.5 mL?min-1,检测波长为284 nm,柱温30℃。结果 11种成分在相应的线性范围内线性关系良好,平均加样回收率(n = 6)均在99.09%-103.60%范围内,RSD < 3.0%。决明子炒制过程中决明子苷、决明子苷B2、决明子苷C及红链霉素-龙胆二糖苷4种苷类成分的含量整体呈下降趋势;决明素、黄决明素、橙黄决明素、美决明子素及大黄素5种苷元类成分的含量在决明子不同炒制程度下变化较小;大黄酚及大黄素甲醚2种苷元类成分的含量在决明子炒制过程中显著升高;11种成分的变化尤以180℃炒制时含量变化最为明显。结论 该方法准确、灵敏、高效可用于决明子中11种成分的含量测定;不同的炒制温度及炒制时间对决明子中11种成分的含量影响较大,在决明子炮制过程中,表面颜色及气味不能作为判断炒决明子炮制终点的依据,为保证炒决明子质量均一稳定,在决明子炮制过程中需建立量化的炮制参数。
[Key word]
[Abstract]
Objective To develop an HPLC method for simultaneous determination of 11 components (cassiaside, cassiaside B2, cassiaside C, rubrofusarin gentiobioside, obtusin, chrysoobtusin, aurantio-obtusin, obtusifolin, emodin, chrysophanol, physcione) and find out the content change rule of the eleven components in Semen Cassiae under different stir-frying degree. Methods Semen Cassiae were fry 3 min, 5 min, 8 min, 10 min, 12 min and 15 min at 140℃, 160℃ and 180℃ respectively. The analysis was performed on a YMC-Pack ODS-A C18 column (250 mm×4.6 mm, 5 μm) using gradient elution with the mobile phase consisting of 0.1% formic acid (A) and acetonitrile (B). The flow rate was 0.5 mL?min-1, and the detection wavelength was set at 284 nm and at 30℃. Results The 11 compounds were linear in the range of the test concentrations, and the average recovery of the method was between 99.09% and 103.60%, RSD < 3.0%. During the stirfrying process, the content of cassiaside, cassiaside B2, cassiaside C and rubrofusarin gentiobioside decreased significantly, the content of obtusin, chrysoobtusin, aurantio-obtusin, obtusifolin and emodin had little change, and the contents of chrysophanol and physcione were increased significantly. The changes of the 11 components were most obvious when they were fried at 180℃. Conclusion The HPLC method is accurate, precise, and efficient, which can be used to quantitatively determine the eleven components. Different stir-frying temperature and time had great influence on the content of eleven components in Semen Cassiae. In the process of Semen Cassiae, the surface color and flavor cannot be used as the basis to judge the end point of processing. In order to ensure uniform and stable quality of Semen Cassiae, quantitative processing parameters should be established in the processing of Semen Cassiae.
[中图分类号]
[基金项目]
国家自然科学基金委员会国家自然科学基金面上项目(81573603):种子类中药“逢子必炒”共性规律及特征性成分质量标准研究,负责人:蔡宝昌;江苏省科学技术厅江苏省重点研发计划-社会发展项目(BE2016626):中成药生产过程药渣废弃物绿色资源化利用关键技术研究,负责人:李伟东;江苏省人力资源和社会保障厅江苏省六大人才高峰项目(SWYY-108):优质中药饮片特征图谱研究与产业化应用示范项目,负责人:秦昆明。