| 摘要: |
| 目的 建立快速、准确的HPLC测定方法，同时测定仙人菇口服液中10种有效成分腺苷、虫草素、芦丁、芒柄花苷、朝藿定B、朝藿定C、淫羊藿苷、毛蕊异黄酮、灵芝酸A、宝藿苷Ⅰ的含量。方法 使用Dikma Diamonsil Plus C18柱（4.6 mm×250 mm，5μm），以乙腈（A）-0.1%冰醋酸水溶液（B）梯度洗脱（0~3 min，2%~5% A；4~7 min，5% A；8~17 min，5%~20% A；18~21 min，20%~30% A；22~38 min，30% A；39~48 min，30%~90% A）；流速为1.0 mL/min，柱温为30℃，检测波长为270 nm，进样量为10 μL。结果 腺苷在0.250~16.0 μg/mL、虫草素和淫羊藿苷在6.25~400 μg/mL、芦丁在1.25~80.0 μg/mL、芒柄花苷在0.500~32.0 μg/mL、朝藿定B在0.375~24.0 μg/mL、朝藿定C在3.12~200 μg/mL、毛蕊异黄酮和灵芝酸A在0.625~40.0 μg/mL、宝藿苷Ⅰ在0.125~8.00 μg/mL浓度范围内呈良好的线性关系（r均>0.999）；精密度、稳定性、重复性实验的RSD均<4%；加样回收率为96.32%~99.60%，符合在85%~115%范围内的标准要求。结论 本实验建立的HPLC测定方法操作简单、准确性高、重复性好，适用于仙人菇口服液中10种有效成分的含量测定，可以作为仙人菇口服液的质量控制方法。 |
| 关键词: 高效液相色谱法 仙人菇口服液 质量控制 含量测定 |
| DOI：10.16781/j.CN31-2187/R.20210829 |
| 投稿时间：2021-08-24修订日期：2023-04-25 |
| 基金项目:上海市科学技术委员会基金（21S21902700）. |
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| Simultaneous determination of 10 active ingredients in Xianrengu oral liquid by high-performance liquid chromatography |
| GAO Shouhong1△,PANG Tao1△,JIANG Daozhen2,WANG Zhipeng1,LU Wenquan1,YUE Xiaoqiang3,ZHAO Jing3* |
(1. Department of Pharmacy, The Second Affiliated Hospital of Naval Medical University (Second Military Medical University), Shanghai 200003, China;
2. Department of Thyroid Breast and Hernia Surgery, The Second Affiliated Hospital of Naval Medical University (Second Military Medical University), Shanghai 200003, China;
3. Department of Traditional Chinese Medicine, The Second Affiliated Hospital of Naval Medical University (Second Military Medical University), Shanghai 200003, China
△Co-first authors.
* Corresponding author) |
| Abstract: |
| Objective To develop a high-performance liquid chromatography (HPLC) method for the simultaneous determination of 10 active ingredients (adenosine, cordycepin, rutin, ononin, epimedin B, epimedin C, icariin, calycosin, ganoderic acid A, and baohuosideⅠ) in Xianrengu oral liquid. Methods A Dikma Diamonsil Plus C18 column (4.6 mm×250 mm, 5 μm) was used for gradient elution with acetonitrile (A) -0.1% glacial acetic acid (B) (0-3 min, 2%-5% A; 4-7 min, 5% A; 8-17 min, 5%-20% A; 18-21 min, 20%-30% A; 22-38 min, 30% A; 39-48 min, 30%-90% A). The flow rate was 1.0 mL/min, the column temperature was 30℃, the detection wavelength was 270 nm, and the injection volume was 10 μL. Results As for the analytes, the linear range of the calibration curve was 0.250-16.0 μg/mL for adenosine, 6.25-400 μg/mL for cordycepin and icariin, 1.25-80.0 μg/mL for rutin, 0.500-32.0 μg/mL for ononin, 0.375-24.0 μg/mL for epimedin B, 3.12-200 μg/mL for epimedin C, 0.625-40.0 μg/mL for calycosin and ganoderic acid A, 0.125-8.00 μg/mL for baohuosideⅠ, respectively (all r>0.999). The relative standard deviation (RSD) values of precision, stability and repeatability were all less than 4%. The recovery rate was 96.32%-99.60%, which met the standard requirements in the range of 85%-115%. Conclusion The established HPLC method has the features of simplicity, accuracy and high repeatability and is applicable for simultaneous determination of 10 active ingredients in Xianrengu oral liquid, making it a method for quality control of Xianrengu oral liquid. |
| Key words: high-performance liquid chromatography Xianrengu oral liquid quality control determination |
