达乌里芯芭质量综合评价方法研究

Study on Comprehensive Quality Evaluation Method for Cymbaria daurica L.

目的:建立达乌里芯芭质量综合评价体系。方法:按照2020版中国药典杂质检查项下要求,实施了重金属、砷盐、灰分、水分及浸出物等检查项目。利用TLC法对达乌里芯芭中益母草苷、梓醇和8-表番木鳖酸进行色谱鉴别。采用HPLC法对不同来源达乌里芯芭进行定量分析,其条件为色谱柱:Agilent ZORBAX Eclipse Plus C18色谱柱(250 mm×4.6 mm, 5μm);流动相:乙腈(A)-水(B);梯度洗脱,A:0~13 min, 15%~25%;13~20 min, 25%~45%。结果:益母草苷和梓醇的展开剂为三氯甲烷-甲醇-甲酸(14∶6∶1),8-表番木鳖的展开剂为三氯甲烷-甲醇-甲酸(14∶7∶1)时,益母草苷、梓醇和8-表番木鳖的斑点清晰、Rf值合理和分离度好。12批达乌里芯芭中重金属、砷盐、水分均符合中国药典标准。达乌里芯芭的灰分、酸不溶灰分、水溶性浸出物和醇溶性浸出物的量变化分别在8.36%~13.10%、1.16%~9.01%、24.50%~41.18%、19.56%~35.25%。达乌里芯芭中被检测成分梓醇、桃叶珊瑚阿苷和益母草苷在较宽的浓度范围内表现出良好的线性关系,梓醇、桃叶珊瑚阿苷和益母草苷在不同批次芯芭中相对含量变化分别为(10.32±0.13)~(11.81±0.16)、(4.03±0.05)~(4.91±0.07)、(2.54±0.03)~(2.93±0.05)mg/g。结论:建立准确、可靠、稳定的达乌里芯芭质量综合评价体系,为该药材的质量控制提供了有力依据。

Objective To establish a comprehensive evaluation system for the quality of Cymbaria daurica. Methods According to the requirements of impurity inspection in the current Chinese Pharmacopoeia(2020 Edition), the limit test for heavy metals and as salt, the determination of moisture, ash and extractives have been carried out. The ajugol, catalpol and 8-epiloganic acid were identified by TLC. HPLC was used to determine the content of Cymbaria daurica from different sources. The HPLC conditions were as follows: Agilent ZORBAX Eclipse Plus C18column(250 mm×4.6 mm, 5μm) with acetonitrile-water as mobile phase, gradient elution, A:0-13 min, 15%-25%;13-20 min, 25%-45%. Results The chloroform-methanol-formic acid(14∶6∶1) was used as developing agent for ajugol and catalpol, and chloroform-methanol-formic acid(14∶7∶1) for 8-epiloganic acid, the spots were clear and reproducible, and Rf values met the requirements. The heavy metals, arsenic salts and moisture in 12 batches of Cymbaria daurica meet the standards of Chinese Pharmacopoeia. The content changes of water, ash, acid insoluble ash, water-soluble extract and alcohol soluble extract in 12 batches of Cymbaria daurica were 8.36%-13.10%, 1.16%-9.01%,24.50%-41.18%,19.56%-35.25%, respectively. The tested components ajugol, catalpol and 8-epiloganic acid in Cymbaria daurica showed a good linear relationship in a wide concentration range. The relative contents of ajugol, catalpol and 8-epiloganic acid in different batches of Cymbaria daurica were(0.353±0.004)-(1.002±0.012),(0.164±0.002)-(0.744±0.010),(0.153±0.002)-(0.262±0.004) and(1.092±0.012)-(2.433±0.033) mg/g, respectively. Conclusion An accurate, reliable and stable comprehensive quality evaluation system for Cymbaria daurica was established, which provided a strong basis for the quality control of the medicinal material.