大蝎子草质量标准及指纹图谱研究

Quality standard and fingerprint for Girardinia diversifolia

目的建立大蝎子草的质量标准及指纹图谱。方法TLC法定性鉴别大蝎子草中的东莨菪内酯,根据2020年版《中国药典》及《国家药品标准工作手册》相关方法测定其水分、总灰分、酸不溶性灰分、浸出物。采用HPLC法建立指纹图谱,该药物的分析采用Agilent C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相0.1%甲酸-乙腈,梯度洗脱;体积流量1.2 mL/min;柱温30℃;检测波长290 nm。采用主成分分析、聚类分析对指纹图谱进行评价,HPLC法测定对羟基肉桂酸、东莨菪内酯、紫云英苷含量。结果TLC显示清晰斑点,分离度好。大蝎子草的水分、总灰分、酸不溶性灰分、浸出物含量分别为9.39%~14.63%、15.13%~19.00%、0.87%~4.80%、15.59%~23.85%。共筛选出9个共有色谱峰,13批样品相似度均在0.900以上,主成分分析和聚类分析结果一致。对羟基肉桂酸、东莨菪内酯、紫云英苷的平均含量分别为0.0605、0.0216、0.1243 mg/g。结论含量测定方法稳定、准确性好;指纹图谱方法分离度良好,稳定可靠,可为完善大蝎子草的质量控制方法提供参考。建议大蝎子草水分不得过13.0%,总灰分不得过21.0%,酸不溶性灰分不得过5.0%,水溶性浸出物(热浸法)含量不得少于14.0%,紫云英苷含量不得少于0.010%。

AIM To establish the quality standard and fingerprint for Girardinia diversifolia(Link)Friis(Himalayan giant nettle).METHODS The Himalayan giant nettle had its scopolamine lactone qualitatively identified by TLC;its moisture,total ash,acid insoluble ash,and extract determined complying with method of Chinese Pharmacopoeia(the 2020 edition)and the National Pharmaceutical Standards Work Manual;and its fingerprint established by HPLC,using a 30℃thermostatic Agilent C_(18)column(250 mm×4.6 mm,5μm),with mobile phase comprising of 0.1%formic acid-acetonitrile flowing at 1.2 mL/min in a gradient elution manner,and 290 nm detection wavelength.The fingerprint was evaluated by principal component analysis and cluster analysis,and the contents of p-hydroxycinnamic acid,scopoletin and astragaloside were determined by HPLC.RESULTS Result of TLC showed clear and well-separated spots.G.diversifolia was quantitatively determined to have 9.39%-14.63%water,15.13%-19.00%total ash,0.87%-4.80%acid insoluble ash and 15.59%-23.85%extract.In terms of the nine totally selected common chromatographic peaks,thirteen batches of samples contributed more than 0.900 similarity,in consistence with the result of principal component analysis and cluster analysis.The average contents of p-hydroxycinnamic acid,scopoletin and astragaloside were determined to be 0.0605 mg/g,0.0216 mg/g and 0.1243 mg/g,respectively.CONCLUSION Use of the content determination method and the fingerprint method of good stability and reliability highlights the quality control of G.diversifolia.We suggest a standard of no more than 13.0%water,21.0%total ash,5.0%acid insoluble ash;and no less than 14.0%water-soluble extract(hot leaching method)and 0.010%astragaloside in the content of G.diversifolia.