[关键词]
[摘要]
目的 建立西青果Terminalia chebula Retz.诃黎勒酸和鞣花酸HPLC检测方法及指纹图谱鉴别方法,同时对15批次西青果药材进行质量标准研究。方法 收集3个道地产地15批次西青果药材,按《中国药典》中方法对西青果药材进行全检;新建诃黎勒酸和鞣花酸HPLC检测方法,流动相为甲醇-0.1%磷酸溶液,梯度洗脱,体积流量为1 mL·min-1,检测波长为258 nm,柱温为35℃,进样量为5 μL,并进行方法学验证;同时建立西青果HPLC指纹图谱检测方法,进行多批次药材相似度分析,指认药材特征峰并进行聚类分析。结果 15批次药材检查结果均符合《中国药典》2020年版标准,薄层色谱法(TLC)结果显示,供试品在西青果对照药材色谱相应位置上显相同颜色的斑点;3产地15批西青果样品中水分、总灰分、酸不溶性灰分、水溶性浸出物(冷浸法)质量分数分别为6.74%~9.36%、2.41%~5.87%、0.05%~0.61%、51.03%~73.23%,平均值分别为7.66%、2.88%、0.22%、64.13%;新建立HPLC方法学考察均符合《中国药典》相关要求,15批次西青果药材中诃黎勒酸、鞣花酸质量分数为122.56~224.37、19.32~63.60 mg·g-1。15批西青果指纹图谱相似度均大于0.90。结论 在西青果原有标准上增加灰分检查,新建诃黎勒酸和鞣花酸含量测定及指纹图谱方法,该方法专属性强,简便可靠,利用所建方法对不同产地批次的15批样品进行测定并综合评价,可为丰富该药材质量控制内容和药典修订提供依据。
[Key word]
[Abstract]
Objective To establish quality stangard of Terminalia chebula Retz. by building content measuring and fingerprint identification HPLC methods. Methods A total of 15 batches of T. chebula from three genuine origin were collected and tested according to Chinese Pharmacopoeia 2020. The mobile phase of HPLC for the determination of chebulagic acid and ellagic acid was established:methanol-0.01% phosphoric acid solution, the flow rate was 1 mL·min-1, the detection wavelength was set at 258 nm, the column temperature was 35 ℃, the sample size was 5 μL, and the methodology was verified. At the same time, HPLC fingerprint detection method of T. chebula was established to analyze the similarity of several batches of medicinal materials, identify the characteristic peaks of medicinal materials and perform cluster analysis. Results The test results of 15 batches of medicinal materials were all in line with the standards of Chinese Pharmacopoeia 2020 edition. TLC results showed that the tested materials showed the same color spots in corresponding positions of the control medicinal materials of T. chebula. The contents of water, total ash, acid insoluble ash and water soluble extract in 15 batches of T. chebula samples from three producing areas were 6.74% to 9.36%, 2.41% to 5.87%, 0.05% to 0.61% and 51.03% to 73.23%, respectively. The average values were 7.66%, 2.88%, 0.22% and 64.13%, respectively. The newly established HPLC methods were in line with the relevant requirements of Chinese Pharmacopoeia. The contents of chebulagic acid and ellagic acid in 15 batches of T. chebula were 122.56 to 224.37 mg·g-1 and 19.32 to 63.60 mg·g-1 respectively. The similarity of fingerprint of 15 batches of T. chebula was greater than 0.90. Conclusion On the basis of the original standard, ash examination, content determination and fingerprint were added in the experiment. The content detection method is more specific, simple and reliable. The established method was used to determine and comprehensively evaluate 15 batches of samples from different origin, which can provide a basis for enriching the quality control content of this herb and the revision of pharmacopoeia.
[中图分类号]
R282
[基金项目]
新疆地州科学自然基金资助项目(2022D01F49);兵团第二师铁门关市重大科技计划项目(2021SFGG02);兵团“强青”科技创新骨干人才计划项目(2022CB029-01)