[關鍵詞]
[摘要]
目的 建立西青果Terminalia chebula Retz.訶黎勒酸和鞣花酸HPLC檢測方法及指紋圖譜鑒別方法,同時對15批次西青果藥材進行質量標準研究。方法 收集3個道地產(chǎn)地15批次西青果藥材,按《中國藥典》中方法對西青果藥材進行全檢;新建訶黎勒酸和鞣花酸HPLC檢測方法,流動相為甲醇-0.1%磷酸溶液,梯度洗脫,體積流量為1 mL·min-1,檢測波長為258 nm,柱溫為35℃,進樣量為5 μL,并進行方法學驗證;同時建立西青果HPLC指紋圖譜檢測方法,進行多批次藥材相似度分析,指認藥材特征峰并進行聚類分析。結果 15批次藥材檢查結果均符合《中國藥典》2020年版標準,薄層色譜法(TLC)結果顯示,供試品在西青果對照藥材色譜相應位置上顯相同顏色的斑點;3產(chǎn)地15批西青果樣品中水分、總灰分、酸不溶性灰分、水溶性浸出物(冷浸法)質量分數(shù)分別為6.74%~9.36%、2.41%~5.87%、0.05%~0.61%、51.03%~73.23%,平均值分別為7.66%、2.88%、0.22%、64.13%;新建立HPLC方法學考察均符合《中國藥典》相關要求,15批次西青果藥材中訶黎勒酸、鞣花酸質量分數(shù)為122.56~224.37、19.32~63.60 mg·g-1。15批西青果指紋圖譜相似度均大于0.90。結論 在西青果原有標準上增加灰分檢查,新建訶黎勒酸和鞣花酸含量測定及指紋圖譜方法,該方法專屬性強,簡便可靠,利用所建方法對不同產(chǎn)地批次的15批樣品進行測定并綜合評價,可為豐富該藥材質量控制內(nèi)容和藥典修訂提供依據(jù)。
[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.
[中圖分類號]
R282
[基金項目]
新疆地州科學自然基金資助項目(2022D01F49);兵團第二師鐵門關市重大科技計劃項目(2021SFGG02);兵團“強青”科技創(chuàng)新骨干人才計劃項目(2022CB029-01)