十大功勞葉藥材的質量標準提高研究
發(fā)布時間:2019-08-30 來源: 歷史回眸 點擊:
中圖分類號 R927 文獻標志碼 A 文章編號 1001-0408(2018)04-0470-04
DOI 10.6039/j.issn.1001-0408.2018.04.10
摘 要 目的:提高十大功勞葉藥材的質量標準。方法:采用薄層色譜法(TLC)對藥材樣品進行定性鑒別。測定藥材樣品水分、灰分、醇浸出物。采用高效液相色譜法測定藥材樣品中鹽酸小檗堿的含量,色譜柱為WondaSil C18,流動相為乙腈-0.05 mol/L磷酸二氫鉀溶液(25 ∶ 75,V/V),流速為1.0 mL/min,檢測波長為264 nm,柱溫為30 ℃,進樣量為10 μL。結果:藥材樣品TLC圖斑點清晰,分離度好。藥材樣品水分為3.92%~7.03%,總灰分為3.65%~6.95%,酸不溶性灰分為0.05%~1.03%,醇浸出物為10.87%~33.14%。鹽酸小檗堿檢測進樣量線性范圍為0.183~0.915 μg(r=0.999 9);定量限、檢測限分別為0.143、0.095 μg;精密度、穩(wěn)定性、重復性試驗的RSD<2.0%(n=6);加樣回收率為95.21%~103.10%(RSD=2.95%,n=6)。結論:藥材水分、總灰分、酸不溶性灰分分別不得過8.0%、6.0%、0.4%,醇浸出物、鹽酸小檗堿含量分別不得低于16.0%、1.0%。所建標準可用于十大功勞葉藥材的質量控制。
關鍵詞 十大功勞葉;質量標準;高效液相色譜法;薄層色譜法
ABSTRACT OBJECTIVE: To improve the quality standard of Folium Mahoniae. METHODS: TLC was used for qualitative identification. The contents of moisture, ash and ethanol extract were determined. The content of berberine hydrochloride was determined by HPLC. The determination was performed on WondaSil C18 column with mobile phase consisted of acetonitrile-0.05 mol/L monopotassium phosphate solution (25 ∶ 75,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was 264 nm, column temperature was 30 ℃, and sample size was 10 μL. RESULTS: TLC spots were clear and well-separated. The contents of moisture, total ash, acid-insoluble ash and ethanol extract were 3.92%-7.03%, 3.65%-6.95%, 0.05%-1.03% and 10.87%-33.14%, respectively. The linear range of berberine hydrochloride was 0.183-0.915 ?g(r=0.999 9); quantitation limit and detection limit was 0.143, 0.095 μg, respectively. RSDs of precision, stability and reproducibility tests were lower than 2.0% (n=6); recovery was 95.21%-103.10%(RSD=2.95%,n=6). CONCLUSIONS: The content of moisture, total ash and acid-insoluble ash of medicinal materials is not exceed 8.0%, 6.0% and 0.4%, respectively. The content of ethanol extract and berberine hydrochloride is not less than 16.0% and 1.0%, respectively. Established standard can be used for quality control of Folium Mahoniae.
KEYWORDS Folium Mahoniae; Quality standard; HPLC; TLC
十大功勞葉味苦、寒,歸肺、肝、腎經,具有滋陰、清熱、止咳化痰的功效,貴州少數民族多用于治療肺癆咳嗽、骨蒸潮熱[1]。我國十大功勞屬的植物有250多種[2],在貴州境內有14個種,分布廣泛[3]。2003年版《貴州中藥材、民族藥材質量標準》收載了長柱十大功勞(Mahonia duclouxiana Gagnep)、小果十大功勞(M. bodinieri Gagnep)、細葉十大功勞[M. fortunei (Lindl.) Fedde]、寬苞十大功勞(M. eurybracteata Fedde)及闊葉十大功勞[M. bealei (Fort.) Carr]5個種作為十大功勞葉藥材來源[1]。但該標準中僅有藥材的性狀描述和闊葉十大功勞葉的橫切面顯微鑒別,難以評價藥材的優(yōu)劣。
小檗堿又名黃連素,為十大功勞葉藥材中主要的藥效成分,具有良好的抗菌、抗微生物、消炎的作用[4-5],這與該藥材的治療范圍相符。本研究以鹽酸小檗堿、鹽酸巴馬汀、鹽酸藥根堿為定性指標,建立了薄層色譜(TLC)定性鑒別方法;以鹽酸小檗堿為定量指標,建立了高效液相色譜(HPLC)定量法;完成了水分、灰分和醇浸出物的檢查,制訂了合理的限度,旨在為提高十大功勞葉藥材的質量標準提供一定參考。
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