不同产地芫花质量标准研究

Study on Quality Standard of Genkwa Flos from Different Habitats

目的:进一步完善和提高芫花药材的质量标准。方法:采用薄层色谱法对芫花中芫花素进行定性鉴别,高效液相色谱法进行定量测定,并建立芫花HPLC指纹图谱;常规检查项目(杂质、水分、总灰分、酸不溶性灰分、重金属、黄曲霉毒素、水和醇溶性浸出物)参照2015年版《中国药典》通则的相关方法进行测定。结果:芫花薄层斑点清晰,分离度好。芫花素在1~240μg/mL范围内有良好线性关系(r=0.9991),加样回收率98.06%~101.67%(RSD=0.87%);10批样品中,HPLC指纹图谱相似度均大于0.950;芫花素含量:939.60~2146.45 mg/kg;杂质含量:0.47%~2.94%;水分含量:8.4%~11.81%;总灰分:4.34%~6.33%,酸不溶性灰分:0.32%~0.44%;水和醇溶性浸出物含量分别:16.73%~26.57%和13.69%~24.90%;砷、镉、汞和铅含量分别:0.429~0.948 mg/kg,0.332~0.995 mg/kg,未检出,3.438~4.752 mg/kg;黄曲霉毒素未检出。结论:所建立的方法简便、准确、重复性好,可用于芫花的质量控制。

Objective: To improve the quality standard of Genkwa Flos. Methods: TLC was used to qualitatively authentication of the medicinal materials. The content of genkwanin was determined by HPLC and the fingerprint of Genkwa Flos was established.The water content, total ash content, acid-insoluble ash content, aflatoxin, foreign matter, Heavy metals and extractives were determined according to the General Principles of the Chinese Pharmacopoeia(2015 edition). Results: The bands of TLC chromatograph of Genkwa Flos were distinct and reproducible. The content of genkwanin had a good linear relationship with the chromatographic peak area between 1 ~ 240 μg/mL(r=0.9991). The recovery was 98.06% ~ 101.67% with RSD 0.87%. Among 10 batches of Genkwa Flos samples, the similarity of HPLC fingerprint was higher than 0.950;the content of genkwanin was 939.60 ~ 2146.45 mg/kg, the foreign matter contents were 0.47% ~ 2.94%;the water contents were 8.4% ~ 11.81%;total ash contents were 4.34% ~ 6.33%, acid-insoluble ash contents were 0.32% ~ 0.44%;water and alcohol soluble extract contents were16.73% ~ 26.57% and 13.69% ~ 24.90%, respectively;The contents of As, Cr, Hg and Pb were 0.429 ~ 0.948 mg/kg, 0.332 ~ 0.995 mg/kg, not detected, 3.438 ~ 4.752 mg/kg, respectively;Aflatoxin was not detected in any collected samples.Conclusion: The established methods are simple, accurate and can be used as quality standard control of this herbal medicine.