桐叶饮片质量标准提升研究

Improvement of Quality Standard of Decoction Slices of Paulowniae Folium

目的提升桐叶饮片的质量控制标准。方法参照2020年版《中国药典(四部)》,对药材样品的显微特征、水分、总灰分、水溶性浸出物进行检测;采用薄层色谱(TLC)法对药材样品进行定性鉴别;采用高效液相色谱(HPLC)法测定药材样品中齐墩果酸和熊果酸的含量,色谱柱为Shim-pack VP-ODS柱(250 mm×4.6 mm,5μm),流动相为乙腈-甲醇-0.1 mol/L乙酸铵溶液(67∶10∶23,V/V/V),流速为1.0 mL/min,检测波长为210 nm,柱温为30℃,进样量为20μL。结果药材样品粉末呈黄绿色,显微特征清晰,可见非腺毛、腺毛、簇晶、方晶、导管等结构。TLC图斑点清晰,且分离度好。齐墩果酸和熊果酸进样量分别在235.038~4700.76 ng(r=0.9994)和509.490~5094.90 ng(r=0.9997)范围内与峰面积积分值线性关系良好;精密度、稳定性、重复性试验结果的RSD均小于2.00%;平均加样回收率分别为99.03%和99.17%,RSD分别为3.55%和3.14%(n=6)。3批药材样品的平均水分、总灰分含量分别为8.85%和5.59%,水溶性浸出物含量均大于20%;齐墩果酸、熊果酸平均含量分别为0.28%,0.83%。结论所建标准可用于桐叶饮片的质量控制。

Objective To improve the quality control standard of decoction slices of Paulowniae Folium.Methods The microscopic characteristics,moisture content,total ash and water-soluble extracts of the Paulowniae Folium were determined according to the Chinese Pharmacopoeia(2020 Edition,VolumeⅣ).Thin-layer chromatography(TLC)was used to qualitatively identify Paulowniae Folium.High-performance liquid chromatography(HPLC)method was used to determine the content of oleanolic acid and ursolic acid in Paulowniae Folium.The chromatographic column was Shim-pack VP-ODS column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-methanol-0.1 mol/L ammonium acetate solution(67∶10∶23,V/V/V),the flow rate was 1.0 mL/min,the detection wavelength was 210 nm,the column temperature was 30℃,and the injection volume was 20μL.Results The sample powder was yellow-green,with clear microscopic characteristics,including nonglandular hair,glandular hair,cluster crystal,square crystal and duct structure.The TLC spots were clear with good separation.The linear ranges of oleanolic acid and ursolic acid were235.038-4700.76 ng(r=0.9994)and 509.490-5094.90 ng(r=0.9997),respectively.The RSDs of precision,stability and repeatability tests were less than 2.00%.The average recoveries of oleanolic acid and ursolic acid were 99.03%and 99.17%with RSDs of 3.55%and 3.14%(n=6),respectively.The average content of moisture and total ash of the three batches of samples was 8.85%and 5.59%respectively,and their water-soluble extract contents were more than 20%.The average content of oleanolic acid and ursolic acid was 0.28%and 0.83%,respectively.Conclusion The established standard can be used for the quality control of decoction slices of Paulowniae Folium.