摘要
目的 建立藏药五味清热汤散的HPLC指纹图谱并测定指标成分没食子酸、没食子酸甲酯、诃子联苯酸、诃子酸、鞣花酸的含量.方法 采用Ultimate XB-C18液相色谱柱(4.6 mm × 250 mm,5 μm),以0.1％磷酸水溶液(A)-甲醇(B)为流动相,梯度洗脱,流速1 mL·min-1,检测波长270 nm,柱温30℃,进样量10μL.结果 五味清热汤散指纹图谱中标识出18个共有峰,指纹图谱相似度＞0.99;指标成分没食子酸、没食子酸甲酯、诃子联苯酸、诃子酸和鞣花酸线性范围分别为2.76～55.17 μg·mL-1(r=0.9998)、1.56～31.13μg·mL-1(r=0.9997)、5.51～110.17 μg·mL-1(r=0.9999)、7.27～145.31 μg·mL-1(r=0.9998)、0.90～18.08 μg·mL-1(r=0.9997);精密度、重复性、稳定性试验的RSD均小于 2.0％(n=6);平均加样回收率分别为 98.27％(RSD=0.72％)、98.31％(RSD=0.94％)、96.48％(RSD=0.73％)、96.86％(RSD=0.80％)、96.07％(RSD=0.81％).8 批样品中没食子酸、没食子酸甲酯、诃子联苯酸、诃子酸和鞣花酸的含量分别为7.85～8.25、4.02～4.23、16.85～17.77、23.55～24.51、3.09～3.18mg·g-1.结论 建立的指纹图谱和指标成分含量测定方法具有简便、准确、稳定、快速等优点,可为五味清热汤散的质量评价提供参考.
Abstract
Objective To establish the HPLC fingerprint of the Tibetan medicine Wuwei Qingre decoction powder and determine the content of gallic acid,methyl gallate,chebulate tannic acid,chebulate acid and ellagic acid.Methods An Ultimate XB-C18 liquid chromatographic column(4.6 mm × 250 mm,5 μm)was used,with 0.1％phosphoric acid aqueous solution(A)-methanol(B)as the mobile phase,gradient elution,flow rate of 1 mL·min-1,detection wavelength of 270 nm,column temperature of 30 ℃,and injection volume of 10 μL.Results Totally 18 common peaks in the fingerprint of Wuwei Qingre decoction powder were confirmed,and the similarity of fingerprint was higher than 0.99,The linear ranges of gallic acid,methyl gallate,chebulate tannic acid,chebulate acid,and ellagic acid were 2.76～55.17 μg·mL-1(r=0.9998),1.56～31.13 μg·mL-1(r=0.9997),5.51～110.17 μg·mL-1(r=0.9999),7.27～145.31 μg·mL-1(r=0.9998),and 0.90～18.08μg·mL-1(r=0.9997),respectively.The RSDs of precision,repeatability and stability tests were all less than 2.0％(n=6).The average recoveries were 98.27％(RSD=0.72％),98.31％(RSD=0.94％),96.48％(RSD=0.73％),96.86％(RSD=0.80％)and 96.07％(RSD=0.81％)respectively.The content of the 5 components in 8 batches sample was 7.85～8.25,4.02～4.23,16.85～17.77,23.55～24.51,and 3.09～3.18 mg·g-1,respectively.Conclusion The fingerprint and content determination method is simple,accurate,stable and rapid,which can provide reference for the quality control of Wuwei Qingre decoction powder.
基金项目
西藏自治区科技厅-日喀则市人民政府区域科技协同创新专项(QYXTZX-RKZ2022-07)
NETL
NSTL
万方数据