土茯苓药材HPLC指纹图谱研究及主成分的含量测定
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篇名: 土茯苓药材HPLC指纹图谱研究及主成分的含量测定
TITLE:
摘要: 目的: 建立土茯苓药材的高效液相色谱(HPLC)指纹图谱及同时测定其中落新妇苷、白藜芦醇含量的方法。方法:采用HPLC法。色谱柱为Zorbax SB-C18,流动相为甲醇-0.2%乙酸溶液(梯度洗脱),流速为1.0 ml/min,检测波长为306 nm,柱温为 30 ℃,进样量为20 μl。以落新妇苷为参照物,对13批样品HPLC图谱采用《中药色谱指纹图谱相似度评价系统》(2004 A版)进行相似度评价。结果:13批样品HPLC图谱有12个共有峰,相似度均>0.90。落新妇苷、白藜芦醇检测质量浓度线性范围分别为6.65~425.6、1.72~110 μg/ml(r均为0.999 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为97.30%~102.30%(RSD=1.97%,n=6)、98.12%~104.02%(RSD=2.57%,n=6)。结论: 该研究所建指纹图谱可为土茯苓药材的鉴别和质量评价提供参考;该测定方法操作简便,精密度、稳定性、重复性良好,可用于土茯苓药材中落新妇苷和白藜芦醇含量的同时测定。
ABSTRACT: OBJECTIVE: To establish the HPLC fingerprint and determine the contents of astilbin and resveratrol in Amilacis rhizoma. METHODS: HPLC was performed on the column of Zorbax SB-C18 with the mobile phase of methanol-0.2% acetic acid solution (gradient elution) at a flow rate of 1.0 ml/min, the detection wavelength was 306 nm, column temperature was 30 ℃,and injection volume was 20 μl. With reference of astilbin, the similarity analysis was conducted for the HPLC chromatograms of 13 batches of samples by using TCM Fingerprint Similarity Evaluation System(2004 A edition). RESULTS: There were totally 12 common peaks in the HPLC chromatograms of 13 batches of samples, similarities were all higher than 0.90. The linear range was 6.65-425.6 μg/ml for astilbin (r=0.999 9) and 1.72-110 μg/ml for resveratrol(r=0.999 9); RSDs of precision, stability and reproducibility tests were lower than 3.0%; recoveries were 97.30%-102.30%(RSD=1.97%,n=6) and 98.12%-104.02%(RSD=2.57%,n=6). CONCLUSIONS: The established fingerprint can provide reference for the identification and quality evaluation of S. rhizoma, the method is simple with good precision, stability and reproducibility, and can be used for the identification of S. rhizoma simultaneous determination of astilbin and resveratrol in S. rhizoma.
期刊: 2016年第27卷第36期
作者: 张永贵,赵力,杨小英
AUTHORS: ZHANG Yonggui,ZHAO Li,YANG Xiaoying
关键字: 土茯苓;落新妇苷;白藜芦醇;指纹图谱;含量测定
KEYWORDS: Smilacis rhizoma; Astilbin; Resveratrol; Fingerprint; Content determination
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