酢浆草的HPLC指纹图谱建立及2种有效成分的含量测定
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篇名: 酢浆草的HPLC指纹图谱建立及2种有效成分的含量测定
TITLE: Establishment of HPLC Fingerprint and Content Determination of Two Components of Oxalis corniculata
摘要: 目的:建立酢浆草的高效液相(HPLC)指纹图谱,并同时测定其中异牡荆素、当药黄素的含量。方法:采用HPLC法。色谱柱为ACEExcel-5-C18,流动相为甲醇-0.1%磷酸水溶液(梯度洗脱),流速为1mL/min,柱温为35℃,检测波长为280nm,进样量为10μL。以异牡荆素峰为参照,绘制12批酢浆草药材样品的HPLC指纹图谱,采用《中药色谱指纹图谱相似度评价系统(2012版)》进行相似度评价,确定共有峰。按上述色谱条件同法测定异牡荆素、当药黄素的含量。结果:12批酢浆草药材样品共有19个共有峰,相似度均大于0.89,同时指认异牡荆素、当药黄素2个共有峰。异牡荆素、当药黄素检测质量浓度的线性范围分别为3.91~117.36μg/mL(r=0.9994)、9.88~118.56μg/mL(r=0.9992);定量限分别为0.675、3.587μg/mL;检测限分别为0.205、1.087μg/mL;精密度、重复性、稳定性试验的RSD均小于2%;加样回收率分别为95.46%~99.10%(RSD=1.23%,n=6)、95.34%~101.23%(RSD=2.74%,n=6);平均含量分别为0.227~1.654、0.641~2.052mg/g。结论:所建指纹图谱可用于酢浆草药材的质量控制;含量测定方法简便、准确,可用于同时测定其中2种成分的含量。
ABSTRACT: OBJECTIVE:To establish the HP LC fing erprints of Oxalis corniculata and to simultaneously determine the contents of isovitexin and swertisin. METHODS :HPLC method was adopted. The determination was performed on ACE Excel- 5-C18column with mobile phase consisted of methanol- 0.1% phosphoric acid water (gradient elution )at the flow rate of 1 mL/min. The column temperature was 35 ℃,and detection wavelength was set at 280 nm. The sample size was 10 μL. Using isovitexin peak as reference,HPLC fingerprints of 12 batches of sample were drawn. The similarity evaluation was performed by using Similarity Evaluation System of Chromatogram Fingerprint of TCM (2012 edition)to determine common peaks. The contents of isovitexin and swertisin were determined by same method of above chromatogram. RESULTS :There were 19 common peaks in HPLC chromatogram of 12 batches of O. corniculata ,with the similarity above 0.89. Two common peaks including isovitexin and swertisin were identified. The linear range of two components were 3.91-117.36 μg/mL(r=0.999 4)and 9.88-118.56 μg/mL(r= 0.999 2),respectively. The limits of quantitation were 0.675 and 3.587 μg/mL;the limits of detection were 0.205 and 1.087 μg/mL, respectively. RSDs of precision ,stability and reproducibility tests were all lower than 2%. The recoveries were 95.46%-99.10% (RSD=1.23% ,n=6),95.34% -101.23%(RSD=2.74% ,n=6),respectively. The average contents were 0.227-1.654, 0.641-2.052 mg/g,respectively. CONCLUSIONS :Established fingerprints can be used for the quality control of O. corniculata ; the content determination method is simple and accu rate,and can be used for simultaneous determination of two components.
期刊: 2020年第31卷第06期
作者: 李小双,李银,刘文静,王广成,郑林,陈思颖,李勇军
AUTHORS: LI Xiaoshuang,LI Yin,LIU Wenjing,WANG Guangcheng,ZHENG Lin,CHEN Siying,LI Yongjun
关键字: 酢浆草;高效液相色谱法;指纹图谱;异牡荆素;当药黄素;含量测定
KEYWORDS: Oxalis corniculata ; HPLC; Fingerprint;
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