小金胶囊的HPLC指纹图谱建立及主成分分析
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篇名: 小金胶囊的HPLC指纹图谱建立及主成分分析
TITLE:
摘要: 目的:建立小金胶囊的高效液相色谱(HPLC)指纹图谱,并进行主成分分析。方法:采用HPLC法。色谱柱为Agilent TC-C18(2),流动相为乙腈-0.2%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为240 nm,柱温为25 ℃,进样量为20 μL。以11-羰基-β-乙酰乳香酸为参照,绘制15批样品的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,确定共有峰,并采用Minitab 17.0软件进行主成分分析。结果:有1批样品相似度小于0.800,且与其他14批样品比较缺13、14、15号共有峰,可能存在质量差异而未进行相关分析。其余14批样品的HPLC图谱有15个共有峰,指认了3个色谱峰,分别为槲皮素、穗花杉双黄酮、11-羰基-β-乙酰乳香酸;14批样品的相似度为0.889~0.990。经主成分分析,2个主成分因子的累积方差贡献率为94.4%,样品中8、9、11、12、14号共有峰(特别是8、9号共有峰)对应成分的含量变化是导致样品质量差异的重要原因。结论:所建指纹图谱及主成分分析结果可为小金胶囊的质量评价提供参考。
ABSTRACT: OBJECTIVE: To establish HPLC fingerprint of Xiaojin capsules, and to conduct principal component analysis. METHODS: HPLC method was adopted. The determination was performed on Agilent TC-C18(2) column with mobile phase consisted of acetonitrile-0.2% formic acid solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was 240 nm, and column temperature was 25 ℃. The sample size was 20 μL. Acetyl-11-keto-β-boswellic acid was used as reference and HPLC fingerprints of 15 batches of Xiaojin capsules were determined. The similarity evaluation of common peaks was conducted by using the TCM Chromatographic Fingerprint Similarity Evaluation System (2004A edition) to confirm common peaks. Principal component analysis was conducted by using Minitab 17.0 software. RESULTS: The similarity of 1 batch of sample was lower than 0.800; there was no common peaks No. 13, 14, 15 in HPLC chromatogram of the batch, compared with other 14 batches. There were 15 common peaks in the HPLC fingerprints of 14 batches of samples and three chromatographic peaks were identified, such as quercetin,amentoflavone, acetyl-11-keto-β-boswellic acid. The similarity of 14 batches ranged 0.889-0.990. Through principal component analysis, accumulative contribution rate of 2 principal component factors was 94.4%. It was indicated that the content change of corresponding components of common peaks No. 8, 9, 11, 12, 14 in samples was an important reason for the quality difference of samples, especially common peaks No.8, 9. CONCLUSIONS: The established HPLC fingerprint and principal component analysis can provide reference for quality evaluation of Xiaojin capsules.
期刊: 2019年第30卷第2期
作者: 明凯利,向阳,杨艳霞,曾添,王丫头,蔡威,朱雯
AUTHORS: MING Kaili,XIANG Yang,YANG Yanxia,ZENG Tian,WANG Yatou,CAI Wei,ZHU Wen
关键字: 小金胶囊;高效液相色谱法;指纹图谱;主成分分析
KEYWORDS: Xiaojin capsules; HPLC; Fingerprint; Principal component analysis
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