中药蝴蝶果UPLC指纹图谱及含量测定

Study on UPLC fingerprint and simultaneous determination of 5 components in Frucius Aceris Fabri

目的:建立中药蝴蝶果超高效液相色谱(UPLC)指纹图谱及没食子酸、原儿茶酸、对羟基肉桂酸、杨梅苷、槲皮苷5个成分的定量分析方法,为中药蝴蝶果质量控制提供依据。方法:采用Waters CORTECS UPLC T3色谱柱(150 mm×2.1 mm,1.6μm),以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,柱温30℃,流速0.20 mL·min^(-1),检测波长300 nm,进样量为1μL;采用“中药色谱指纹图谱相似度评价系统”生成对照指纹图谱并进行相似度分析,结合聚类分析、TOPSIS多元统计分析法进行评价。结果:建立了中药蝴蝶果UPLC指纹图谱,共标示了14个共有峰,指认了其中没食子酸、原儿茶酸、对羟基肉桂酸、杨梅苷、槲皮苷5个成分,并建立了该5个成分的定量分析方法。10批次中药蝴蝶果的指纹图谱相似度均在0.9以上,其中来源于江西的样品S9聚为Ⅰ类,质量最佳;来源于广西和广东的样品聚为Ⅱ类,质量次之;来源于江西的样品S1、S4、S6聚为Ⅲ类,质量最差。10批样品中上述5个成分的含量分别为0.236~0.356、0.118~0.398、0.108~0.141、0.146~0.222、0.046~0.104 mg·g^(-1)。结论:所建立的蝴蝶果指纹图谱及含量测定分析方法精密度高,稳定性好,可用于中药蝴蝶果的质量控制及评价。

Objective:To establish a method of UPLC fingerprint and quantitative analysis of gallic acid,protocat⁃echuic acid,p-hydroxycinnamic acid,myricitrin and quercitrin for Frucius Aceris Fabri,and to provide a refer⁃ence for the quality control of Frucius Aceris Fabri.Methods:The determination was performed on a Waters CORTECS UPLC T3 column(150 mm×2.1 mm,1.6μm),with mobile phase consisting of acetonitrile-0.1%phosphoric acid by gradually elution at a flow rate of 0.20 mL·min^(-1).The column temperature was 30℃,and detection wavelength was set at 300 nm.The quality of 10 batches of Frucius Aceris Fabri was evaluated by similarity analysis,CA and TOPSIS analysis of fingerprints.Results:The UPLC fingerprint of Frucius Aceris Fab⁃ri was established,and 14 peaks were selected as the characteristic fingerprint peaks.Five chemical components were identified,which were gallic acid,protocatechuic acid,p-hydroxycinnamic acid,myricitrin and quercitrin.And a quantitative method for the determination of the 5 chemical components was established.Good similarities were found in the established fingerprint through similarity analysis.CA and TOPSIS analysis showed that 10 bat⁃ches of Frucius Aceris Fabri samples could be clustered into 3 groups.The sample S9 from Jiangxi was classified as classⅠwith best quality.The samples from Guangxi and Guangdong were classified as ClassⅡwith medium quality.The samples S1,S4 and S6 from Jiangxi were classified asⅢwith worst quality.The linear relationship of the 5 chemical components was good,and the r values were all above 0.999.The contents of the 5 chemical components in 10 batches of samples were 0.236-0.356 mg·g^(-1),0.118-0.398 mg·g^(-1),0.108-0.141 mg·g^(-1),0.146-0.222 mg·g^(-1) and 0.046-0.104 mg·g^(-1),respectively.Conclusion:The established UPLC fingerprint and quantitative analysis methods of Frucius Aceris Fabri are precise and stable,which can be used for evaluating and controlling the quality of Frucius Aceris Fabri.