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干鱼腥草药材及饮片的指纹图谱建立、化学计量学分析及含量测定
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| 篇名： | 干鱼腥草药材及饮片的指纹图谱建立、化学计量学分析及含量测定 |
| TITLE： | Study on the fingerprint establishment ，chemometrics analysis and content determination of dried Houttuynia cordata and its decoction pieces |
| 摘要： | 目的 建立干鱼腥草药材及饮片的指纹图谱，并进行化学计量学分析，同时测定其中新绿原酸等5种黄酮类成分的含量。方法采用高效液相色谱（HPLC）法，以槲皮苷为参照，绘制10批干鱼腥草药材及饮片的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；采用SIMCA-P14.1软件进行主成分分析（PCA）和偏最小二乘法-判别分析（PLS-DA），以变量重要性投影（VIP）值大于1为标准筛选影响干鱼腥草药材及饮片质量的差异性成分；采用同一HPLC法测定干鱼腥草药材及饮片中新绿原酸等5种成分的含量。结果10批干鱼腥草药材及饮片均有20个共有峰，相似度均大于0.960；共指认了其中5个共有峰，分别为新绿原酸（1号峰）、绿原酸（3号峰）、隐绿原酸（4号峰）、芦丁（7号峰）、槲皮苷（11号峰）。PCA和PLS-DA结果均显示，干鱼腥草药材及饮片各自分为一类；VIP值大于1的共有峰依次为7号峰（芦丁）、20号峰、5号峰、13号峰、2号峰、18号峰、3号峰（绿原酸）、14号峰、17号峰和19号峰。新绿原酸、绿原酸、隐绿原酸、芦丁和槲皮苷检测质量浓度的线性范围分别为3.77～60.29μg/mL（r＝0.9997）、1.40～22.42μg/mL（r＝0.9995）、3.76～60.22μg/mL（r＝0.9999）、2.19～35.06μg/mL（r＝0.9999）、25.49～407.88μg/mL（r＝0.9997）；精密度、稳定性（24h）、重复性试验的RSD均小于3％；干鱼腥草药材及饮片中上述5种成分的平均加样回收率分别为98.72％～101.12％、98.86％～100.63％（RSD均小于3％，n＝9）。干鱼腥草药材中上述5种成分的平均含量分别为0.87、0.33、0.59、0.61、6.17mg/g，饮片中分别为0.42、0.11、0.26、0.23、3.16mg/g。结论所建指纹图谱及含量测定方法稳定、可行，可用于干鱼腥草药材及饮片的质量控制；芦丁等成分可能是影响其药材及饮片质量的差异性成分；干鱼腥草药材经炮制后，新绿原酸等5种黄酮类成分的平均含量均有所降低。 |
| ABSTRACT： | OBJECTIVE To establish the fingerprints of dried Houttuynia cordata and its decoction pieces ，conduct chemometrics analysis and determine the contents of 5 flavonoids such as neochlorogenic acid. METHODS High performance liquid chromatography （HPLC）method was adopted. Using quercitrin as reference ，HPLC fingerprints of 10 batches of dried H. cordata and its decoction pieces were drawn. The similarity evaluation was conducted by Similarity Evaluation System of TCM Chromatographic Fingerprint （2012 edition），the common peaks were also confirmed. SIMCA-P 14.1 software was applied for principal component analysis （PCA）and partial least square-discriminant analysis （PLS-DA），and the variable importance in projection（VIP）value more than 1 was considered as a standard to screen the differential components affecting the quality of these two products ；meanwhile，the contents of 5 components such as neochlorogenic acid in both products were determined by the same HPLC method. RESULTS There were 20 common peaks in 10 batches of dried H. cordata and 10 batches of its decoction pieces with the similarity values more than 0.960. A total of 5 common peaks were identified ，which were neochlorogenic acid （peak 1）， chlorogenic acid （peak 3），cryptochlorogenic acid （peak 4），rutin（peak 7）and quercitrin （peak 11）. The results of PCA and PLS-DA showed that dried H. cordata could be distinguished from its decoction pieces obviously ；the common peaks with VIP value greater than 1 were as follows ：peak 7（rutin），peak 20，peak 5，peak 13，peak 2，peak 18，peak 3（chlorogenic acid ）， peak 14，peak 17 and peak 19. The linear range of neochlorogenic acid ，chlorogenic acid ，cryptochlorogenic acid ，rutin and quercitrin were 3.77-60.29 μg/mL（r＝0.999 7），1.40-22.42 μg/mL（r＝0.999 5），3.76-60.22 μg/mL（r＝0.999 9），2.19-35.06 μg/mL （r＝0.999 9）and 25.49-407.88 μg/mL（r＝0.999 7），respectively. RSDs of precision ，stability（24 h）and reproducibility E-mail：20190394@njucm.edu.cn tests were all lower than 3％. The average recoveries of the above components in these two products were 98.72％-101.12％ and 98.86％ -100.63％ with RSDs less than 3％（n＝9）. In dried H. cordata ，the average contents of 5 components were 0.87，0.33，0.59，0.61 and 6.17 mg/g，while the average contents were 0.42，0.11，0.26，0.23 and 3.16 mg/g in its decoction pieces ，respectively. CONCLUSIONS HPLC fingerprint and the method of content determination are stable and feasible ，which could be used for the quality control of dried H. cordata and its decoction pieces. Besides ，rutin and other components may be the differential components which could affect the quality of these two products ；the average contents of the 5 flavonoids such as neochlorogenic acid in dried H. cordata all decrease after processing. |
| 期刊： | 2022年第33卷第08期 |
| 作者： | 王静，朱广飞，梁思予，张科卫，陆兔林，毛春芹 |
| AUTHORS： | WANG Jing，ZHU Guangfei ，LIANG Siyu，ZHANG Kewei ，LU Tulin，MAO Chunqin |
| 关键字： | 干鱼腥草；药材；饮片；指纹图谱；含量测定；高效液相色谱法；化学计量学分析 |
| KEYWORDS： | dried Houttuynia cordata ； medicinal material ； decoction pieces ； fingerprint； content determination ； high |
| 阅读数： | 182 次 |
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