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ABSTRACT OBJECTIVE:To establish characteristic chromatogram of Cornus officinalis and its different wine-processed
products,investigate the differences of chromaticity values,and analyze them with chemical pattern recognition technology.
METHODS:UPLC method was adopted. Using loganin as reference,UPLC characteristic chromatograms were drawn for 10
batches of C. officinalis and 20 batches of different wine-processed products (stewing with wine,steaming with wine). TCM
Fingerprint Similarity Evaluation System(2012A edition)was used for similarity evaluation,and common peaks were confirmed.
The chromaticity values [lightness(L),red and green tone value(a),yellow and blue tone value(b),color difference value(ΔE)]
were determined by spectrophotometer. SPSS 20.0 and SIMCA 14.0 software were used for cluster analysis,principal component
analysis and partial least squares-discriminant analysis;taking the area of characteristic peak and chromaticity value as indexes,and
the variable importance projection greater than 1 as the standard,the difference markers affecting its quality were screened.
RESULTS:There were 6 common peaks in the chromatograms for decoction piece of C. officinalis,7 common peaks for
wine-processed C. officinalis(stewing with wine)and wine-processed C. officinalis(steaming with wine). Four components were
identified as gallic acid,5-hydroxymethylfurfural,morroniside,loganin. 5-hydroxymethylfurfural was produced after processing.
The similarity between C. officinalis and different wine-processed products (stewing and steaming with wine) was low
(0.869-0.937,0.845-0.944),but the similarity between different wine-processed products was higher than 0.99. ΔL,Δa,Δb and ΔE
of C. officinalis decoction pieces and wine-processed C. officinalis decoction pieces(stewing in wine)were -9.42--3.58,-24.92-
-15.00,-11.33- -7.00 and 17.01-28.12,respectively. ΔL,Δa,Δb and ΔE of C. officinalis decoction pieces and wine-processed
C. officinalis(steaming in wine)decoction pieces were -8.58--2.42,-25.08--13.83,-10.92--6.08,15.58-28.67. ΔL,Δa,Δb
and ΔE of wine-processed C. officinalis decoction pieces (stewing and steaming with wine) were -2.17-3.00,-0.75-2.50,
0.25-1.42 and 1.25-3.83,respectively. Results of cluster analysis showed that 30 batches of sample were clustered into two
categories,S1-S10 were clustered into one category,and S11-S30 were clustered into other category. Principal component analysis
showed that cumulative contribution rate of former two main components was 83.147%. Results of partial least squares-discriminant
analysis showed that morroniside,No.5 peak and chromaticity values(L,a,b)were the difference markers affecting its quality.
CONCLUSIONS:Established UPLC characteristic chromatogram is stable and feasible,and can be used to rapidly identify
C. officinalis and its different wine-processed products. Established chemical mode can be used to identify different wine-processed
products.
KEYWORDS Cornus officinalis decoction piece;Wine-processed products;UPLC;Characteristic chromatogram;Chromaticity
value;Cluster analysis;Principal component analysis;Partial least squares-discriminant analysis
山茱萸为山茱萸科植物山茱萸 Cornus officinalis 进行要求 。鉴于两者颜色均较深,指标成分均为马钱
[2]
[1]
Sieb. et Zucc.的干燥成熟果肉,始载于《神农本草经》 , 苷和莫诺苷,且酒萸肉的规定限度低于山萸肉,若存在
具有补益肝肾、收涩固脱的功效,主要用于治疗眩晕耳 混用情况,仅通过观察饮片的外观性状、色泽,则无法较
鸣、腰膝酸痛、阳痿遗精、遗尿尿频、崩漏带下、大汗虚 好地对两者进行区分。目前,关于山萸肉的研究主要涉
[2]
脱、内热消渴等症 。2020 年版《中国药典》(一部)收载 及其饮片炮制前后特征成分的含量变化 [7-10] ,而应用视
[2]
有山萸肉和酒萸肉等两种饮片 。现代研究表明,山萸 觉分析仪客观量化饮片外观色泽,同时结合其特征图谱
肉饮片长于敛汗固脱,其降血糖、抗凝血、抗心律失常作 快速鉴别的研究较少。基于此,本研究采用超高效液相
用较强;而酒制品补益肝肾作用较强,常入滋补方剂 。 色谱法(UPLC)建立山萸肉及其不同酒制品饮片的特征
[3]
可见,山茱萸不同炮制品功效差异较大,临床不宜 图谱,同时结合色差原理测定其色度值;采用聚类分析、
混用。 主成分分析、偏最小二乘法-判别分析等化学模式识别
2020年版《中国药典》(一部)中记载,酒萸肉饮片的 进行分析,旨在为山萸肉饮片及其不同酒制品饮片的快
炮制方法为酒炖或酒蒸 。安徽、北京、云南、浙江等地 速鉴别及质量综合评价提供参考。
[2]
[3]
多采用酒蒸,而江苏、广西则多采用酒炖 。2020 年版 1 材料
《中国药典》(一部)中对酒萸肉饮片的外观性状描述为 1.1 仪器
“形如山茱萸,表面紫黑色或黑色,质滋润柔软,微有酒 实验所用仪器有:H-class 型UPLC仪(包括QSM型
[2]
香气”。中药成分复杂,在炮制的动态过程中,随着饮 四元溶剂管理器、SM-FTN型样品管理器、CH-A型高温
片色泽加深,化学成分的组成与含量也随之变化。在传 柱温箱、光电二极管阵列检测器,美国 Waters 公司)、
统的中药炮制中,多以饮片外观性状、色泽作为炮制终 TS7600 型分光测色仪(深圳市三恩时科技有限公司)、
点的判别指标,但主观性较强,易导致不同产地酒萸肉 XP26 型百万分之一分析天平和 ME204E 型万分之一分
饮片的质量差异较大 [4-6] 。 析天平(瑞士 Mettler Toledo 公司)、Milli-Q Direct 8 型超
2020 年版《中国药典》(一部)对山萸肉和酒萸肉的 纯水系统(德国 Merck 公司)、KQ-500DE 型数控超声波
鉴别项、检查项、浸出物项规定均相同,未有明确区分; 清洗器(昆山市超声仪器有限公司)、H22-X3 型电陶炉
虽然两者的含量测定采用同种指标成分,但以不同限度 (杭州九阳生活电器有限公司)。
中国药房 2021年第32卷第2期 China Pharmacy 2021 Vol. 32 No. 2 ·207 ·