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1.山东中医药大学 药学院,济南 250355
2.山东宏济堂制药集团股份有限公司,济南 250103
3.山东省食品药品审评查验中心,济南 250014
4.北京中医药大学,北京 100102
王帅,在读硕士,从事中药新药与中药炮制原理研究,E-mail:1747403648@qq.com
张超,博士,教授,从事中药新药与中药炮制原理研究,Tel:0531-89628590,E-mail:tougaotcm@163.com
收稿日期:2021-11-02,
网络出版日期:2022-01-27,
纸质出版日期:2022-11-05
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王帅,王丽丽,房娟娟等.滇黄精酒制过程中颜色与5种成分含量变化的相关性分析[J].中国实验方剂学杂志,2022,28(21):156-162.
WANG Shuai,WANG Lili,FANG Juanjuan,et al.Correlation Analysis Between Color and Content Changes of Five Components of Wine-processed Polygonatum kingianum Rhizoma During Processing[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(21):156-162.
王帅,王丽丽,房娟娟等.滇黄精酒制过程中颜色与5种成分含量变化的相关性分析[J].中国实验方剂学杂志,2022,28(21):156-162. DOI: 10.13422/j.cnki.syfjx.20220252.
WANG Shuai,WANG Lili,FANG Juanjuan,et al.Correlation Analysis Between Color and Content Changes of Five Components of Wine-processed Polygonatum kingianum Rhizoma During Processing[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(21):156-162. DOI: 10.13422/j.cnki.syfjx.20220252.
目的
2
研究滇黄精酒制过程样品粉末外观颜色与5个非糖类成分含量的关联性,确定颜色量化值用于判断酒黄精炮制终点的可行性,从甾体皂苷和黄酮类成分中筛选滇黄精酒制过程控制标志物。
方法
2
利用色差仪量化滇黄精酒制不同时间点样品粉末的表观颜色变化,计算总色值(
E
*
ab
)、总色差值(Δ
E
*
ab
),采用超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定炮制0、5、10、14、16、18、20、22、24、26、28 h的酒黄精(编号S0~S10)中原薯蓣皂苷、伪原薯蓣皂苷、薯蓣皂苷、薯蓣皂苷元和水仙苷的含量,利用多元统计方法对样品粉末色度值与5个成分含量进行聚类分析(HCA)、主成分分析(PCA)、偏最小二乘法-判别分析(PLS-DA)及Pearson相关性分析。
结果
2
在滇黄精酒制过程中,样品粉末
E
*
ab
呈下降趋势,外观颜色由浅黄色向漆黑色变化;5个成分含量随时间动态变化趋势明显,且呈现出不同的变化规律。HCA结果显示,滇黄精酒制过程大致分为3个阶段,即炮制前期(样品S0~S1)、中期(样品S2~S4)和后期(样品S5~S10);PCA结果显示,初始样品与炮制过程样品的颜色、5个成分含量存在较大差异,样品S8和S9的差异最小;PLS-DA结果显示,
b
*
、伪原薯蓣皂苷含量、水仙苷含量、薯蓣皂苷元含量和原薯蓣皂苷含量的变量重要性投影(VIP)值均
>
1;Pearson相关性分析结果显示,原薯蓣皂苷、薯蓣皂苷和水仙苷的含量与
E
*
ab
呈显著正相关(
P
<
0.01),薯蓣皂苷元含量与
E
*
ab
呈显著负相关(
P
<
0.01),而伪原薯蓣皂苷含量与
E
*
ab
无线性相关。
结论
2
在滇黄精酒制过程中,颜色量化值与化学成分之间存在一定的相关性,且能客观判定酒黄精的炮制终点,可考虑将原薯蓣皂苷作为滇黄精酒制过程控制的标志物。
Objective
2
To study the correlation between the appearance color of the sample powder and the contents of five non-sugar components of wine-processed
Polygonatum kingianum
rhizoma during processing, and determine the feasibility of color quantitative value for judging the processing end point of the wine-processed products, and to screen steroidal saponins and flavonoids as markers for the control of the wine-processed products during processing.
Method
2
The changes of apparent color of the sample powder at different time points of the wine-processed products were measured by colorimeter, and the total color value (
E
*
ab
),the total color difference value (Δ
E
*
ab
) were calculated. The contents of protodioscin, pseudoprotodioscin, dioscin, diosgenin and narcissoside in the wine-processed products (No. S0-S10) after processing for 0, 5, 10, 14, 16, 18, 20, 22, 24, 26, 28 h were determined simultaneously by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Cluster analysis (HCA), principal component analysis (PCA), partial least squares discriminant analysis (PLS-DA) and Pearson correlation analysis were used to analyze the chromaticity value of the sample powder and the content of the five components.
Result
2
During processing of wine-processed
P. kingianum
rhizoma,
E
*
ab
of the sample powder showed a decreasing trend and the apparent color changed from light yellow to lacquer black. The contents of the five components showed an obvious dynamic change trend with time, and showed different laws. HCA results showed that the processing process of the wine-processed products could be divided into three stages, namely, the early stage (samples S0-S1), the middle stage (samples S2-S4) and the late stage (samples S5-S10). PCA results showed that there were significant differences in color and contents of five components between the initial sample and the processing samples, and the difference between samples S8 and S9 was the smallest. PLS-DA results showed that the variable importance in the projection (VIP) values of
b
*
, the contents of pseudoprotodioscin, narcissoside, diosgenin and protodioscin were
>
1. Pearson correlation analysis showed that the contents of protodioscin, diosgenin and narcissoside had a significant positive correlation with
E
*
ab
(
P
<
0.01), the content of diosgenin had a significant negative correlation with
E
*
ab
(
P
<
0.01), while the content of pseudoprotodioscin had no linear correlation with
E
*
ab
.
Conclusion
2
In the process of wine-processed
P. kingianum
rhizoma, there is a certain linear correlation between color quantitative value and chemical composition, and the processing end point can be determined objectively. It can be considered that protodioscin can be used as a marker for the control of the wine-processed products.
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