摘要
目的:以色空间法结合统计学分析探究当归炭炮制过程中外观颜色及理化性质的变化规律,为当归炭炮制终点确定和饮片质量评价提供参考。方法:以炮制时间(4、8、12、16 min)和炮制温度(180、200、220、240℃)为影响因素,采用完全随机实验设计制备不同炮制程度的当归炭饮片;采用分光测色仪测定当归炭明暗度值(L^(*))、红绿色度值(a^(*))、黄蓝色度值(b^(*))和总色度值(E^(*)ab),并计算色差值(ΔE),通过判别分析法对当归炭色度值数据进行分析;采用pH计、紫外-可见分光光度法和超高效液相色谱法分别测定不同炮制程度当归炭的pH、炭素吸附力,以及鞣质、5-羟甲基糠醛(5-HMF)、色氨酸、绿原酸、阿魏酸、洋川芎内酯I、洋川芎内酯H、藁本内酯的含量。利用主成分分析(PCA)对各理化指标数据进行分析,确定当归炭炮制工艺后,建立区分不同炮制程度当归炭饮片的典则判别函数并进行留一法交叉验证;Pearson相关性分析探究各理化指标成分与色度值之间的关联。结果:随着炮制时间延长,L^(*)、a^(*)、b^(*)、E^(*)ab均呈下降趋势,建立的基于颜色参数的判别模型能对不同炮制程度的当归炭进行区分。随炮制时间延长,pH呈上升趋势,炭素吸附力、鞣质、5-HMF、色氨酸的含量均呈现先增后降的趋势,其中炭素吸附力和鞣质、5-HMF含量在炮制8~12 min时相继达到最大值;绿原酸、阿魏酸、洋川芎内酯I、洋川芎内酯H、藁本内酯的含量均呈下降趋势,在炮制至8 min时下降60%~80%,最佳炮制时间应为8~12 min。PCA可明显区分不同炮制时间的当归炭,而温度对炮制程度无明显影响。12批工艺验证结果(10 min,180~240℃)显示,除3个批次被判别为Ⅱ类轻炭外,其余批次均判别为Ⅲ类标准炭,且各批次当归炭色度值指标均在Ⅱ~Ⅲ类当归炭色度值参考值范围内。相关性分析结果显示,各色度值与pH、炭素吸附力均呈负相关,与色氨酸、绿原酸、阿魏酸、洋川芎内酯I、洋川芎内酯H、藁本内酯含量均呈正相关;pH和炭素吸附力与上述成分含量均呈负相关;炭素吸附力与5-HMF含量呈正相关。结论:当归炭的色度值和各理化指标成分含量随炮制时间延长发生明显改变,且色度值和各理化成分指标之间普遍存在相关性,结合色泽及理化指标变化情况确定当归炭的最佳炮制时间应为8~12 min。该研究揭示了当归炭炮制过程的相关指标动态变化规律,可为当归炭炮制程度判别及炮制终点量化研究提供参考。
Objective:To study the changing law of appearance color and physicochemical properties of Angelicae Sinensis Radix Carbonisata(ASRC)during the processing by color space method combined with statistical analysis,so as to provide reference for determining the processing endpoint and evaluating the quality of the decoction pieces.Methods:Taking processing time(4,8,12,16 min)and temperature(180,200,220,240℃)as factors,ASRC decoction pieces with different processing degrees were prepared in a completely randomized design.Then,the brightness value(L^(*)),red-green value(a^(*)),yellowblue value(b^(*)),and total chromaticity value(E^(*)ab)of the decoction pieces were determined by spectrophotometer,the color difference value(ΔE)was calculated,and the data of colorimetric values were analyzed by discriminant analysis.At the same time,the pH,charcoal adsorption,and contents of tannins,5-hydroxymethylfurfural(5-HMF),tryptophan,chlorogenic acid,ferulic acid,senkyunolide I,senkyunolide H and ligustilide of ASRC with different processing degrees were determined by pH meter,ultraviolet and visible spectrophotometry and ultra-high performance liquid chromatography(UPLC).Principal component analysis(PCA)was used to analyze the data of physicochemical indexes,after determining the processing technology of ASRC,the canonical discriminant function was established to distinguish the decoction pieces with different processing degrees,and leave-oneout cross validation was conducted.Finally,Pearson correlation analysis was used to explore the correlation between various physicochemical indexes and chromaticity values.Results:With the prolongation of the processing time,L^(*),a^(*),b^(*)and E^(*)ab all showed a decreasing trend,and the established discriminant model based on color parameters was able to distinguish ASRC with different processing degrees.The pH showed an increasing trend with the prolongation of processing time,and the charcoal adsorption,and the contents of tannins,5-HMF,and tryptophan all showed an increasing and then decreasing trend.Among them,the charcoal adsorption,contents of tannin and 5-HMF reached their maximum values successively after processing for 8-12 min.While the contents of chlorogenic acid,ferulic acid,senkyunolide I,senkyunolide H and ligustilide decreased with the increase of processing time,with a decrease of 60%-80%at 8 min of processing.Therefore,the optimal processing time should be determined to be 8-12 min.PCA could clearly distinguish ASRC with different processing degrees,while temperature had no significant effect on the processing degree.The 12 batches of process validation results(10 min,180-240℃)showed that except for 3 batches identified as classⅡlight charcoal,all other batches were identified as classⅢstandard charcoal,and the chromaticity values of each batch of ASRC were within the reference range of classⅡ-Ⅲsample chromaticity values.The correlation analysis showed that the chromaticity values were negatively correlated with pH and charcoal adsorption,and positively correlated with contents of tryptophan,chlorogenic acid,ferulic acid,senkyunolide I,senkyunolide H,and ligustilide.And both pH and charcoal adsorption were negatively correlated with the contents of the above components,but the charcoal adsorption was positively correlated with the content of 5-HMF.Conclusion:The chromaticity values and the contents of various physicochemical indicators of ASRC undergo significant changes with the prolongation of processing time,and there is a general correlation between chromaticity values and various physicochemical indicators.Based on the changes in color and physicochemical indicators,the optimal processing time for ASRC is determined to be 8-12 min.This study reveals the dynamic changes of the relevant indexes in the processing of ASRC,which can provide a reference for the discrimination of the processing degree and the quantitative study of the processing endpoint.
作者
覃柳莹
黄瑶
甘力帆
刘远俊
邓淙友
孙冬梅
梁丽金
周林
QIN Liuying;HUANG Yao;GAN Lifan;LIU Yuanjun;DENG Congyou;SUN Dongmei;LIANG Lijin;ZHOU Lin(Guangdong Provincial Key Laboratory of Traditional Chinese Medicine Formula Granules in Enterprises,Guangdong Efong Pharmaceutical Co.Ltd.,Foshan 528244,China)
出处
《中国实验方剂学杂志》
北大核心
2025年第9期201-210,共10页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家工信部产业技术基础公共服务平台项目(2022-230-221)
佛山市南海区重点领域科技攻关专项(南科[2023]20号-18)。
关键词
当归
炮制
炒炭存性
色度值
判别分析
成分分析
相关性分析
Angelicae Sinensis Radix
processing
fried charcoal survivability
chromaticity value
discriminant analysis
component analysis
correlation analysis
