CN-121978290-A - Quality evaluation method for spatholobus stem decoction pieces based on excellent shape and high quality

CN121978290ACN 121978290 ACN121978290 ACN 121978290ACN-121978290-A

Abstract

The invention discloses a spatholobus stem decoction piece quality evaluation method based on a 'excellent shape and high quality' theory, and belongs to the technical field of traditional Chinese medicine quality evaluation. According to the method, the appearance property indexes (powder color delta E is more than or equal to 35, diameter and maximum number of turns of a tangent plane) and the internal quality indexes (catechin, epicatechin and alcohol-soluble extract content) of the suberect spatholobus stem decoction pieces are measured, key property indexes (number of turns, diameter and delta E) are screened out by utilizing principal component analysis, correlation analysis and partial least squares discriminant analysis (OPLS-DA), and quantitative association and prediction models of the key property indexes and the internal component content are established. By setting key character threshold values (delta E is more than or equal to 35, turns are more than or equal to 5, and diameters are more than or equal to 5.0 cm) or using a prediction model, the quick and objective evaluation of the quality of the suberect spatholobus stem decoction pieces can be realized, the traditional subjective identification and complex instrument detection can be effectively replaced, and reliable standards are provided for medicinal material quality control and market circulation.

Inventors

TIAN HUI
ZHANG JUANJUAN
PAN XIAOJIAO
HUANG YONG
Han Qizhen
OU HAIJIE
LIU XUEMEI
ZHANG YATING

Assignees

广西中医药大学

Dates

Publication Date: 20260505
Application Date: 20260208

Claims (7)

1. A spatholobus stem decoction piece quality evaluation method based on 'excellent shape and high quality' is characterized by comprising the following steps: 1) Obtaining 8 index data of spatholobus stem Obtaining index data of suberect spatholobus stem decoction pieces to obtain 6 appearance character index data of suberect spatholobus stem decoction pieces, wherein the index data comprise powder colors (delta L, delta a, delta b and delta E), decoction piece diameters and decoction piece maximum circle numbers; obtaining 2 pieces of internal quality index data of caulis Spatholobi decoction pieces, namely catechin content and epicatechin content measured by High Performance Liquid Chromatography (HPLC), and alcohol-soluble extract content measured by referring to pharmacopoeia method; 2) Principal component analysis A) Data preprocessing and modeling Constructing a suberect spatholobus stem decoction piece 'character-quality' sample database based on 8 index data obtained in the step 1), carrying out standardized pretreatment on the data in the database, determining the association direction and strength of appearance character indexes and internal quality indexes through Pearson correlation analysis, screening character indexes which contribute significantly to quality classification by adopting partial least squares discriminant analysis (OPLS-DA), and constructing a prediction model of appearance characters on internal quality by utilizing multiple regression analysis; B) Key trait index screening Screening out 2-3 key appearance property indexes capable of representing the quality of suberect spatholobus stem decoction pieces according to an OPLS-DA result (variable importance projection value VIP > 1) and Pearson correlation significance level (P < 0.05); 3) Quality evaluation And (3) evaluating the quality of the suberect spatholobus stem decoction pieces based on the prediction model constructed by the key appearance character indexes screened in the step (2).
2. The method for evaluating the quality of spatholobus stem decoction pieces based on excellent shape and quality according to claim 1, wherein in the step 1), the method for measuring the appearance property index is as follows: a) Powder color parameter determination Spreading proper amount of caulis Spatholobi decoction pieces powder in a cuvette, measuring DeltaL, deltaa and Deltab by using a spectrocolorimeter (the light source is D65 and the aperture is 8 mm), measuring 3 parts of each batch of samples in parallel, measuring 6 times at random, and taking an average value to calculate a comprehensive color difference value DeltaE; B) Diameter measurement of decoction pieces Measuring the cross-section diameter of the suberect spatholobus stem decoction pieces by using a vernier caliper, measuring 3 decoction pieces for each batch of samples, and taking an average value; C) Measuring the maximum number of turns of decoction pieces: the cross section of the suberect spatholobus stem decoction pieces is visually observed, the maximum number of turns of the reddish brown layer is counted, 3 decoction pieces are measured for each batch of samples, and the average value is obtained.
3. The method for evaluating the quality of the spatholobus stem decoction pieces based on excellent quality of claim 1 is characterized in that in the step 1), catechin content and epicatechin content are measured by an HPLC method, and specific conditions are that a chromatographic column is an X-Peonyx chromatographic column, a mobile phase is acetonitrile (A) -0.1% phosphoric acid aqueous solution (B), a gradient elution program is 0-10 min, 5-15% A, 10-20 min, 15-25% A, 20-30 min, 25-35% A, 30-40 min, 35-5%A, a detection wavelength is 280nm, a volume flow is 1.0 mL-min -1 , a sample injection amount is 10 mu L, and a column temperature is 30 ℃.
4. The method for evaluating the quality of spatholobus stem decoction pieces based on excellent quality according to claim 3, wherein the preparation method of the sample solution and the reference solution in the HPLC method is as follows: a) Preparation of control solution Precisely weighing catechin standard substance and epicatechin standard substance, dissolving with 45% methanol solution to obtain mixed reference substance solutions with concentration of 1.36mg/mL and 1.15mg/mL, filtering with 0.22 μm filter membrane, and storing at 4deg.C; b) Preparation of test solution Precisely weighing 1.0g of caulis Spatholobi decoction piece powder (sieving with No. 3 sieve), placing in a conical flask with a plug, adding 60mL of methanol, standing for 30min, performing ultrasonic extraction for 45min, filtering, collecting filtrate, evaporating filtrate in water bath, dissolving residue with 20mL of distilled water, transferring to a separating funnel, adding 20mL of ethyl acetate for extraction, repeating for 4 times, combining the extractive solutions, concentrating under reduced pressure to dryness, dissolving residue with 45% methanol and fixing volume to 10mL volumetric flask, filtering with 0.22 μm filter membrane, and collecting subsequent filtrate.
5. The method for evaluating the quality of spatholobus stem decoction pieces based on excellent quality according to claim 1, wherein in the step 1), the method for measuring the content of the alcohol-soluble extract is as follows: Precisely weighing caulis Spatholobi decoction piece powder (sieving with No. 3 sieve) about 2g, placing in conical flask, adding 95% ethanol 45mL, sealing, weighing, standing for 1 hr, condensing, refluxing for slightly boiling for 1 hr, cooling, weighing, supplementing with 95% ethanol for weight loss, filtering, evaporating filtrate 25mL in water bath, drying in 105 deg.C drying oven for 3 hr, cooling for 30min, precisely weighing, and calculating alcohol soluble extract content.
6. The method for evaluating the quality of spatholobus stem decoction pieces based on excellent quality according to claim 1, wherein in the step 2), a Z-score standardization method is adopted for data preprocessing, and a data analysis tool is implemented by carrying out Pearson correlation analysis and multiple regression analysis through SPSS26.0 software and OPLS-DA through SIMCA14.1 software.
7. The method for evaluating the quality of spatholobus stem decoction pieces based on excellent quality according to claim 1, wherein in the step 3), the criterion of the quality evaluation is: When the key appearance property index meets delta E of more than or equal to 35, the maximum circle number of more than or equal to 5 and the diameter of more than or equal to 5.0cm, judging the tablet as high-quality suberect spatholobus stem decoction pieces, or comparing the internal quality predicted value calculated by a prediction model with a preset high-quality decoction piece component content threshold (catechin of more than or equal to 0.8mg/g and epicatechin of more than or equal to 0.6 mg/g), and judging the tablet as high-quality decoction pieces when the tablet meets the threshold requirement.

Description

Quality evaluation method for spatholobus stem decoction pieces based on excellent shape and high quality Technical Field The invention belongs to the technical field of traditional Chinese medicine quality evaluation, and particularly relates to a spatholobus stem decoction piece quality evaluation method based on an excellent shape high-quality theory, which realizes objective and rapid evaluation of the quality of spatholobus stem decoction pieces and provides technical support for quality control and standardized application of spatholobus stem decoction pieces. Background Caulis Spatholobi is firstly carried in the Chancan Su Yi (compendium of materia Medica), is a dry rattan of the bean (Spatholobus suberectus Dunn) of the Leguminosae plant, has the effects of activating blood circulation, replenishing blood, regulating menstruation, relieving pain, relaxing tendons, activating collaterals and the like, is clinically used for treating symptoms such as blood deficiency sallow, limb numbness, rheumatalgia and the like, is a core raw material of Chinese patent medicines such as black-bone chicken white phoenix pills, spatholobus stem paste and the like, and is widely used for regulating qi and blood in national medicines. Modern pharmacological researches show that the medicinal materials of suberect spatholobus stem mainly comprise flavonoid components (such as catechin and epicatechin), and the content of the flavonoid components directly determines the clinical curative effect of suberect spatholobus stem decoction pieces, wherein the flavonoid components have the activities of resisting oxidation, resisting osteoporosis, improving microcirculation and the like. The quality evaluation of the traditional Chinese medicine and the modern pharmacopoeia on the spatholobus stem is mainly based on subjective descriptions such as 'the circle number of the tangent plane reddish brown layer is most good', 'the surface reddish brown or blackish brown and the excellent with longitudinal grooves', and the like, and the lack of quantitative standards leads to large difference of judging results of different identifiers and uneven quality of market decoction pieces. The existing research on chemical component separation, pharmacological activity verification and DNA bar code identification of the multi-focus caulis spatholobi at home and abroad does not systematically explore the quantitative association of appearance characters such as circle number, color, diameter and the like with active components such as catechin, epicatechin and the like, and the internal quality cannot be rapidly predicted through appearance. The current internal quality detection of spatholobus stem mainly depends on large-scale instruments such as High Performance Liquid Chromatography (HPLC), and the like, requires complex sample pretreatment, has long detection period, and is not suitable for rapid quality screening in basic-level pharmacy and medicinal material markets. The excellent quality is a core theory of traditional quality evaluation of traditional Chinese medicines, and has been verified in medicinal materials such as salvia miltiorrhiza, radix scrophulariae and the like. In conclusion, the quality of the caulis spatholobi is evaluated through the appearance characters, the effective components, the yield and other multidimensional degrees of the caulis spatholobi, the scientificity of the "differentiation theory quality" in the identification of the caulis spatholobi decoction pieces is clarified, and a theoretical basis is provided for constructing an evaluation system for rapid nondestructive identification of the quality of the caulis spatholobi. Disclosure of Invention Aiming at the problems of strong subjectivity, unknown correlation between characters and internal quality and complex detection method of the prior spatholobus stem decoction piece quality evaluation, the invention provides a spatholobus stem quality evaluation method based on dialectical theory The invention aims to utilize principal component analysis to carry out joint analysis on the appearance shape index, the effective components and the yield of the spatholobus stem to construct a multidimensional evaluation model, rapidly predicts the content of the effective components of the spatholobus stem through the appearance property index of the spatholobus stem, realizes the precise evaluation of the quality of the spatholobus stem, and provides a theoretical basis for constructing an evaluation system for rapidly and nondestructively identifying the quality of the spatholobus stem. In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a spatholobus stem decoction piece quality evaluation method based on 'excellent shape and high quality' is characterized by comprising the following steps: 1) Obtaining 8 index data of spatholobus stem Obtaining index data of the suberect spatholobus stem decoction pieces, and o