CN116990420A - Feature-map-based honey bran fructus aurantii comprehensive quality evaluation method - Google Patents
Feature-map-based honey bran fructus aurantii comprehensive quality evaluation method Download PDFInfo
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
Abstract
The invention discloses a honey bran fructus aurantii comprehensive quality evaluation method based on characteristic patterns, which takes honey bran fructus aurantii in different producing areas as a research object, takes moisture, total ash content, alcohol-soluble extract, naringin, neohesperidin, nobiletin, chrysoidine and pattern similarity as indexes, adopts a principal component analysis method in combination with a TOPSIS method to comprehensively evaluate the quality of the honey bran fructus aurantii in different producing areas, carries out characteristic quality index screening through multiple linear regression analysis, finally searches for the characteristic index of the quality of the honey bran fructus aurantii decoction pieces, wherein the influence of the alcohol-soluble extract, neohesperidin and characteristic pattern similarity on the quality of the honey bran fructus aurantii decoction pieces is the greatest, further constructs a honey bran fructus aurantii comprehensive quality evaluation system, is favorable for updating and improving the detection standard of the honey bran fructus aurantii, and can promote sustainable healthy development of traditional Chinese medicine processing decoction pieces.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine quality control, in particular to a honey bran fructus aurantii comprehensive quality evaluation method based on characteristic patterns.
Background
Fructus Aurantii is dry immature fruit of Citrus aurantium L. And its cultivar, mainly produced in Sichuan, jiangxi and Zhejiang, and also distributed in Hubei, hunan and Chongqing, and is commonly used for regulating qi stagnation in chest and hypochondrium, distention and pain, indigestion, phlegm retention, internal stagnation, etc. The honey refined flavor is sweet and neutral, can alleviate pungent and dry nature of the bitter orange, and also enhance the curative effect of invigorating spleen and promoting qi. Under the action of high temperature and high pressure, refined honey can quickly and uniformly permeate into the fructus aurantii, and plays a certain role in protecting the active ingredients of flavone and alkaloid while blending the whole fructus aurantii, so that the drying effect is better.
Along with the progress of modern traditional Chinese medicine analysis means, the quality control method of the fructus aurantii medicinal material mainly comprises an HPLC method, a multi-index content measurement method and a fingerprint spectrum and content measurement combination method, and the method has the advantages of high sensitivity and good repeatability, can provide quantitative data for controlling the fructus aurantii medicinal material, but has the problems that a single index cannot reflect the integral characteristics of the medicinal material, the multi-index content measurement depends on various reference substances, and certain index components cannot reflect the medicinal effect.
For example, chinese patent publication No. CN113030325A provides a method for constructing characteristic spectrum of fructus Aurantii and bran-parched fructus Aurantii and a method for identifying the same. The identification method comprises the following steps: preparing a sample solution to be tested: taking a sample to be detected, adding an extraction solvent for extraction, and preparing a sample solution to be detected; and (3) detection: detecting the sample solution to be detected by using an ultra-high performance liquid chromatography, and comparing the detected spectrum with the characteristic spectrum of the bitter orange constructed by the construction method or the characteristic spectrum of the bran-fried bitter orange constructed by the construction method; the mobile phase A adopted by the ultra-high performance liquid chromatography is acetonitrile, the mobile phase B is phosphoric acid aqueous solution with the volume concentration of 0.03-0.07%, and the elution mode is gradient elution. The characteristic spectrum construction method of the bitter orange and the bran-fried bitter orange belongs to 11 common peaks of the bitter orange and the bran-fried bitter orange, and simultaneously 8 chemical components (including flavonoid glycosides and fat-soluble components) are identified and measured in actual use.
In the above patent, only the characteristic spectrum of the bitter orange is constructed, the construction of the characteristic spectrum of the honey bran bitter orange and the evaluation method of the comprehensive quality are lacked, and the screening of the characteristic quality index of the bitter orange is not accurate enough, so that the comprehensive quality evaluation system of the honey bran bitter orange cannot be comprehensively and accurately constructed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for screening characteristic quality indexes by taking the similarity of alcohol extract, neohesperidin and characteristic patterns as characteristic indexes and adopting a principal component analysis method and a TOPSIS method and adopting a multiple linear regression analysis, and the constructed comprehensive quality evaluation system is beneficial to updating the detection standard of honey bran fructus aurantii and promoting the sustainable healthy development of traditional Chinese medicine processed decoction pieces.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a honey bran fructus aurantii comprehensive quality evaluation method based on characteristic patterns comprises the following steps:
step 1, weighing a certain amount of refined honey, adding water, uniformly stirring, pouring the mixture into wheat bran, uniformly stirring, setting a temperature of 50 ℃ by using an oven, drying for 106 minutes until the mixture is not sticky, taking out the mixture, and rubbing the mixture to obtain the honey bran, wherein the water refined honey ratio is 42% and the refined honey wheat bran ratio is 28%; uniformly dispersing honey bran in a hot pot, adding fructus Aurantii after smoking, parching until the color of fructus Aurantii is deepened to yellowish, rapidly taking out of the pot, cooling, and sieving to remove excessive honey bran to obtain coarse powder of honey bran fructus Aurantii;
step 2, weighing 0.5g of coarse powder of honey bran fructus aurantii, placing the coarse powder into a conical flask with a plug, adding 50mL of methanol, heating and refluxing for 1.5 hours, filtering, placing filtrate into a volumetric flask with 50mL, and obtaining a sample solution after constant volume; quantitatively weighing naringin, neohesperidin, nobiletin and exocarpium Citri rubrum reference substances, respectively placing into 25mL volumetric flasks to prepare mother liquor, then sucking equal amount of mother liquor from each volumetric flask, placing into the same 50mL volumetric flask, adding methanol to constant volume to scale, and obtaining mixed reference substance solution;
step 3, sucking a sufficient amount of mixed reference substance solution, performing a precision test according to set chromatographic conditions, sucking a sufficient amount of sample solution, performing a stability test according to set chromatographic conditions, performing a repeatability test according to set chromatographic conditions, and establishing a honey bran fructus aurantii comprehensive reference characteristic map;
step 4, constructing a multi-index decision matrix by the established honey bran fructus aurantii comprehensive comparison characteristic map, carrying out standardization processing on the original data in the decision matrix to obtain a dimensionless decision matrix, then obtaining the characteristic value and variance of the dimensionless decision matrix through principal component analysis, and determining the optimal principal component number N in the multi-index by taking the variance contribution rate of the characteristic value lambda > 1 as a judging condition;
step 5, dividing the main component load of each index variable by the square root of the initial characteristic value of the load according to the determined optimal main component number N to obtain a coefficient corresponding to each index in the N main components, namely a characteristic vector, and constructing a function expression of the N main components by taking the characteristic vector of the dimensionless decision matrix of each index as a weight;
step 6, calculating the sum of products of the coefficients corresponding to each index in the N main components obtained in the step 5 and the corresponding variance contribution rate obtained in the step 4, and taking the ratio of the sum of products to the total contribution rate of the N main components as a weight to obtain a main component comprehensive model M;
step 7, according to the obtained principal component comprehensive model M, normalizing each index, calculating the weight occupied by each index, further constructing a normalized weighted decision matrix, and calculating the optimal vector A of each evaluation object + And the worst vector A - By calculating A of a weighted decision matrix + And A - Calculating a positive ideal solution distance D for each evaluation object using a Euclidean distance calculation formula i + Sum of negative ideal solution distance D i - ；
Step 8, according to the calculated ideal solution distance D i + Sum of negative ideal solution distance D i - Applying formula C i ＝D i - /(D i + +D i - ) Computing relative proximity C of optimal solution i Relative proximity C i The larger indicates the better the quality of the evaluation object.
Specifically, the chromatographic conditions in step 3 are:
performing gradient elution on a chromatographic column Diamond C18 by taking methanol-0.1% phosphoric acid aqueous solution as a mobile phase, and detecting the wavelength to 320nm; column temperature is 30 ℃; the sample injection amount was 10. Mu.L.
Specifically, the test procedure of the precision test in the step 3 is as follows:
sucking a sufficient amount of mixed reference substance solution, repeatedly sampling for 6 times according to a set chromatographic condition, comparing the obtained chromatogram with a traditional Chinese medicine chromatographic fingerprint, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, calculating the area RSD of each peak, and verifying the precision of a test instrument;
the test process of the stability test is as follows:
absorbing enough sample solution, respectively measuring at 0h, 2h, 4h, 8h, 12h and 24h according to set chromatographic conditions, comparing the obtained chromatogram with traditional Chinese medicine chromatographic fingerprints, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, calculating the areas RSD of the peaks, and verifying the stability of the sample solution;
the test process of the repeatability test is as follows:
taking enough honey bran fructus aurantii coarse powder prepared according to the method in the step 1, dividing the honey bran fructus aurantii coarse powder into 6 parts, preparing a sample solution according to the method in the step 2, measuring according to set chromatographic conditions, comparing the obtained chromatogram with a traditional Chinese medicine chromatographic fingerprint, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, calculating the areas RSD of the peaks, and verifying the repeatability of the methods in the step 1 and the step 2.
Specifically, in the step 3, a honey bran fructus aurantii characteristic spectrum is established, and the process is as follows:
taking 18 batches of fructus aurantii samples, marking the samples as S1-S18, preparing coarse powder of the honey bran fructus aurantii according to the method in the step 1, preparing a solution of a test sample according to the method in the step 2, measuring according to set chromatographic conditions, comparing and analyzing the obtained chromatogram with a traditional Chinese medicine chromatographic fingerprint, taking the S1 as a reference chromatogram, adopting an average method, and adopting a time window with the width of 0.1min to match by using a multipoint correction mark peak, so as to establish a honey bran fructus aurantii comprehensive comparison characteristic chromatogram.
Specifically, in step 4, a multi-index decision matrix is constructed from the established comprehensive control characteristic spectrum of the honey bran fructus aurantii, wherein the multi-index decision matrix comprises moisture, total ash, naringin, neohesperidin, chrysoidine, nobiletin, alcohol-soluble extract and similarity of characteristic spectrum, and the moisture, total ash and alcohol-soluble extract are determined by the following method:
moisture content: taking quantitative honey bran fructus aurantii coarse powder, adding 200mL of toluene into a containing bottle, slowly heating, adjusting the temperature when the toluene starts boiling, distilling 2 drops per second, flushing the interior of a condensing tube with toluene when the water is completely distilled, pushing the toluene attached to the tube wall by a long brush saturated with toluene, continuously distilling for 5 minutes, cooling to room temperature, completely separating the water from the toluene, reading the water quantity, and calculating the water content in the honey bran fructus aurantii;
total ash: putting quantitative honey bran fructus aurantii coarse powder into a crucible which burns to constant weight, gradually heating the honey bran fructus aurantii coarse powder to complete carbonization, gradually increasing the temperature to 550 ℃, completely ashing the honey bran fructus aurantii coarse powder to constant weight, and calculating the total ash content in the honey bran fructus aurantii according to the weight of residues;
alcohol-soluble extract: putting quantitative honey bran fructus aurantii coarse powder into a conical flask, adding 70% ethanol for 100mL, weighing after sealing, standing for 1 hour, connecting a reflux condenser tube, heating to boiling, keeping micro boiling for 1 hour, cooling, taking down the conical flask sealing, weighing again, supplementing the weight of loss, filtering, measuring 25mL of filtrate, putting the filtrate into an evaporation dish dried to constant weight, evaporating in a water bath, drying for 3 hours at 105 ℃, cooling for 30 minutes, rapidly weighing, and calculating the content of alcohol-soluble extract of the honey bran fructus aurantii.
In summary, the invention also constructs a comprehensive quality evaluation system through screening the characteristic indexes, which is helpful for realizing the rapid detection of the comprehensive quality of the honey bran fructus aurantii, and the specific construction process comprises the following steps: and performing multiple linear regression analysis by taking the measured value of the honey bran fructus aurantii index as an independent variable and the relative proximity as a dependent variable, screening out characteristic indexes according to the obtained fitting equation, and constructing a honey bran fructus aurantii comprehensive quality evaluation system by using the screened characteristic indexes for subsequent comprehensive quality evaluation of the honey bran fructus aurantii.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a method for evaluating the comprehensive quality of honey bran fructus aurantii, which can organically combine general inspection indexes such as water content, total ash content, alcohol-soluble extract and the like of honey bran fructus aurantii with intrinsic content indexes such as naringin, nobiletin, neohesperidin and the like and characteristic maps simultaneously. Meanwhile, the traditional TOPSIS method is improved based on the principal component analysis method, the principal component analysis method is adopted for assignment, the TOPSIS method is adopted for comprehensive evaluation and optimal batch screening, and scientific basis and reference are provided for comprehensively and objectively evaluating the comprehensive quality conditions of honey bran fructus aurantii in different production places and the purchase of raw materials and the stability of the production quality of honey bran fructus aurantii decoction pieces in actual production.
2. According to the comprehensive quality evaluation method for the honey bran fructus aurantii, a drying method is adopted for preparing the honey bran fructus aurantii, the temperature is relatively low, maillard reaction is not generated, and the generation of components such as a Maillard reaction product 5-hydroxymethylfurfural and the like is not generated, so that the evaluation result is more reliable.
3. According to the honey bran fructus aurantii comprehensive quality evaluation method, honey bran fructus aurantii in different producing areas is taken as a research object, moisture, total ash, alcohol-soluble extract, naringin, neohesperidin, nobiletin, chrysoidine and characteristic spectrum similarity are taken as indexes, a principal component analysis method is combined with a TOPSIS method to comprehensively evaluate the quality of the honey bran fructus aurantii in different producing areas, characteristic quality index screening is carried out through multiple linear regression analysis, the alcohol-soluble extract, neohesperidin and characteristic spectrum similarity are finally screened out to be the honey bran fructus aurantii quality characteristic index, and the constructed comprehensive quality evaluation system is favorable for updating of honey bran fructus aurantii detection standards and promotes sustainable healthy development of traditional Chinese medicine processing decoction pieces.
Drawings
FIG. 1 is a superposition diagram of 18 batches of honey bran fructus aurantii in the honey bran fructus aurantii comprehensive quality evaluation method based on characteristic spectrum;
FIG. 2 is a comprehensive comparison characteristic spectrum of 18 batches of honey bran fructus aurantii in the characteristic spectrum-based honey bran fructus aurantii comprehensive quality evaluation method;
fig. 3 is a chromatogram of a mixed reference substance in the honey bran fructus aurantii comprehensive quality evaluation method based on characteristic patterns.
Detailed Description
The invention is described in detail below with reference to the attached drawings and examples:
the following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Reagents and apparatus used in the following examples
Instrument:
111B traditional Chinese medicine pulverizer (Rui An Shi Yongli pharmaceutical machinery Co., ltd.), GZX-9076MBE electrothermal blast drying oven (Shanghai Bo Xie medical equipment Co., ltd.), HH-6 digital display constant temperature water bath (national electric Co., ltd.), waterse2695 high performance liquid chromatograph (U.S. Waters Co.), BX53+ DP73 type positive microscope (Japan Olympus Co.), SHZ (III) circulating water type vacuum pump (incorporated by reference of the Ministry of China, limited of the instruments), KQ-500E ultrasonic cleaner (incorporated by reference of the ultrasound instruments of Kunshan, inc.), resistance furnace (Shanghai Bo Hi-Kun-shan, inc. medical equipment factory), one ten thousandth balance (OHAUS Co., ltd.), silica gel thin layer plate (Qingdao sea wave silica gel desiccant Co., ltd.).
Reagent:
naringin (purity not less than 98%, lot number: CHB 201202), neohesperidin (purity not less than 98%, lot number: CHB 201120), all purchased from Chengdu Cromax Biotechnology Co. The methanol and the phosphoric acid are chromatographic purity, the methanol and ethanol reagent is analytical purity, and the water is purified water.
The 18 batches of fructus Aurantii were purchased from decoction pieces factory in the river, and identified as dried immature fruits of Citrus aurantium L. And its cultivar of Rutaceae by professor Qianfeng of the university of Chinese medicine processing discipline in the river, and the origin information is shown in Table 1 below.
Table 1, 18 batches of fructus Aurantii producing areas
。
Example 1
The implementation provides a honey bran fructus aurantii comprehensive quality evaluation method based on characteristic patterns, which comprises the following steps:
step 1, weighing a certain amount of refined honey, adding water, uniformly stirring, pouring the mixture into wheat bran, uniformly stirring, setting a temperature of 50 ℃ by using an oven, drying for 106 minutes until the mixture is not sticky, taking out the mixture, and rubbing the mixture to obtain the honey bran, wherein the water refined honey ratio is 42% and the refined honey wheat bran ratio is 28%; uniformly dispersing honey bran in a hot pot, adding fructus Aurantii after smoking, parching until the color of fructus Aurantii is deepened to yellowish, rapidly taking out of the pot, cooling, and sieving to remove excessive honey bran to obtain coarse powder of honey bran fructus Aurantii;
step 2, weighing 0.5g of coarse powder of honey bran fructus aurantii, placing the coarse powder into a conical flask with a plug, adding 50mL of methanol, heating and refluxing for 1.5 hours, filtering, placing filtrate into a volumetric flask with 50mL, and obtaining a sample solution after constant volume; quantitatively weighing naringin, neohesperidin, nobiletin and exocarpium Citri rubrum reference substances, respectively placing into 25mL volumetric flasks to prepare mother liquor, then sucking equal amount of mother liquor from each volumetric flask, placing into the same 50mL volumetric flask, adding methanol to constant volume to scale, and obtaining mixed reference substance solution;
and 3, sucking a sufficient amount of mixed reference substance solution, performing a precision test according to set chromatographic conditions, sucking a sufficient amount of sample solution, performing a stability test according to set chromatographic conditions, performing a repeatability test according to set chromatographic conditions, and establishing a honey bran bitter orange characteristic spectrum.
Specifically, the chromatographic conditions in step 3 are:
performing gradient elution on a chromatographic column Diamond C18 by taking methanol-0.1% phosphoric acid aqueous solution as a mobile phase, and detecting the wavelength to 320nm; column temperature is 30 ℃; the sample injection amount was 10. Mu.L.
Specifically, the test procedure of the precision test in the step 3 is as follows:
sucking a sufficient amount of mixed reference substance solution, repeatedly sampling for 6 times according to set chromatographic conditions, comparing the obtained chromatogram with traditional Chinese medicine chromatographic fingerprints, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, and calculating the area RSD of each peak, wherein the result is shown in the following table 2;
TABLE 2 precision test
。
The peak areas RSD calculated by the precision test are respectively 0.84%, 0.93%, 0.47% and 0.85%, which shows that the instrument precision is good.
The test process of the stability test is as follows:
sucking enough sample solution, measuring at 0h, 2h, 4h, 8h, 12h and 24h according to set chromatographic conditions, comparing the obtained chromatogram with traditional Chinese medicine chromatographic fingerprint, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, and calculating the area RSD of each peak, wherein the result is shown in the following table 3;
TABLE 3 stability test
。
The peak areas RSD calculated in the stability test were 1.09%, 1.11%, 0.37% and 0.96%, respectively, indicating that the test sample solution was stable well within 24 h.
The test process of the repeatability test is as follows:
taking enough honey bran fructus aurantii coarse powder prepared in the step 1, dividing the honey bran fructus aurantii coarse powder into 6 parts, preparing a sample solution according to the method in the step 2, measuring according to set chromatographic conditions, comparing the obtained chromatogram with a traditional Chinese medicine chromatographic fingerprint, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, and calculating the areas RSD of the peaks, wherein the results are shown in the following table 4;
table 4, repeatability test
。
The peak areas RSD calculated in the repeatability test were 0.54%, 0.42%, 0.46%, and 0.36%, respectively, indicating that the repeatability of the methods described in step 1 and step 2 of the present invention is good.
Specifically, in the step 3, a honey bran fructus aurantii characteristic spectrum is established, and the process is as follows:
taking 18 batches of fructus aurantii samples, recording as S1-S18, preparing coarse powder of honey bran fructus aurantii according to the method in the step 1, preparing solution to be tested (MFZQ 01-MFZQ 18) according to the method in the step 2, measuring according to set chromatographic conditions, introducing the obtained chromatograms into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system software (2012 130723) version, analyzing, obtaining 18 batches of honey bran fructus aurantii superposition graphs, taking S1 as a reference map, adopting an average method, and using a time window width of 0.1min, and performing multi-point correction mark peak matching to obtain 18 batches of honey bran fructus aurantii comprehensive comparison characteristic graphs, wherein the MFZQR represents the comprehensive comparison characteristic graphs obtained from the 18 batches of honey bran fructus aurantii superposition graphs, and further obtaining 18 batches of honey bran fructus aurantii characteristic graph similarity as shown in the following table 5;
table 5, 18 batches of honey bran fructus Aurantii feature map similarity
。
The common peaks of 18 batches of honey bran fructus Aurantii are identified, and 4 common peaks are identified by comparing the color spectrograms of the mixture control as shown in figure 3, wherein the No. 7 peak is naringin, the No. 9 peak is neohesperidin, the No. 12 peak is nobiletin, and the No. 13 peak is rubeosin.
Further, the content of naringin, neohesperidin, nobiletin and chrysoidine in 18 batches of honey bran fructus aurantii is measured, and the measurement results are shown in the following table 6;
TABLE 6 determination of content
。
Based on the above technical scheme, the embodiment further provides a comprehensive quality evaluation method of the honey bran fructus aurantii, which is based on the honey bran fructus aurantii characteristic spectrum established by 18 batches of fructus aurantii samples, and is used for analyzing the comprehensive quality of 18 batches of honey bran fructus aurantii, and specifically comprises the following steps:
step 4, 18 batches of honey bran fructus aurantii are taken as research objects, SPSS21.0 statistical analysis software is utilized to analyze the comprehensive quality of 18 batches of honey bran fructus aurantii, in order to eliminate adverse effects possibly caused by different dimensions, the original data in the constructed decision matrix are standardized to obtain a dimensionless decision matrix, then the eigenvalue and variance of the dimensionless decision matrix are obtained through principal component analysis, the optimal principal component number N in multiple indexes is determined by taking the variance contribution ratio of the eigenvalue lambda > 1 as a judgment condition, and the eigenvalue and variance of the decision matrix obtained through principal component analysis are shown in the following table 7;
tables 7, 18 sets of eigenvalues and variances of the honey bran fructus Aurantii decision matrix
。
As can be seen from table 7, the variance contribution ratio of the characteristic values of the first 3 main components is greater than 1, the variance contribution ratios are 47.3481%, 21.4895 and 14.5759%, respectively, and the cumulative contribution ratio reaches 83.4134%, so that the original index information can be basically reflected, and therefore the initial 8 quality indexes (moisture, total ash, naringin, neohesperidin, chrysoidine, nobiletin, alcohol-soluble extract and characteristic spectrum similarity) are reduced to 3 main components which are not related to each other, and in this embodiment, the 3 main components which are not related to each other are alcohol-soluble extract, neohesperidin and characteristic spectrum similarity.
Step 5, dividing the principal component load of each index variable by the square root of the initial characteristic value of the load according to the determined optimal principal component number N=3 to obtain a coefficient corresponding to each index in the 3 principal components, namely a characteristic vector, and constructing a function expression of the 3 principal components by taking the characteristic vector of the dimensionless decision matrix of each index as a weight:
；
wherein Z is 1 、Z 2 、Z 3 Respectively represent 3 main components which are not related to each other, C 1 、C 2 、C 3 、C 4 、C 5 、C 6 、C 7 、C 8 Respectively representing the initial 8 quality indexes;
step 6, calculating the sum of products of the coefficients corresponding to each index in the 3 main components obtained in the step 5 and the corresponding variance contribution rates obtained in the step 4, and taking the ratio of the sum of products to the total contribution rate of the 3 main components as a weight to obtain a main component comprehensive model M:
；
step 7, according to the obtained main component comprehensive model M, normalizing each index, and calculating the weight W occupied by each index j J=1, 2,..8, the results are shown in table 8 below, and a normalized weighted decision matrix z= [ a ] is constructed ij ] m×n In which A ij =W j D ij M is the evaluation object (18 batches of honey bran fructus Aurantii), n is the evaluation index,D ij representing the specific gravity of the ith evaluation object under the jth evaluation index, and calculating the optimal vector A of each evaluation object + And the worst vector A - ，A + ＝(，/>，…，/>)，A - ＝(/>，/>，…，/>) The results are shown in Table 9 below, by calculating A of the weighted decision matrix + And A - Calculating a positive ideal solution distance D for each evaluation object using a Euclidean distance calculation formula i + Sum of negative ideal solution distance D i - ：
；
，(i=1，2，…，n)；
Wherein, the liquid crystal display device comprises a liquid crystal display device,＝max(A 1j ， A 2j ，…， A mj )，/>＝min(A 1j ，A 2j ，…，A mj )；
table 8, weights of the indices
。
Table 9, weighting matrix, optimal vector and worst vector
。
Step 8, as shown in the following Table 10, according to the calculated positive ideal solution distance D i + Sum of negative ideal solution distance D i - Applying formula C i ＝D i - /(D i + +D i - ) Computing relative proximity C of optimal solution i Relative proximity C i The larger indicates the better the quality of the evaluation object. In this embodiment, the relative proximity C of each batch i Scores of 0.2406-0.1620, C of batch MFZQ14 (Hunan Yiyang) samples i Scoring highest, scoring best object; sample MFZQ11 (Sichuan south China) i The score was lowest, and the worst object was evaluated.
Table 10, 18 batch honey bran fructus Aurantii comprehensive evaluation results
。
Specifically, in step 4, a multi-index decision matrix is constructed from the established characteristic spectrum of the honey bran fructus aurantii, wherein the multi-index comprises moisture, total ash, naringin, neohesperidin, chrysoidine, nobiletin, alcohol-soluble extract and similarity of characteristic spectrum, and the moisture, total ash and alcohol-soluble extract are determined by the following method:
moisture content: taking quantitative honey bran fructus aurantii coarse powder, adding 200mL of toluene into a containing bottle, slowly heating, adjusting the temperature when the toluene starts boiling, distilling 2 drops per second, flushing the interior of a condensing tube with toluene when the water is completely distilled, pushing the toluene attached to the tube wall by a long brush saturated with toluene, continuously distilling for 5 minutes, cooling to room temperature, completely separating the water from the toluene, reading the water quantity, and calculating the water content in the honey bran fructus aurantii;
total ash: putting quantitative honey bran fructus aurantii coarse powder into a crucible which burns to constant weight, gradually heating the honey bran fructus aurantii coarse powder to complete carbonization, gradually increasing the temperature to 550 ℃, completely ashing the honey bran fructus aurantii coarse powder to constant weight, and calculating the total ash content in the honey bran fructus aurantii according to the weight of residues;
alcohol-soluble extract: putting quantitative honey bran fructus aurantii coarse powder into a conical flask, adding 70% ethanol for 100mL, weighing after sealing, standing for 1 hour, connecting a reflux condenser tube, heating to boiling, keeping micro boiling for 1 hour, cooling, taking down the conical flask sealing, weighing again, supplementing the weight of loss, filtering, measuring 25mL of filtrate, putting the filtrate into an evaporation dish dried to constant weight, evaporating in a water bath, drying for 3 hours at 105 ℃, cooling for 30 minutes, rapidly weighing, and calculating the content of alcohol-soluble extract of the honey bran fructus aurantii.
In summary, the invention also constructs a comprehensive quality evaluation system through screening the characteristic indexes, which is helpful for realizing the rapid detection of the comprehensive quality of the honey bran fructus aurantii, and the specific construction process comprises the following steps: multiplex linear regression analysis was performed with the honey bran fructus Aurantii index measurements given in Table 9 as independent variables and relative proximity as dependent variables in Table 10 to obtain the fitting equation:
（R 2 =0.9963，P＜0.001）
wherein x is 1 ，x 2 ，x 3 The similarity of the alcohol-soluble extract, the neohesperidin and the characteristic spectrum respectively shows that the similarity of the alcohol-soluble extract, the neohesperidin and the characteristic spectrum is the characteristic index of 18 batches of honey bran fructus aurantii, and the characteristic index is used for constructing a honey bran fructus aurantii comprehensive quality evaluation system, so that the method can be used for subsequent rapid comprehensive quality evaluation of the honey bran fructus aurantii.
The above description is only of the preferred embodiment of the present invention, and is not intended to limit the structure of the present invention in any way. Any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention fall within the technical scope of the present invention.
Claims (6)
1. A honey bran fructus aurantii comprehensive quality evaluation method based on characteristic patterns is characterized by comprising the following steps:
step 1, weighing a certain amount of refined honey, adding water, uniformly stirring, pouring the mixture into wheat bran, uniformly stirring, setting a temperature of 50 ℃ by using an oven, drying for 106 minutes until the mixture is not sticky, taking out the mixture, and rubbing the mixture to obtain the honey bran, wherein the water refined honey ratio is 42% and the refined honey wheat bran ratio is 28%; uniformly dispersing honey bran in a hot pot, adding fructus Aurantii after smoking, parching until the color of fructus Aurantii is deepened to yellowish, rapidly taking out of the pot, cooling, and sieving to remove excessive honey bran to obtain coarse powder of honey bran fructus Aurantii;
step 2, weighing 0.5g of coarse powder of honey bran fructus aurantii, placing the coarse powder into a conical flask with a plug, adding 50mL of methanol, heating and refluxing for 1.5 hours, filtering, placing filtrate into a volumetric flask with 50mL, and obtaining a sample solution after constant volume; quantitatively weighing naringin, neohesperidin, nobiletin and exocarpium Citri rubrum reference substances, respectively placing into 25mL volumetric flasks to prepare mother liquor, then sucking equal amount of mother liquor from each volumetric flask, placing into the same 50mL volumetric flask, adding methanol to constant volume to scale, and obtaining mixed reference substance solution;
step 3, sucking a sufficient amount of mixed reference substance solution, performing a precision test according to set chromatographic conditions, sucking a sufficient amount of sample solution, performing a stability test according to set chromatographic conditions, performing a repeatability test according to set chromatographic conditions, and establishing a honey bran fructus aurantii comprehensive reference characteristic map;
step 4, constructing a multi-index decision matrix by the established honey bran fructus aurantii comprehensive comparison characteristic map, carrying out standardization processing on the original data in the decision matrix to obtain a dimensionless decision matrix, then obtaining the characteristic value and variance of the dimensionless decision matrix through principal component analysis, and determining the optimal principal component number N in the multi-index by taking the variance contribution rate of the characteristic value lambda > 1 as a judging condition;
step 5, dividing the main component load of each index variable by the square root of the initial characteristic value of the load according to the determined optimal main component number N to obtain a coefficient corresponding to each index in the N main components, namely a characteristic vector, and constructing a function expression of the N main components by taking the characteristic vector of the dimensionless decision matrix of each index as a weight;
step 6, calculating the sum of products of the coefficients corresponding to each index in the N main components obtained in the step 5 and the corresponding variance contribution rate obtained in the step 4, and taking the ratio of the sum of products to the total contribution rate of the N main components as a weight to obtain a main component comprehensive model M;
step 7, according to the obtained principal component comprehensive model M, normalizing each index, calculating the weight occupied by each index, further constructing a normalized weighted decision matrix, and calculating the optimal vector A of each evaluation object + And the worst vector A - By calculating A of a weighted decision matrix + And A - Calculating a positive ideal solution distance D for each evaluation object using a Euclidean distance calculation formula i + Sum of negative ideal solution distance D i - ；
Step 8, according to the calculated ideal solution distance D i + Sum of negative ideal solution distance D i - Applying formula C i ＝D i - /(D i + +D i - ) Computing relative proximity C of optimal solution i Relative proximity C i The larger indicates the better the quality of the evaluation object.
2. The method for evaluating the comprehensive quality of honey bran fructus aurantii based on characteristic spectrum as claimed in claim 1, wherein the chromatographic condition in the step 3 is as follows:
performing gradient elution on a chromatographic column Diamond C18 by taking methanol-0.1% phosphoric acid aqueous solution as a mobile phase, and detecting the wavelength to 320nm; column temperature is 30 ℃; the sample injection amount was 10. Mu.L.
3. The method for evaluating the comprehensive quality of honey bran fructus aurantii based on characteristic spectrum as claimed in claim 1, wherein the test process of the precision test in the step 3 is as follows:
sucking a sufficient amount of mixed reference substance solution, repeatedly sampling for 6 times according to a set chromatographic condition, comparing the obtained chromatogram with a traditional Chinese medicine chromatographic fingerprint, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, calculating the area RSD of each peak, and verifying the precision of a test instrument;
the test process of the stability test is as follows:
absorbing enough sample solution, respectively measuring at 0h, 2h, 4h, 8h, 12h and 24h according to set chromatographic conditions, comparing the obtained chromatogram with traditional Chinese medicine chromatographic fingerprints, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, calculating the areas RSD of the peaks, and verifying the stability of the sample solution;
the test process of the repeatability test is as follows:
taking enough honey bran fructus aurantii coarse powder prepared according to the method in the step 1, dividing the honey bran fructus aurantii coarse powder into 6 parts, preparing a sample solution according to the method in the step 2, measuring according to set chromatographic conditions, comparing the obtained chromatogram with a traditional Chinese medicine chromatographic fingerprint, finding out peaks corresponding to naringin, neohesperidin, nobiletin and chrysoidine in the chromatogram, calculating the areas RSD of the peaks, and verifying the repeatability of the methods in the step 1 and the step 2.
4. The method for evaluating the comprehensive quality of the honey bran fructus aurantii based on the characteristic spectrum of claim 1, which is characterized by comprising the following specific processes of:
taking 18 batches of fructus aurantii samples, marking the samples as S1-S18, preparing coarse powder of honey bran fructus aurantii according to the method in the step 1, preparing a sample solution according to the method in the step 2, measuring according to set chromatographic conditions, comparing the obtained chromatogram with a traditional Chinese medicine chromatographic fingerprint, analyzing by taking the S1 as a reference chromatogram, adopting an average method, enabling the time window width to be 0.1min, and utilizing multi-point correction mark peak matching to establish a comprehensive comparison characteristic chromatogram of 18 batches of honey bran fructus aurantii.
5. The method for evaluating the comprehensive quality of the honey bran fructus aurantii based on the characteristic spectrum according to claim 1, wherein in the step 4, a multi-index decision matrix is constructed by the established comprehensive comparison characteristic spectrum of the honey bran fructus aurantii, and the multi-index comprises moisture, total ash, naringin, neohesperidin, chrysoidine, nobiletin, alcohol-soluble extract and characteristic spectrum similarity, wherein the moisture, total ash and alcohol-soluble extract are determined by the following methods:
moisture content: taking quantitative honey bran fructus aurantii coarse powder, adding 200mL of toluene into a containing bottle, slowly heating, adjusting the temperature when the toluene starts boiling, distilling 2 drops per second, flushing the interior of a condensing tube with toluene when the water is completely distilled, pushing the toluene attached to the tube wall by a long brush saturated with toluene, continuously distilling for 5 minutes, cooling to room temperature, completely separating the water from the toluene, reading the water quantity, and calculating the water content in the honey bran fructus aurantii;
total ash: putting quantitative honey bran fructus aurantii coarse powder into a crucible which burns to constant weight, gradually heating the honey bran fructus aurantii coarse powder to complete carbonization, gradually increasing the temperature to 550 ℃, completely ashing the honey bran fructus aurantii coarse powder to constant weight, and calculating the total ash content in the honey bran fructus aurantii according to the weight of residues;
alcohol-soluble extract: putting quantitative honey bran fructus aurantii coarse powder into a conical flask, adding 70% ethanol for 100mL, weighing after sealing, standing for 1 hour, connecting a reflux condenser tube, heating to boiling, keeping micro boiling for 1 hour, cooling, taking down the conical flask sealing, weighing again, supplementing the weight of loss, filtering, measuring 25mL of filtrate, putting the filtrate into an evaporation dish dried to constant weight, evaporating in a water bath, drying for 3 hours at 105 ℃, cooling for 30 minutes, rapidly weighing, and calculating the content of alcohol-soluble extract of the honey bran fructus aurantii.
6. The method for evaluating the comprehensive quality of honey bran fructus aurantii based on characteristic spectrum as claimed in claim 1, further comprising screening characteristic indexes to construct a comprehensive quality evaluation system, wherein the method comprises the following steps: and performing multiple linear regression analysis by taking the measured value of the honey bran fructus aurantii index as an independent variable and the relative proximity as a dependent variable, screening out characteristic indexes according to the obtained fitting equation, and constructing a honey bran fructus aurantii comprehensive quality evaluation system by using the screened characteristic indexes for subsequent comprehensive quality evaluation of the honey bran fructus aurantii.
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