CN113866298B - Quality evaluation method for distinguishing green tangerine peel from vinegar green tangerine peel - Google Patents
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Abstract
The invention belongs to the field of material analysis, and particularly relates to a quality evaluation method for distinguishing green tangerine peel from vinegar green tangerine peel. The evaluation method is realized by the following steps: preparing a sample solution and a reference substance solution, respectively establishing fingerprint patterns of green tangerine orange peel and vinegar green tangerine peel by utilizing high performance liquid chromatography, and carrying out green tangerine peel and vinegar green tangerine peel distinguishing verification through the fingerprint patterns. The invention systematically researches the change of chemical components before and after vinegar processing of green tangerine peel, screens the quality markers of the vinegar green tangerine peel, and provides scientific basis for formulating more reasonable vinegar green tangerine peel quantity standard and further researching the processing principle of the vinegar processed green tangerine peel; the method is stable and reliable, the established fingerprint analysis method can systematically reflect the difference of chemical components of green tangerine peel and vinegar green tangerine peel decoction pieces, and the screened newly added components can be used as quality markers for distinguishing the green tangerine peel and the vinegar green tangerine peel, so that scientific basis is provided for formulating more reasonable vinegar green tangerine peel quantity standards and further researching the processing principle of the vinegar-roasted green tangerine peel.
Description
Technical Field
The invention belongs to the field of material analysis, and particularly relates to a quality evaluation method for distinguishing green tangerine peel from vinegar green tangerine peel.
Background
The pericarpium Citri Reticulatae viride is Citrus reticulata of RutaceaeCitrus reticulataThe pericarp of the dried young fruit or immature fruit of Blanco and its cultivated variety has effects of dispersing stagnated liver qi, removing qi stagnation, and resolving food stagnation, and can be used for treating chest and hypochondrium distending pain, hernia pain,
nodules of breast, acute mastitis, food retention and qi stagnation, abdominal distention and pain [1] . Vinegar green skin was recorded in Song' three-cause-electrode-one disease at the earliest
The "rice vinegar decoction" of the province theory and the "Chinese pharmacopoeia" 2020 edition collect two decoction pieces of green tangerine peel and vinegar green tangerine peel,
however, the quality standards of the two decoction pieces are different except for the appearance characteristics and the content limitation of hesperidin (the content of hesperidin in green tangerine peel is not less than 4.0 percent, the content of hesperidin in vinegar green tangerine peel is not less than 3.0 percent), and no clear vinegar green tangerine peel quantity marker exists, so that the powder of green tangerine peel different processed products or the Chinese patent medicine containing green tangerine peel different processed products with the appearance characteristics being lost cannot be effectively distinguished. Modern researches have found that the green tangerine peel mainly contains active ingredients such as volatile oil (D-limonene), flavonoids (hesperidin), alkaloids (synephrine) and the like, and the contents of the volatile oil, hesperidin and synephrine are reduced after vinegar processing. Wang Yaoli et al have determined the fingerprint patterns of green tangerine peel before and after vinegar processing by HPLC, identified hesperidin, considered that the fingerprint patterns of green tangerine peel before and after vinegar processing and the relative peak area difference are smaller, and can not effectively distinguish the green tangerine peel from the green tangerine peel.
Disclosure of Invention
Aiming at the technical problem that the green tangerine peel and the green tangerine peel cannot be effectively distinguished in the prior art, the invention provides a quality evaluation method for distinguishing the green tangerine peel and the green tangerine peel.
The technical scheme adopted by the invention for achieving the purpose is as follows:
the invention provides a quality evaluation method for distinguishing green tangerine peel from vinegar green tangerine peel, which comprises the following steps:
(1) Preparation of test solution: taking green tangerine peel or vinegar green tangerine peel sample powder, precisely weighing, precisely adding methanol, weighing, performing ultrasonic treatment, cooling, compensating for weight loss, filtering, collecting the subsequent filtrate, and passing through microporous filter membrane to obtain the final product;
(2) Preparation of a control solution: respectively weighing synephrine and hesperidin, precisely weighing, adding methanol to prepare reference substance stock solution, precisely sucking the reference substance stock solution, adding methanol to dilute and fix volume, and preparing mixed reference substance solution;
(3) Respectively establishing fingerprint patterns of green tangerine peel and vinegar green tangerine peel by utilizing high performance liquid chromatography;
(4) And (5) distinguishing and verifying green tangerine peel and vinegar green tangerine peel through a fingerprint spectrogram.
The specific preparation process of the sample solution provided by the invention comprises the following steps: sample powder was weighed approximately 0.20 and g, placed in a 50 mL stoppered conical flask, added with 100% methanol precisely 25mL, stoppered, weighed, sonicated (100 w,40 khz) for 30 min, cooled, made up for weight loss, filtered, and the subsequent filtrate was filtered through a 0.45 μm microfiltration membrane.
The specific preparation process of the reference substance solution provided by the invention comprises the following steps: and respectively weighing a proper amount of synephrine and hesperidin, precisely weighing, adding methanol to prepare reference substance stock solutions containing 1.10 mg synephrine and 0.335 mg hesperidin in each 1 mL, precisely sucking each 1 mL of the reference substance stock solutions, placing the reference substance stock solutions into a 25mL volumetric flask, adding methanol to dilute and fix the volume, and preparing a mixed reference substance solution containing 44.00 mug of synephrine and 13.40 mug of hesperidin in each 1 mL.
Further, the conditions of the high performance liquid chromatography are as follows: chromatographic column: thermo Hypersil GOLD C 18 Chromatographic column (250X 4.6 mm,5 μm); mobile phase: acetonitrile (a) -0.1% phosphoric acid water (B); sample injection volume: 10. mu L; flow rate: 1 mL/min; column temperature: 35. the temperature is lower than the temperature; detection wavelength: 283nm, and performing gradient elution.
Further, the conditions of the gradient elution are as follows: 0-8 min,10% -14% of A; 8-17 min,14% -16% of A; 17-38 min,16% -18% of A; 38-50 min,18% -30% of A; 50-72 min,30% -38% of A; 72-88 min,38% -50% of A; 88-88.01 min,50% -10% of A; 88.01-98 min,10% A.
According to the quality evaluation method provided by the invention, the quality markers of green tangerine peel and vinegar green tangerine peel can be distinguished into No. 1 peak and No. 5 peak.
The beneficial effects of the invention are as follows:
(1) According to the invention, HPLC finger prints before and after green tangerine peel vinegar processing are established and chemometric analysis is performed, the change of chemical components before and after green tangerine peel vinegar processing is systematically researched, and quality markers of the green tangerine peel are screened, so that scientific basis is provided for formulating more reasonable green tangerine peel quantity standards and further researching the processing principle of the green tangerine peel vinegar processing.
(2) The fingerprint analysis method of the green tangerine peel and the vinegar green tangerine peel provided by the invention is stable and reliable, and can be used for researching and identifying the fingerprints of the green tangerine peel and the vinegar green tangerine peel. The established fingerprint analysis method can systematically reflect the difference of chemical components of green tangerine peel and vinegar green tangerine peel decoction pieces, and the screened newly added components can be used as quality markers for distinguishing green tangerine peel and vinegar green tangerine peel, thereby providing scientific basis for formulating more reasonable vinegar green tangerine peel quantity standard and further researching the processing principle of vinegar-processed green tangerine peel.
Drawings
FIG. 1 is an HPLC fingerprint of green tangerine orange peel and vinegar green tangerine orange peel;
wherein A is green tangerine peel; b is vinegar green tangerine peel.
Fig. 2 is a HPLC profile of the mixed standard.
Fig. 3 is a green tangerine peel and vinegar green Pi Yinpian PCA 3D score plot (a) and a load plot (B).
FIG. 4 is a model score chart (A) and a model test chart (B) of green tangerine peel and vinegar green tangerine peel PLS-DA.
Fig. 5 is a VIP image of partial least squares analysis of green tangerine peel decoction pieces and vinegar green tangerine peel decoction pieces.
Fig. 6 is a tree diagram of the cluster analysis of green tangerine peel decoction pieces and vinegar green Pi Yinpian decoction pieces.
Detailed Description
The technical scheme of the invention is further explained and illustrated by the specific embodiments.
Example 1
1. Instrument and reagent
1.1 Instrument for measuring and controlling the intensity of light
Agilent 1200 high performance liquid chromatograph (including DAD detector, agilent company, usa), KQ-500DE digitally controlled ultrasonic cleaner (kunshan ultrasonic instruments limited), METTLER TOLEDO one ten million electronic balance (mertretolide company, usa), synergy UV ultra-water purifier (millbot company, usa).
1.2 Reagent(s)
Hesperidin reference (lot number 110721-201316) and synephrine reference (lot number 110727-200306) are all purchased from China food and drug inspection institute; acetonitrile and methanol are chromatographic purity; the water is self-made ultrapure water; the rest reagents are all analytically pure; glutinous rice aromatic vinegar (Laiyang Lu Hua vinegar industry Co., ltd., batch No. 20201222).
1.3 Material
10 batches of green tangerine peel were identified as Rutaceae plant orange by teaching through a teaching and research room Li Feng for identifying traditional Chinese medicines at Shandong university of traditional Chinese medicineCitrus reticulataProcessing products of the pericarp of dried young or immature fruits of Blanco and its cultivars. Sample information is shown in Table 1.
TABLE 1 batch green tangerine peel information
2.1 Preparation of vinegar green tangerine peel
According to the processing method of vinegar green tangerine peel of the 2020 edition of Chinese pharmacopoeia, stir-frying to slight yellow. Corresponding to the green Pi Yinpian numbers S1-S10, and the numbers of the vinegar green peels are marked as C1-C10.
2.2 Chromatographic conditions
Chromatographic column: thermo Hypersil GOLD C 18 Chromatographic column (250X 4.6 mm,5 μm); mobile phase: acetonitrile (a) -0.1% phosphoric acid water (B); sample injection volume: 10. mu L; flow rate: 1 mL/min; column temperature: 35. the temperature is lower than the temperature; detection wavelength: 283nm. The gradient elution conditions were: 0-8 min,10% -14% of A; 8-17 min,14% -16% of A; 17-38 min,16% -18% of A; 38-50 min,18% -30% of A; 50-72 min,30% -38% of A; 72-88 min,38% -50% of A; 88-88.01 min,50% -10% of A; 88.01-98 min,10% A.
2.3 Preparation of the solution
2.3.1 Preparation of control solution
And respectively weighing a proper amount of synephrine and hesperidin, precisely weighing, and adding methanol to prepare reference stock solutions containing 1.10 mg synephrine and 0.335 mg hesperidin in each 1 mL. And precisely sucking the reference substance stock solutions 1 mL respectively, placing the reference substance stock solutions in a 25mL volumetric flask, adding methanol for dilution and volume fixing, and preparing a mixed reference substance solution containing 44.00 mu g of synephrine and 13.40 mu g of hesperidin in each 1 mL.
2.3.2 Preparation of test solutions
Sample powder (sieving with No. 5 sieve) about 0.20 g, precisely weighing, placing in 50 mL conical flask with plug, precisely adding 100% methanol 25mL, sealing, weighing, ultrasonic treating (100W, 40 KHz) for 30 min, cooling, compensating for weight loss, filtering, collecting filtrate, and filtering with 0.45 μm microporous membrane.
2.4 Methodology investigation
2.4.1 Reference peak selection
The experiment uses hesperidin as a reference peak for calculating the relative retention time and the relative peak area of the fingerprint spectrum common peak.
2.4.2 Precision test
Taking a sample solution of green tangerine peel (batch number: 2007001), continuously injecting sample for 6 times according to the chromatographic condition under the item of 2.2, recording a chromatogram, introducing the chromatogram into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, taking the retention time of a No. 3 peak (hesperidin) as a reference peak, and recording the relative retention time of each common chromatographic peak. The result shows that the relative retention time of the common peak and the relative peak area RSD value range are 0.04% -0.97%, and the instrument precision meets the requirement.
2.4.3 Stability test
Taking a sample solution of green tangerine peel (batch No. 2007001), respectively injecting samples at 0,3,6,9, 12 and 24 hours according to the chromatographic condition under the item of 2.2, recording chromatograms, introducing the sample solution into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, and recording the relative retention time of each common chromatographic peak by taking the retention time of peak No. 3 (hesperidin) as a reference. The result shows that the relative retention time of the common peak and the relative peak area range of the RSD value are 0.05% -1.00%, and the test sample solution is stable within 24 hours.
2.4.4 Repeatability test
Taking green tangerine peel (batch number: 2007001) powder, preparing a sample solution according to the item "2.3.2", preparing 6 parts in parallel, injecting sample according to the chromatographic condition under the item "2.2", recording a chromatogram, introducing the chromatogram into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system ", taking the retention time of peak No. 3 (hesperidin) as a reference, and recording the relative retention time of all common chromatographic peaks. The results show that the relative retention time of the common peak and the RSD value range of the relative peak area are 0.03% -0.54%, and the method repeatability is good.
2.5 Fingerprint establishment and similarity analysis
2.5.1 Establishment and analysis of HPLC finger-print of green tangerine peel before and after vinegar processing
Sample solutions were prepared according to the method described under "2.3.2" and measured according to the chromatographic conditions described under "2.2". Recording chromatograms, introducing software of a traditional Chinese medicine chromatographic fingerprint similarity evaluation system (2012A edition), adopting a median method and a multipoint correction method, performing Mark peak matching for 0.10min, respectively establishing HPLC fingerprints before and after green tangerine peel vinegar processing, and respectively establishing green tangerine peel and vinegar green tangerine peel control fingerprints on the basis, as shown in figure 1. 8 common peaks are marked in the green tangerine peel fingerprint, 9 common peaks are marked in the vinegar green tangerine peel fingerprint, wherein the No. 5 peak is a common new peak in the vinegar green tangerine peel fingerprint. Comparison of the reference substances shows that the peak No. 1 is synephrine, the peak No. 3 is hesperidin, and the peak No. 5 is unknown component, as shown in FIG. 2. The chromatographic peak of No. 3 hesperidin with higher peak area and better separation degree is selected as a reference peak, the relative retention time of the common peaks of all samples is basically consistent, the RSD is less than or equal to 3.21%, the difference is smaller, the relative peak area RSD of all common peaks is 25.96% -192.24%, which indicates that the components of all batches of decoction pieces are similar, but the content of the components is different to a certain extent.
2.5.2 Similarity evaluation
And calculating the similarity between the green tangerine peel and the vinegar green tangerine peel and the respective control patterns by adopting software of a traditional Chinese medicine chromatographic fingerprint similarity evaluation system 2012A edition, wherein the similarity is shown in tables 2-4. The similarity of the green tangerine peel fingerprint spectrum and the comparison spectrum thereof is more than or equal to 0.956, the similarity of the vinegar green tangerine peel fingerprint spectrum and the comparison spectrum thereof is more than or equal to 0.941, the similarity range between the two decoction pieces is 0.937-0.999, which indicates that the similarity between each batch of samples is high, and the processing technology is stable, but the similarity evaluation is difficult to effectively distinguish the green tangerine peel from the vinegar green tangerine peel, the difference needs to be further clarified, and the two decoction pieces are effectively distinguished.
Table 2 green Pi Yinpian fingerprint similarity evaluation results
Table 3 results of evaluation of finger print similarity of acerola Pi Yinpian
TABLE 4 evaluation results of green tangerine peel and vinegar green Pi Yinpian fingerprint similarity
2.6 Multivariate statistical analysis of green tangerine peel and vinegar green tangerine peel fingerprint
2.6.1 Principal component analysis
The raw green tangerine peel and vinegar green tangerine peel common peak and vinegar green tangerine peel No. 5 peak area data are imported into SIMCA14.1 software, an unsupervised identification mode is established based on PCA, the distribution trend of the sample is observed, and the result is shown in Table 5. From Table 5, the variables can be fit to two principal components (PC 1, PC 2), PC1 describes a sample change of 55.8%, PC2 describes a sample change of 27.4%, and the total predictive power is 63.1%, the model is considered better. Green tangerine peel is gathered into one type, and vinegar green tangerine peel is gathered into one type, and the green tangerine peel and the vinegar green tangerine peel can be effectively distinguished. And obtaining a PCA three-dimensional projection graph and a distribution graph of 9 variables of all samples according to principal component analysis, wherein the result is shown in FIG. 3. The 9 variables are distributed at different positions and reflect the proportion of each chromatographic peak in the principal component analysis, and the contribution of points which are farther from the Y axis to the PC1 is larger, so the contribution degree to the PC1 is from large to small: peak No. 8 > peak No. 9 > peak No. 6 > peak No. 2 > peak No. 3 (hesperidin) > peak No. 7 > peak No. 5 > peak No. 1 (synephrine) > peak No. 4. The more points are farther from the X-axis, the greater the contribution to PC2, so the greater the contribution to the PC2 peak: peak No. 1 > peak No. 4 > peak No. 5 > peak No. 7 > peak No. 3 (hesperidin) > peak No. 2 > peak No. 9 > peak No. 6 > peak No. 8.
TABLE 5 PCA parameters
2.6.2 Partial least squares discriminant analysis (PLS-DA)
PLS-DA belongs to supervised pattern recognition analysis, and takes the common peak area of green tangerine peel and vinegar green tangerine peel and the peak area of No. 5 vinegar green tangerine peel as variables for further screening components which have great influence on the quality of two decoction pieces. Based on the analysis of the primary components in the early stage, SIMCA14.1 software is adopted to perform PLS-DA analysis on the peak areas of the two decoction pieces respectively to obtain a model score diagram and a model inspection diagram, the result is shown in fig. 4, the result can be seen from the model score diagram, green tangerine peel and vinegar green tangerine peel can be effectively distinguished, the intersection points with the abscissa axis are all less than 0.5, the intersection points with the ordinate are all less than 1, the left simulation R2 and Q2 are all less than the right, and the model is considered to have no fitting phenomenon and has good prediction capability. The results are shown in FIG. 5, with the peak numbers on the abscissa and the projection values (variable important in project, VIP) indicating the importance of the variables on the ordinate. VIP values it is generally believed that a component with a VIP value greater than 1 is the main difference component, the higher the VIP value, the higher the contribution rate to distinguishing the two samples. From the statistical results, VIP of peak No. 5 and peak No. 1 is greater than 1, so that the components represented by these 2 chromatographic peaks are considered to be quality markers for distinguishing green tangerine peel from vinegar green tangerine peel.
2.6.3 Mean value cluster analysis and hierarchical cluster analysis
And (5) introducing the peak area of the No. 5 peak with the larger contribution value into SPSS Statistics 22 software for mean K-cluster analysis, wherein the result is shown in Table 6. As can be seen from Table 6, green tangerine peel and vinegar green tangerine peel can be classified into two types, 10 batches of green tangerine peel belong to group 1, most vinegar green tangerine peel belongs to group 2, and C2, C8 and green tangerine peel are classified into one type. Hierarchical cluster analysis was further performed and the results are shown in FIG. 6. As can be seen from fig. 6, green tangerine peel may be classified as one type, and vinegar green tangerine peel may be classified as one type.
TABLE 6 mean K-Cluster analysis results
The green tangerine peel and the vinegar green tangerine peel chromatograms are subjected to principal component analysis, partial least squares discriminant analysis and cluster analysis to find that 2 principal components exist, and the green tangerine peel and the vinegar green tangerine peel can be distinguished. In order to further distinguish the difference of chemical components in green tangerine peel and vinegar green tangerine peel, a partial least square discriminant analysis model is established, the established model has better resolving power and predicting capability, and a No. 1 peak and a No. 5 peak are determined to be the difference components of green tangerine peel and vinegar green tangerine peel. When the peak 1 and the peak 5 or the peak 1 alone are used for K-cluster analysis, the degree of distinction is not good, the green tangerine peel cannot be distinguished, the peak 5 alone is used for K-cluster analysis, the green tangerine peel can be clustered into one type, the green tangerine peel can be mostly clustered into one type, but the average cluster of C2 and C8 and other green tangerine peel samples cannot be clustered into one type. The analysis reason is that the number 5 peak area in the two sample chromatograms is smaller and cannot be effectively distinguished from the biological chromatograms.
The experiment shows that the No. 5 peak is a common newly added chromatographic peak in all the green tangerine peel chromatograms, and other newly added chromatographic peaks are also included, but the newly added chromatographic peak is different due to different samples, so the No. 5 peak is considered to be a newly added component chromatographic peak after the green tangerine peel is roasted with vinegar.
Claims (3)
1. The quality evaluation method for distinguishing green tangerine peel from vinegar green tangerine peel is characterized by comprising the following steps:
(1) Preparation of test solution: taking green tangerine peel or vinegar green tangerine peel sample powder, precisely weighing, precisely adding methanol, weighing, performing ultrasonic treatment, cooling, compensating for weight loss, filtering, collecting the subsequent filtrate, and passing through microporous filter membrane to obtain the final product;
(2) Preparation of a control solution: respectively weighing synephrine and hesperidin, precisely weighing, adding methanol to prepare reference substance stock solution, precisely sucking the reference substance stock solution, adding methanol to dilute and fix volume, and preparing mixed reference substance solution;
(3) Respectively establishing fingerprint patterns of green tangerine peel and vinegar green tangerine peel by utilizing high performance liquid chromatography;
(4) Taking hesperidin as a reference peak, and carrying out green tangerine orange peel and vinegar green tangerine peel distinguishing verification through a fingerprint spectrogram;
the conditions of the high performance liquid chromatography are as follows: chromatographic column: thermo Hypersil GOLD C 18 A chromatographic column, 250X 4.6 mm,5 μm; the mobile phase A is acetonitrile, and the mobile phase B is 0.1% phosphoric acid water; sample injection volume: 10. mu L; flow rate: 1 mL/min; column temperature: 35. the temperature is lower than the temperature; detection wavelength: 283nm, performing gradient elution;
the conditions of the gradient elution are as follows: 0-8 min,10% -14% of A; 8-17 min,14% -16% of A; 17-38 min,16% -18% of A; 38-50 min,18% -30% of A; 50-72 min,30% -38% of A; 72-88 min,38% -50% of A; 88-88.01 min,50% -10% of A; 88.01-98 min,10% A.
2. The method for evaluating quality according to claim 1, wherein in the step (1), the sample solution is specifically prepared by: sample powder was measured at about 0.20 and g, precisely weighed, placed in a 50 mL stoppered conical flask, precisely added with 100% methanol 25 and mL, stoppered, weighed, sonicated at 100w at 40khz for 30 min, cooled, made up for weight loss, filtered, and the subsequent filtrate was filtered through a 0.45 μm microfiltration membrane.
3. The quality evaluation method according to claim 1 or 2, wherein in the step (2), the specific preparation process of the reference solution is as follows: and respectively weighing a proper amount of synephrine and hesperidin, precisely weighing, adding methanol to prepare reference substance stock solutions containing 1.10 mg synephrine and 0.335 mg hesperidin in each 1 mL, precisely sucking each 1 mL of the reference substance stock solutions, placing the reference substance stock solutions into a 25mL volumetric flask, adding methanol to dilute and fix the volume, and preparing a mixed reference substance solution containing 44.00 mug of synephrine and 13.40 mug of hesperidin in each 1 mL.
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