CN111671782A - Pomegranate peel processing method, quality control method and application - Google Patents
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Abstract
The invention belongs to the technical field of quality detection, and discloses a pomegranate rind processing method, a quality control method and application, wherein a sample pretreatment module is used for pretreating pomegranate rind; the processing module is used for processing the pomegranate rind based on orthogonal design; the parameter determination module is used for determining the water content, the total polyphenol content, the total triterpene content and the contents of gallic acid and ellagic acid; the comprehensive evaluation module is used for comprehensively analyzing the content measurement result and determining the processing influence parameters and the optimal processing parameters of the pomegranate rind; the quality control module is used for orthogonally optimizing the pomegranate bark carbonizing process; the odor analysis module is used for analyzing the odor change before and after the pomegranate rind is charred by utilizing a principal component analysis method and a linear discriminant analysis method. The method can better control the quality of the pomegranate bark decoction pieces, enables the subjective character standard of the processing degree of the pomegranate bark to be digital and visible, and provides reference for the electronic nose technology in the standardized application of the traditional Chinese medicine decoction pieces.
Description
Technical Field
The invention belongs to the technical field of measurement, and particularly relates to a pomegranate peel processing method, a quality control method and application.
Background
At present, the pomegranate peel is the dry peel of pomegranate (Punica granatum L.) belonging to the family punicaceae, has a long medicinal history in China, and has the effects of relieving diarrhea with astringents, stopping bleeding, expelling parasites and the like. In clinical medication, the most commonly used pomegranate peel decoction pieces comprise 2 raw products and charcoal products. However, the quality control indexes of the current pomegranate rind are limited to a small amount of components such as gallic acid, tannin, ellagic acid and the like, and thus the quality of the pomegranate rind medicinal material and the preparation thereof cannot be comprehensively controlled. The quality standard of the pomegranate bark charcoal serving as a processed product of pomegranate bark decoction pieces is only black and yellow on the surface in 2015 edition of Chinese pharmacopoeia, the internal tan character is specified, the standard is too simple, and the processing degree is influenced by subjective influence easily.
At present, the processing standard of the pomegranate peel carbon product is judged mainly based on sense and content measurement, the sense is easily influenced subjectively, and the odor is used as an important index of the sense and is difficult to form the standard. For example, the descriptions of "smell faint scent" and "burnt smell" in the pharmacopoeia are too subjective and fuzzy, and the electronic nose can better digitally express the "smell" in the processing process of traditional Chinese medicines. Compared with liquid chromatography and gas chromatography, the electronic nose technology is relatively simple to operate, only simple sample pretreatment is needed, and the integrity information of the sample is saved.
In the prior art, different processed products such as rhizoma zingiberis recens coptis chinensis, wine coptis chinensis and the like are accurately identified by using an electronic nose technology, and the identification rate is up to 96.4 percent through linear discriminant analysis. In the second prior art, the electronic nose is adopted to collect and analyze the odor before and after processing of 8-flavor wine-processed traditional Chinese medicines recorded in 2015 edition of Chinese pharmacopoeia, so that the odor difference of different processed products is digitalized and visualized, and the identification rate of the established discrimination model reaches 96.7%. In the prior art, three hawthorn samples in the same batch are fried at different time, the response value of an odor sensor is obtained by an electronic nose, the change of the odor in the hawthorn processing process is found to be related to the change of the content of 5-HMF, and the sugar degradation reaction and the Maillard reaction are inferred to be possibly one of the action mechanisms of the odor change in the hawthorn processing process. Therefore, the objective and quantitative research on the processing process of the traditional Chinese medicine is not only beneficial to perfecting the inspection and the determination of the character indexes related to the quality, but also beneficial to establishing the quality standard specification of the traditional Chinese medicine.
In conclusion, the problem of the existing pomegranate peel processing quality control is as follows:
(1) in the existing standard, the quality control of pomegranate bark processing is carried out according to the content of ellagic acid and tannin, and the processed pomegranate bark is not comprehensive enough to be used as the evaluation of the quality evaluation standard.
(2) The processing of the pomegranate rind requires the existence of fried charcoal, generates coke aroma and burnt flavor in the frying process, and lacks a system control method.
The difficulty of solving the technical problems is as follows: the processing quality control of the pomegranate rind is mainly based on content, visual observation and smelling, especially for controlling the smell, the objective index is lacked, and the use of an electronic nose ensures that the change of the smell of the pomegranate rind has certain objective index.
The significance of solving the technical problems is as follows: through comprehensive quality control of pomegranate peel processing, the content of the existing standard ellagic acid is reflected, the content control of other components of total polyphenol, total triterpene and gallic acid is increased, and the problem that the odor of the processed product lacks quality control means is fundamentally solved through the odor detection of an electronic nose.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a pomegranate rind processing method, a quality control method and application.
The invention is realized in the way, and the pomegranate rind processing method is characterized in that a stainless steel wok of the pomegranate rind processing method is placed on an induction cooker, the middle gear is opened, the temperature is heated, an infrared thermometer is used for measuring the temperature of the bottom of the wok, the pomegranate rind is placed when the temperature is 330 ℃, the pomegranate rind is quickly stir-fried, and after the surface is black and smoke is generated, the pomegranate rind is taken out after 16min, dried in the air and screened to remove scraps.
The invention also aims to provide a pomegranate bark processing quality control method of the pomegranate bark processing method, and the pomegranate bark processing quality control method comprises the following steps:
firstly, repeatedly washing pomegranate rind with tap water to remove impurities adhered to the pomegranate rind, washing with distilled water for 3 times, drying in a 45 ℃ oven, and storing for later use;
step two, selecting three levels of temperature and stir-frying time in the pomegranate bark stir-frying process according to L9(34) Processing pomegranate rind on an orthogonal table;
measuring the moisture content, the total polyphenol content, the total triterpene content and the contents of gallic acid and ellagic acid of the pomegranate rind after single processing;
step four, comprehensively analyzing the water content, the total polyphenol content, the total triterpene content and the determination results of the contents of the gallic acid and the ellagic acid, and determining the processing influence parameters and the optimal processing parameters of the pomegranate rind; analyzing the odor change before and after the pomegranate bark is charred by using a principal component analysis method and a linear discriminant analysis method;
and fifthly, orthogonally optimizing the pomegranate bark carbonizing process based on the optimal processing parameters and the related odor analysis result, and controlling the processing quality of the pomegranate bark.
Further, in the third step, the method for measuring the moisture content, the total polyphenol content, the total triterpene content and the contents of gallic acid and ellagic acid specifically comprises the following steps:
(1) and (3) determination of moisture content: taking the crushed and sieved pomegranate rind and processed pomegranate rind product powder with different degrees to be more than 0.5g, uniformly paving the powder on a sample disc of a rapid moisture tester, closing a sample chamber, and testing the moisture content in the sample according to the operation procedure of the tester;
(2) content determination of total polyphenols:
(3) the method for measuring the content of the total triterpene comprises the following steps:
(4) determination of the content of gallic acid and ellagic acid:
further, the method for measuring the content of the total polyphenol comprises the following steps:
1) preparing a gallic acid standard curve: weighing 25mg of gallic acid standard substance, dissolving with anhydrous ethanol, and metering to 25ml to obtain 1mg/ml gallic acid standard substance solution; precisely absorbing 0.00 ml, 0.20 ml, 0.40 ml, 0.60 ml, 0.80 ml, 1.00 ml and 1.20ml of gallic acid standard solution into a 25ml volumetric flask, adding 6ml of ferrous tartrate solution, shaking uniformly and standing for 10 min; fixing the volume with phosphate buffer solution of pH7.5, shaking, standing for color development, measuring absorbance with ultraviolet-visible spectrophotometer at 540nm wavelength after 30min, repeating for 3 times, and taking average value;
2) preparing a test article: weighing 1g of pericarpium Granati crude product and processed product powder, adding 20ml of 40% ethanol solution according to a material-to-liquid ratio of 1:20, ultrasonically extracting at 30 deg.C under high power for 30min, centrifuging at 8000r/min for 10min after ultrasonic extraction is finished, collecting supernatant, and diluting to 100ml with 40% ethanol solution to obtain sample solution; measuring 0.5ml of test solution,
adding 6ml of ferrous tartrate solution, shaking uniformly and standing for 10 min; and (3) adding phosphate buffer solution with the pH value of 7.5 to constant volume, shaking up, standing for color development, measuring the A value by using an ultraviolet-visible spectrophotometer at the wavelength of 540nm after 30min, repeating for 3 times, taking the average value, and calculating the content of the total polyphenol in each sample.
Further, the method for determining the content of the total triterpene comprises the following steps:
1) preparing an ursolic acid standard curve: weighing 5.00mg of ursolic acid standard substance in a 25ml volumetric flask, dissolving with methanol and fixing the volume to obtain 0.2mg/ml ursolic acid standard substance solution; accurately measuring 0.00, 0.20, 0.40, 0.60, 0.80, 1.00, 1.20 and 1.40ml of ursolic acid standard solution respectively, placing the ursolic acid standard solution in a 25ml test tube with a plug scale, heating in a water bath at 70 ℃ to volatilize the solvent, adding 0.6ml of 0.5 percent vanillin-glacial acetic acid solution and 2ml perchloric acid, cooling in an ice bath after 20min in a water bath at 60 ℃, adding glacial acetic acid to 25ml, fully shaking, measuring absorbance at a wavelength of 550nm, repeating for 3 times, and taking an average value;
2) preparing a test sample: weighing 1g of raw pomegranate rind and processed product powder, adding 20ml of ethanol solution with volume fraction of 70% according to a material-liquid ratio of 1:20, carrying out high-power ultrasonic extraction at 50 ℃ for 30min, after the extraction reaction is finished, carrying out centrifugal separation at 10000r/min for 10min, collecting supernatant, evaporating in a water bath, dissolving dry paste with methanol, and fixing the volume to 100ml to obtain a test solution; measuring a sample solution 1ml, placing the sample solution in a test tube with a plug scale, heating in a water bath at 70 ℃ to volatilize the solvent completely, adding 0.6ml of a 0.5% vanillin-glacial acetic acid solution and 2ml perchloric acid, cooling in an ice bath after 20min in a water bath at 60 ℃, adding glacial acetic acid to 25ml, fully shaking, measuring absorbance at a wavelength of 550nm, repeating for 3 times, and taking an average value; and calculating the content of the triterpenoid in the sample.
Further, the method for measuring the content of gallic acid and ellagic acid comprises the following steps:
1) preparing a reference solution: weighing 2.00mg of gallic acid, and diluting with ultrapure water to constant volume in a 10ml volumetric flask to obtain gallic acid reference solution with concentration of 0.2000 mg/ml; accurately weighing 2.62mg of ellagic acid, and metering to a 10ml volumetric flask with dimethyl sulfoxide to obtain an ellagic acid reference solution with a concentration of 0.2620 mg/ml; accurately sucking 5ml of gallic acid reference substance solution and ellagic acid reference substance solution respectively, and mixing by vortex shaking to obtain mixed reference substance solution with concentration of gallic acid 0.1mg/ml and ellagic acid 0.131 mg/ml;
2) drawing a standard curve: taking the mixed reference substance solution, respectively injecting 20 μ l, 15 μ l, 10 μ l, 5 μ l and 2 μ l, measuring peak areas under the wavelength conditions of 270nm and 254nm, and drawing a standard curve by taking the peak areas as ordinate and the content unit μ g as abscissa;
3) preparing a test solution: accurately weighing 0.25g of pericarpium Granati crude product and processed product, adding 25ml of distilled water, performing high power ultrasonic extraction for 30min, centrifuging at 10000r/min for 5min after ultrasonic extraction is finished, collecting supernatant, and filtering with 0.45 μm microporous membrane to obtain the final product;
4) determination precision: precisely absorbing a proper amount of a gallic acid and ellagic acid mixed reference solution, carrying out quantitative sample injection for 20 mu l, carrying out continuous sample injection for 6 times, storing the peak area of a target object in an off-line workstation, and calculating an RSD value;
5) and (3) measuring the stability: taking any sample powder, preparing a sample solution, respectively measuring for 0 h, 2h, 4 h, 6h, 8 h and 16h, storing the peak area of a target object in an off-line workstation, and calculating an RSD value;
6) determining the repeatability: sampling sample powder, preparing 6 parts of sample solution in parallel, storing the peak area of a target object in an off-line workstation, and calculating an RSD value;
7) and (3) measuring the content: respectively and precisely sucking the test solution to be tested at a flow rate of 0.8mg/ml for 0-12 min; 1mg/ml for 12-25 min; the column temperature is 30 ℃; the sample amount is 20 mul; detecting the wavelength of 270nm for 0-12 min and the wavelength of 254nm for 12-25 min; the detection time is 25 min; performing chromatographic determination, and determining the contents of gallic acid and ellagic acid simultaneously by the same method.
And thirdly, detecting the odor change of the pomegranate rind before and after charring through an electronic nose.
1) Pretreatment of samples
Crushing and sieving raw pomegranate rind and processed products, weighing 20g of the raw pomegranate rind and the processed products, placing the raw pomegranate rind and the processed products in a dry conical flask, sealing and standing, collecting odor information of a sample by adopting a standing headspace sampling method, wherein the headspace generation time is 120min, namely, the sample is placed in the conical flask and then sealed and kept standing for 2 h.
2) Detecting parameters
After the PEN3 electronic nose is connected with a computer, the configuration software WinMuster is operated. The detection parameters of the electronic nose are set as follows: clean dry air is used as carrier gas, the preparation time of pre-sampling is 8s, the sampling time is 160s, the gas flow is 0.4L/min, the waiting time is 10s, and the cleaning time is 50 s.
3) Odor collection
And (3) detecting headspace gas in the conical flask by using an electronic nose, collecting stable data of each sample, and repeatedly measuring each sample for 3 times.
4) Data analysis
The Principal Component Analysis (PCA) scatter diagram and the Linear Discriminant Analysis (LDA) projection diagram are adopted to effectively distinguish the processed products from the raw products and also can effectively distinguish the duration of the stir-frying charm.
The invention also aims to provide the pomegranate rind prepared by the pomegranate rind processing method.
The invention also aims to provide an antidiarrheal drug with astringents, which is prepared from the pomegranate rind.
Another object of the present invention is to provide a hemostatic drug prepared from the pomegranate rind.
Another object of the present invention is to provide an insect repellent prepared from the pomegranate rind.
In summary, the advantages and positive effects of the invention are: the quality of the pomegranate bark decoction pieces can be better controlled, the contents of gallic acid and ellagic acid in the decoction pieces are simultaneously determined by establishing HPLC, the contents of total polyphenol and total triterpene are determined by adopting a UV method, and the processing technology of the pomegranate bark is optimized by evaluating pomegranate bark carbon products with different processing degrees by multiple indexes. The electronic nose technology is used for detecting the odor change of the raw pomegranate bark product and the processed product, and the main component analysis method and the linear discriminant analysis method are used for distinguishing the raw pomegranate bark product from the charcoal product, so that the subjective character standard of the processing degree of the pomegranate bark is digitalized and visualized, and a reference is provided for the electronic nose technology in the standardized application of the traditional Chinese medicine decoction pieces.
Drawings
Fig. 1 is a flowchart of a processing quality control method for pomegranate rind according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of a gallic acid standard curve provided by the embodiment of the present invention.
Fig. 3 is a schematic diagram of a standard curve of ursolic acid provided by the embodiment of the present invention.
FIG. 4 is an HPLC plot of a control solution provided in an embodiment of the invention.
FIG. 5 is an HPLC chart of a sample solution provided in an embodiment of the present invention.
Fig. 6 is a schematic diagram of an HPLC standard curve of gallic acid provided by the embodiments of the present invention.
FIG. 7 is a schematic representation of the HPLC standard curve of ellagic acid provided by an embodiment of the present invention.
FIG. 8 is a diagram of the principal component analysis at different processing times according to the embodiment of the present invention.
In the figure: (a) at 270 deg.C for 8min, 12min, and 16 min; (b)300 deg.C, 8min, 12min, 16 min; (c) at 330 deg.C, 8min, 12min, 16 min.
FIG. 9 is a linear discriminant analysis diagram for different processing times according to an embodiment of the present invention.
In the figure: (a) at 270 deg.C for 8min, 12min, and 16 min; (b)300 deg.C, 8min, 12min, 16 min; (c) at 330 deg.C, 8min, 12min, 16 min.
FIG. 10 is a diagram of the principal component analysis at different processing temperatures according to the embodiment of the present invention.
In the figure: (a)8min, 270 deg.C, 300 deg.C, 330 deg.C; (b)12min at 270 deg.C, 300 deg.C, 330 deg.C; (c)16min, 270 deg.C, 300 deg.C, 330 deg.C.
FIG. 11 is a graph of linear discriminant analysis for different processing temperatures according to an embodiment of the present invention;
in the figure: (a)8min, 270 deg.C, 300 deg.C, 330 deg.C; (b)12min at 270 deg.C, 300 deg.C, 330 deg.C; (c)16min, 270 deg.C, 300 deg.C, 330 deg.C.
Fig. 12 is a principal component analysis diagram of a raw material and a processed product according to an embodiment of the present invention.
Fig. 13 is a linear discriminant analysis diagram of a raw material and a processed material according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The technical scheme and the technical effect of the invention are explained in detail in the following with the accompanying drawings.
The pomegranate rind processing method provided by the embodiment of the invention comprises the following steps:
repeatedly washing pericarpium Granati with tap water to remove impurities adhered to pericarpium Granati body, washing with distilled water for 3 times, drying in oven at 45 deg.C, and storing;
measuring the temperature of the bottom of the pan with an infrared thermometer, adding pericarpium Granati when the temperature is 330 deg.C, parching rapidly, taking out after the surface is black and smoke is generated, air drying, and sieving to remove debris.
As shown in fig. 1, the processing quality control method for pomegranate rind provided by the embodiment of the invention comprises the following steps:
s101: repeatedly washing pericarpium Granati with tap water to remove impurities adhered to pericarpium Granati body, washing with distilled water for 3 times, drying in oven at 45 deg.C, and storing.
S102: selecting three levels of temperature and stir-frying time in the process of stir-frying the pomegranate rind to be charcoal according to L9(34) Processing pericarpium Granati on orthogonal surface.
S103: measuring the moisture content, total polyphenol content, total triterpene content and gallic acid and ellagic acid content of the processed pericarpium Granati.
S104: comprehensively analyzing the water content, the total polyphenol content, the total triterpene content and the determination results of the contents of the gallic acid and the ellagic acid, and determining processing influence parameters and optimal processing parameters of the pomegranate rind; and analyzing the odor change of the pomegranate rind before and after charring by using a principal component analysis method and a linear discriminant analysis method.
S105: and orthogonally optimizing the pomegranate bark carbonizing process based on the optimal processing parameters and the related odor analysis results, and controlling the processing quality of the pomegranate bark.
The method for measuring the moisture content, the total polyphenol content, the total triterpene content and the contents of the gallic acid and the ellagic acid provided by the embodiment of the invention specifically comprises the following steps:
(1) and (3) determination of moisture content: and (3) taking the crushed and sieved pomegranate rind and processed pomegranate rind product powder with different degrees to be more than 0.5g, uniformly paving the powder on a sample plate of a rapid moisture tester, closing a sample chamber, and testing the moisture content in the sample according to the operation procedure of the tester.
(2) Content determination of total polyphenols:
(2.1) preparation of gallic acid Standard Curve: accurately weighing 25mg of gallic acid standard, dissolving with anhydrous ethanol, and metering to 25ml to obtain 1mg/ml gallic acid standard solution; precisely absorbing 0.00 ml, 0.20 ml, 0.40 ml, 0.60 ml, 0.80 ml, 1.00 ml and 1.20ml of gallic acid standard solution into a 25ml volumetric flask, adding 6ml of ferrous tartrate solution, shaking uniformly and standing for 10 min; then adding phosphate buffer solution with pH of 7.5 to constant volume, shaking, standing for color development, measuring absorbance with ultraviolet-visible spectrophotometer at 540nm wavelength after 30min, repeating for 3 times, and taking average value.
(2.2) preparing a test article: accurately weighing 1g of powder of pericarpium Granati crude product and processed product, adding 20ml of 40% ethanol solution according to a material-liquid ratio of 1:20, ultrasonically extracting at 30 deg.C under high power for 30min, centrifuging at 8000r/min for 10min after ultrasonic extraction is finished), collecting supernatant, and diluting to 100ml with 40% ethanol solution to obtain sample solution; 0.5ml of the test solution is measured.
Adding 6ml of ferrous tartrate solution, shaking uniformly and standing for 10 min; and (3) adding phosphate buffer solution with the pH value of 7.5 to constant volume, shaking up, standing for color development, measuring the A value by using an ultraviolet-visible spectrophotometer at the wavelength of 540nm after 30min, repeating for 3 times, taking the average value, and calculating the content of the total polyphenol in each sample.
(3) The method for measuring the content of the total triterpene comprises the following steps:
(3.1) preparing an ursolic acid standard curve: accurately weighing 5.00mg of ursolic acid standard substance in a 25ml volumetric flask, dissolving with methanol and fixing the volume to obtain 0.2mg/ml ursolic acid standard substance solution; accurately measuring 0.00, 0.20, 0.40, 0.60, 0.80, 1.00, 1.20 and 1.40ml of ursolic acid standard solution respectively, placing the ursolic acid standard solution in a 25ml test tube with a plug scale, heating in a water bath at 70 ℃ to volatilize the solvent, adding 0.6ml of 0.5 percent vanillin-glacial acetic acid solution and 2ml perchloric acid, cooling in the ice bath after 20min in the water bath at 60 ℃, adding glacial acetic acid to 25ml, fully shaking, measuring the absorbance at the wavelength of 550nm, repeating for 3 times, and taking the average value.
(3.2) preparation of a test article: accurately weighing 1g of powder of pericarpium Granati crude product and processed product, adding 20ml of 70 vol% ethanol solution according to a material-liquid ratio of 1:20, ultrasonically extracting at 50 deg.C under high power for 30min, centrifuging at 10000r/min for 10min after extraction reaction, collecting supernatant, evaporating in water bath, dissolving dry extract with methanol, and diluting to 100ml to obtain sample solution; measuring a sample solution 1ml, placing the sample solution in a test tube with a plug scale, heating in a water bath at 70 ℃ to volatilize the solvent completely, adding 0.6ml of a 0.5% vanillin-glacial acetic acid solution and 2ml perchloric acid, cooling in an ice bath after 20min in a water bath at 60 ℃, adding glacial acetic acid to 25ml, fully shaking, measuring absorbance at a wavelength of 550nm, repeating for 3 times, and taking an average value; and calculating the content of the triterpenoid in the sample.
(4) Determination of the content of gallic acid and ellagic acid:
(4.1) preparing a reference solution: accurately weighing 2.00mg of gallic acid, and diluting with ultrapure water to constant volume in a 10ml volumetric flask to obtain gallic acid reference solution with concentration of 0.2000 mg/ml; accurately weighing 2.62mg of ellagic acid, and metering to a 10ml volumetric flask with dimethyl sulfoxide to obtain an ellagic acid reference solution with a concentration of 0.2620 mg/ml; accurately sucking 5ml of gallic acid reference substance solution and ellagic acid reference substance solution respectively, and mixing by vortex and shaking to obtain mixed reference substance solution with concentration of gallic acid 0.1mg/ml and ellagic acid 0.131 mg/ml.
(4.2) drawing a standard curve: and taking the mixed control solution, respectively injecting 20 mu l, 15 mu l, 10 mu l, 5 mu l and 2 mu l of the mixed control solution, measuring peak areas under the conditions of wavelengths of 270nm and 254nm, and drawing a standard curve by taking the peak areas as vertical coordinates and the content unit mu g as horizontal coordinates.
(4.3) preparation of test solutions: accurately weighing 0.25g of pericarpium Granati crude product and processed product, adding 25ml of distilled water, performing high power ultrasonic extraction for 30min, centrifuging at 10000r/min for 5min after ultrasonic extraction is finished, collecting supernatant, and filtering with 0.45 μm microporous membrane.
(4.4) precision of measurement: precisely absorbing a proper amount of the mixed reference substance solution of the gallic acid and the ellagic acid, carrying out quantitative sample injection for 20 mu l, carrying out continuous sample injection for 6 times, storing the peak area of a target object in an off-line workstation, and calculating the RSD value.
(4.5) measurement of stability: taking any sample powder, preparing sample solution, measuring at 0, 2, 4, 6, 8 and 16h respectively, storing the peak area of the target object in an off-line workstation, and calculating RSD value.
(4.6) determination of reproducibility: sampling powder, preparing 6 parts of test solution in parallel, storing the peak area of a target object in an off-line workstation, and calculating the RSD value.
(4.7) measuring the content: respectively and precisely sucking the test solution to be tested at a flow rate of 0.8mg/ml for 0-12 min; 12-25 min at 1 mg/ml; the column temperature is 30 ℃; the sample amount is 20 mul; detecting the wavelength of 270nm for 0-12 min and the wavelength of 254nm for 12-25 min; the detection time is 25 min; performing chromatographic determination, and determining the contents of gallic acid and ellagic acid simultaneously by the same method.
(5) The electronic nose evaluates the odor change of the pomegranate rind before and after charring.
(5.1) pretreatment of the sample
Crushing and sieving raw pomegranate rind and processed products, weighing 20g of the raw pomegranate rind and the processed products, placing the raw pomegranate rind and the processed products in a dry conical flask, sealing and standing, collecting odor information of a sample by adopting a standing headspace sampling method, wherein the headspace generation time is 120min, namely, the sample is placed in the conical flask and then sealed and kept standing for 2 h.
(5.2) detecting the parameters
After the PEN3 electronic nose is connected with a computer, the configuration software WinMuster is operated. The detection parameters of the electronic nose are set as follows: clean dry air is used as carrier gas, the preparation time of pre-sampling is 8s, the sampling time is 160s, the gas flow is 0.4L/min, the waiting time is 10s, and the cleaning time is 50 s.
(5.3) odor Collection
And (3) detecting headspace gas in the conical flask by using an electronic nose, collecting stable data of each sample, and repeatedly measuring each sample for 3 times.
(5.4) data analysis
The Principal Component Analysis (PCA) scatter diagram and the Linear Discriminant Analysis (LDA) projection diagram are adopted to effectively distinguish the processed products from the raw products and also can effectively distinguish the duration of the stir-frying charm.
The best processing technology of the pomegranate rind provided by the embodiment of the invention specifically comprises the step of frying at 330 ℃ for 16 min.
The technical solution of the present invention will be further described with reference to the following specific examples.
Example 1:
1. materials and instruments
1.1 test materials
Pomegranate rind (variety: acid pomegranate, produced in Bo, Anhui, identified as certified acid pomegranate rind by professor Zhang Hua, college of food science and pharmaceutical engineering, Hoozhou, school of jujube and village).
1.2 test reagents
The reagents used in the test are shown in Table 1.
TABLE 1 test reagents
1.3 test apparatus
The instruments and equipment used in the test are shown in Table 2.
TABLE 2 instruments and apparatus
2. Experimental methods
2.1 pretreatment of pomegranate rind
Repeatedly washing the purchased pomegranate rind with tap water to remove impurities adhered to the pomegranate rind body, washing with distilled water for 3 times, drying in an oven at 45 ℃, and storing for later use.
2.2 processing of pomegranate rind
Taking 60g of clean pomegranate rind, investigating temperature and stir-frying time in the pomegranate rind charcoal frying process, selecting three levels respectively according to L9(34) Orthogonal tables are designed, orthogonal design factor levels are shown in table 3, and orthogonal design tests are shown in table 4. Processing pericarpium Granati, pulverizing pericarpium Granati and its processed product into powder with a small pulverizer, sieving with 45 mesh sieve, and sealing in a sample bottle.
TABLE 3 pomegranate rind charcoal-frying orthogonal design factor horizon
2.3 determination of the moisture content
Taking more than 0.5g of the powder of the pomegranate rind and processed products of the pomegranate rind with different degrees after being crushed and sieved under the item 2.2, uniformly paving the powder on a sample plate of a rapid moisture tester, closing a sample chamber, and measuring the moisture content in the sample according to the operation procedure of the tester.
2.4 content determination of Total polyphenols
2.4.1 preparation of Gallic acid Standard Curve
Accurately weighing 25mg of gallic acid standard, dissolving with anhydrous ethanol, and metering to 25ml to obtain 1mg/ml gallic acid standard solution. Precisely absorbing 0.00 ml, 0.20 ml, 0.40 ml, 0.60 ml, 0.80 ml, 1.00 ml and 1.20ml of gallic acid standard solution into a 25ml volumetric flask, adding 6ml of ferrous tartrate solution, shaking uniformly and standing for 10 min; then adding phosphate buffer solution with pH of 7.5 to constant volume, shaking, standing for color development, measuring absorbance with ultraviolet-visible spectrophotometer at 540nm wavelength after 30min, repeating for 3 times, and taking average value.
2.4.2 preparation of test articles
Accurately weighing 1g of powder of pericarpium Granati crude product and processed product, adding 20ml of 40% ethanol solution at a ratio of 1:20, and ultrasonic extracting (30 deg.C, 30min, high power). After the ultrasonic treatment is finished, the supernatant is collected by centrifugal separation (8000r/min, 10min), and the volume is determined to be 100ml by 40% ethanol solution to be used as a test solution. Measuring 0.5ml of test solution, measuring A value at 540nm wavelength according to the method of '3.4.1', repeating for 3 times, averaging, and calculating total polyphenol content in each sample.
2.5 determination of Total triterpene content
2.5.1 preparation of Ursolic acid Standard Curve
Accurately weighing 5.00mg of ursolic acid standard substance in a 25ml volumetric flask, dissolving with methanol and fixing the volume to obtain 0.2mg/ml ursolic acid standard substance solution. Accurately measuring 0.00, 0.20, 0.40, 0.60, 0.80, 1.00, 1.20 and 1.40ml of ursolic acid standard solution respectively, placing the ursolic acid standard solution in a 25ml test tube with a plug scale, heating in a water bath at 70 ℃ to volatilize the solvent, adding 0.6ml of 0.5 percent vanillin-glacial acetic acid solution and 2ml perchloric acid, cooling in the ice bath after 20min in the water bath at 60 ℃, adding glacial acetic acid to 25ml, fully shaking, measuring the absorbance at the wavelength of 550nm, repeating for 3 times, and taking the average value.
2.5.2 preparation of test articles
Accurately weighing 1g of powder of pericarpium Granati crude product and processed product, adding 20ml of 70% ethanol solution at a ratio of 1:20, and ultrasonic extracting (50 deg.C, 30min, high power). After the extraction reaction is finished, centrifugally separating (10000r/min, 10min) and collecting supernatant, evaporating to dryness in water bath, dissolving dry paste with methanol and fixing the volume to 100ml to be used as a test solution. Measuring 1ml of test solution, measuring the light absorption value according to the method under the item '2.5.1', and calculating the content of the triterpenoid in the sample.
2.6 determination of the content of Gallic acid and ellagic acid
2.6.1 preparation of control solutions
Accurately weighing 2.00mg of gallic acid, and diluting with ultrapure water to a volume of 10ml volumetric flask to obtain gallic acid reference solution (0.2000 mg/ml).
Accurately weighing ellagic acid 2.62mg, and metering to 10ml volumetric flask with dimethyl sulfoxide (DMSO) to obtain ellagic acid control solution (0.2620 mg/ml).
Accurately sucking 5ml of gallic acid control solution and ellagic acid control solution respectively, and mixing by vortex and shaking to obtain mixed control solution (gallic acid 0.1mg/ml, ellagic acid 0.131 mg/ml).
2.6.2 drawing of Standard Curve
Taking the mixed reference substance solution, injecting 20 μ l, 15 μ l, 10 μ l, 5 μ l and 2 μ l respectively, measuring peak areas under the conditions of 270nm and 254nm wavelength, and drawing a standard curve by taking the peak areas as ordinate and the content (μ g) as abscissa.
2.6.3 preparation of test solutions
Accurately weighing 0.25g pericarpium Granati crude product and processed product, adding 25ml distilled water, performing high power ultrasonic extraction for 30min, centrifuging (10000r/min, 5min) after ultrasonic extraction, collecting supernatant, and filtering with 0.45 μm microporous membrane.
2.6.4 chromatographic conditions
TABLE 5 chromatographic conditions
TABLE 6 mobile phase System
2.6.5 precision
Precisely sucking a proper amount of a gallic acid and ellagic acid mixed reference solution under the item of '2.6.1', quantitatively injecting 20 mu l of sample, continuously injecting for 6 times, storing the peak area of a target object in an off-line workstation, and calculating the RSD value.
2.6.6 stability
Taking any sample powder, preparing sample solution according to the method under '2.6.3', measuring at 0, 2, 4, 6, 8, 16h respectively, storing the peak area of the target object at off-line workstation, and calculating RSD value.
2.6.7 repeatability
Taking sample powder as the item 2.6.6, preparing 6 parts of sample solution in parallel, storing the peak area of the target object by an off-line workstation, and calculating the RSD value.
2.6.8 content determination
Precisely absorbing the test solution, and determining the contents of gallic acid and ellagic acid simultaneously by the method according to the chromatographic condition under the item of 2.6.4.
2.7 determination of odor
2.7.1 pretreatment of samples
Crushing and sieving raw pomegranate rind and processed products, weighing 20g of the raw pomegranate rind and the processed products, placing the raw pomegranate rind and the processed products in a dry conical flask, sealing and standing, collecting odor information of a sample by adopting a standing headspace sampling method, wherein the headspace generation time is 120min, namely, the sample is placed in the conical flask and then sealed and kept standing for 2 h.
2.7.2 detection parameters
After the PEN3 electronic nose is connected with a computer, the configuration software WinMuster is operated. The detection parameters of the electronic nose are set as follows: clean dry air is used as carrier gas, the preparation time of pre-sampling is 8s, the sampling time is 160s, the gas flow is 0.4L/min, the waiting time is 10s, and the cleaning time is 50 s.
2.7.3 odor collection
And (3) detecting headspace gas in the conical flask by using an electronic nose, collecting stable data of each sample, and repeatedly measuring each sample for 3 times.
2.7.4 data analysis
2.7.4.1 principal component analysis
The principal component analysis can keep the information of original measured data to the maximum extent, the data transformation and the dimension reduction are carried out on the multi-index information measured by the electronic nose sensor, the multi-index information is classified, and finally, a main two-dimensional scatter diagram is displayed on the PCA analysis scatter diagram.
2.7.4.2 linear discriminant analysis
Linear Discriminant Analysis (LDA) constructs a discriminant function from original data through linear combination, divides a multidimensional space into subspaces, can furthest distinguish different samples, and has good classification effect and easy realization. This analysis focuses more on the distribution of the samples in space and the distance between them, and projects the sample signal data through an algorithm into a direction such that the projections are as far apart as possible from group to group.
3. Results and analysis
3.1 Properties of processed samples
Pomegranate rind was processed under the orthogonal test conditions in Table 4, and the properties of the samples are shown in Table 7.
TABLE 7 pomegranate rind processed product characteristics
3.2 moisture content measurement results
The results of measuring the moisture content of the pomegranate rind and the processed pomegranate rind products by the method under item 2.3 are shown in table 8, 0 represents raw product, and 1 to 9 represent each processed product under orthogonal condition.
TABLE 8 moisture content of pomegranate rind and pomegranate rind processed product
3.3 Total Polyphenol content measurement results
3.3.1 Gallic acid Standard Curve
Measuring the light absorption value according to the method under the item of '2.4.1', taking the concentration of the gallic acid as a horizontal coordinate and the absorbance as a vertical coordinate, and performing linear regression on the average value of the parallel measurement results to obtain an equation between the concentration (x) of the gallic acid and the light absorption value (y): 14.336x+0.0009，R20.9994. The gallic acid concentration is shown to be within the range of 0.008-0.0112 mg/ml, and has a good linear relation with the light absorption value.
3.3.2 analysis of Total Polyphenol content
In the measurement of the total polyphenol content, the total polyphenol content of the raw product is 20.31%, the total polyphenol content of each processed product is obviously reduced after processing, the analysis of the result of the total polyphenol content is shown in table 10, in addition, the stir-frying temperature has significant influence on the quality of the pomegranate rind decoction pieces, the stir-frying time has no significant influence, and the analysis of variance is shown in table 11.
The total polyphenol content calculation method comprises the following steps:
in the formula (1), W is the total polyphenol content (%) of the pomegranate rind and pomegranate rind processed products, c is the concentration (mg/ml) of the total polyphenol to be measured, V is the volume (ml) of the test solution, n is the dilution multiple, M is the mass (g) of the sample, and W is the water content (%) of the sample.
TABLE 10 analysis of results of orthogonal test for determining total polyphenol content
TABLE 11 analysis of variance of total polyphenol content
3.4 Total triterpene assay results
3.4.1 Ursolic acid Standard Curve
Determining the light absorption value according to the method under item 2.5.2, taking the concentration of the ursolic acid as an abscissa and the absorbance as an ordinate, and performing linear regression on the average value of the parallel determination results to obtain an equation between the concentration (x) of the ursolic acid and the light absorption value (y): y 47.837x +0.0044, R20.999. Within the range of 0.0016-0.0112 mg/ml of ursolic acid concentration, the ursolic acid concentration and the light absorption value have a good linear relation.
3.4.2 Total triterpene assay results analysis
In the total triterpene content measurement, the raw total triterpene content was 2.94%, the triterpene content of each processed product was not changed greatly after processing, the processing temperature and processing time did not significantly affect the quality of the pomegranate rind decoction pieces, the result analysis and the variance analysis are shown in table 12 and 13, respectively.
The total triterpene content calculation method comprises the following steps:
in the formula (2), W is the total triterpene content (%) of the pomegranate rind and the processed pomegranate rind product, c is the concentration (mg/ml) of the total triterpene, V is the volume (ml) of the test solution, n is the dilution multiple, M is the sampling mass (g), and W is the water content (%) of the sample.
TABLE 12 results of orthogonal assay for total triterpene content
TABLE 13 analysis of variance of total triterpene content
3.5 determination of Gallic acid and ellagic acid content
3.5.1 results of HPLC identification of gallic acid and ellagic acid
The separation of gallic acid, ellagic acid and other components can reach baseline, and the separation effect of gallic acid and ellagic acid is good under the chromatographic condition of the experiment.
3.5.2 determination of Gallic acid content
3.5.2.1 gallic acid standard curve
Measuring peak area according to the method under the item of '2.6.4', drawing a standard curve according to the method in '2.6.2', and obtaining a linear regression equation by taking the concentration (x) of gallic acid as a horizontal coordinate and the peak area (y) as a vertical coordinate: 3635.6x-3.2146，R20.9996. The gallic acid concentration and peak area are in linear relationship in the range of 0.2-2 μ g gallic acid mass. As shown in fig. 5.
3.5.2.2 analysis of gallic acid content
In the determination of gallic acid content, 0.1% of gallic acid was added to each processed product after processing, but the processing temperature and processing time did not significantly affect the pomegranate rind charcoal product, and the analysis of gallic acid content under each processing condition is shown in table 14, and the analysis of variance is shown in table 15.
The method for calculating the content of the gallic acid comprises the following steps:
in the formula (3), W is the content (%) of gallic acid in the pomegranate rind and the processed product of the pomegranate rind, M is the mass (μ g) of gallic acid to be measured, n is the dilution factor, M is the mass (g) of the sample, and W is the water content (%) of the sample.
TABLE 14 analysis of results of gallic acid content determination by orthogonal assay
TABLE 15 analysis of gallic acid content and variance
3.5.3 measurement results of ellagic acid content
3.5.3.1 Standard Curve of ellagic acid
Measuring peak area according to the method under item "2.6.4", drawing a standard curve according to the method in item "2.6.2", and obtaining a linear regression equation by taking the concentration of gallic acid (X) as abscissa and the peak area (A) as ordinate: 13811x-396.08, R20.9992. In the range of ellagic acid mass of 0.262-2.62 μ g, ellagic acid concentration and peak area are linear, as shown in fig. 6.
3.5.3.2 analysis of ellagic acid assay results
In the content measurement of ellagic acid, the content of ellagic acid in the raw pomegranate bark is 1.08%, the content of ellagic acid in each processed product is increased after processing, the processing temperature has a significant influence on the quality of the pomegranate bark decoction pieces, the result analysis of ellagic acid is shown in table 16, and the variance analysis is shown in table 17.
The ellagic acid content calculation method comprises the following steps:
in the formula (4), W is the content (%) of ellagic acid in the pomegranate rind and the processed pomegranate rind, M is the mass (μ g) of the total polyphenol to be measured, n is the dilution factor, M is the mass (g) of the sample, and W is the water content (%) of the sample. The results of the measurement of ellagic acid content are shown in Table 16, and the analysis of variance is shown in FIGS. 5 to 11.
TABLE 16 results of the measurement of ellagic acid content by orthogonal test
TABLE 17 ellagic acid content ANOVA TABLE
3.5.4 precision test results
Experiments were carried out according to the method under item "2.4.3.3", and the RSD values of gallic acid and ellagic acid were 1.48% and 0.67%, respectively, indicating good precision of the instrument.
3.5.5 stability test results
Experiments were carried out according to the method under "2.4.3.4", and the RSD values of gallic acid and ellagic acid were 1.96% and 1.27%, respectively, indicating that the test solution was stable for at least 16 h.
3.5.6 repeatability test results
Experiments were performed according to the method in "2.4.3.5" and the RSD values of gallic acid and ellagic acid were 2.49% and 2.31%, respectively, indicating that the reproducibility of the test method was good.
3.6 Total Polyphenol, Total triterpene, Gallic acid and ellagic acid content determination and analysis
Selecting processing time (X) under the premise of same specification of decoction pieces1) Processing temperature (X)2) As a factor, the total polyphenol content (Y)1) Total triterpene content (Y)2) Total amount of gallic acid and ellagic acid (Y)3) As an evaluation index, different weighting coefficients are given to the index differences to obtain a composite score (Y) in the formula of Y ═ Y1/y1max)*40+(y2/y2max)*20+(y3/y3max)*20+(y4/y4max) 20, the optimal processing technology of the obtained pomegranate peel is A3B3Namely, the processing temperature is 330 ℃, the processing time is 16min, blank factor terms are taken as error terms, and the temperature obtained by variance analysis has significant influence on the processing of the pomegranate peel charcoal product. The visual analysis table of composite scores is shown in Table 18, and the analysis of variance table is shown in Table 19.
TABLE 18 comprehensive scoring results for assay
TABLE 19 ANOVA TABLE
3.7 comparison of the pomegranate rind raw product with the optimized charcoal
The optimal optimized pomegranate peel charcoal frying process is A3B3Experiments prove that after the pomegranate rind is stir-fried to be charcoal, the total polyphenol content, the total triterpene content, the gallic acid content and the ellagic acid content of the raw product and the charcoal product are shown in the table 20. The content of relatively crude product is reduced to 89.46%, the content of total triterpene is reduced to 97.62%, and the content of gallic acid and ellagic acid is lower than that of relatively crude productThe secondary rises to 270% and 105.55%. In the pomegranate bark carbonizing process, under the high-temperature condition, the polyphenol is decomposed to generate gallic acid and ellagic acid, and the conclusion is consistent with the study on the content change rule of the gallic acid and the ellagic acid in the pomegranate bark carbonizing process by using Zhou Qian and the like.
TABLE 20 comparison of the contents of the ingredients of raw product and charcoal
3.8 odor analysis results of crude and charcoal pomegranate rind
3.8.1 differentiation of odor by processing time
After the odor information of the pomegranate rind sample is measured according to the detection parameters under the item '2.7.2', the main component analysis and the linear discriminant analysis are carried out on the sample data of different processing times under the same processing temperature. As shown in FIG. 7, when the processing time is 8min, 12min, and 16min, PC1 at 270 deg.C, 300 deg.C, and 330 deg.C respectively sequentially comprises: 79.85%, 98.11%, 93.50%; as shown in fig. 8, the linear discriminant analysis by LD1 is: 94.75%, 97.44% and 98.67%. The data of the electronic noses of the processed products in different processing time are not overlapped under the same temperature condition, and the discrimination is better. Further analysis shows that the processed products with different processing time are mainly distributed in three areas, which shows that the volatile smells of the three processed products can be clearly distinguished. This shows that the electronic nose technology can well carry out qualitative identification on the pomegranate rind processed products at different processing times.
3.8.2 differentiation of odor by processing temperature
After the odor information of the pomegranate rind sample is measured according to the detection parameters under the item '2.7.2', the main component analysis and the linear discriminant analysis are carried out on the sample data of different processing temperatures under the same time condition. The main component analysis is shown in FIG. 9, PC1 is 90.27%, 94.99% and 95.12% respectively at processing temperature of 270 deg.C, 300 deg.C and 330 deg.C for 8min, 12min and 16min, and the linear discriminant analysis is shown in FIG. 10, LD1 is 97.26%, 88.67% and 88.05% respectively. The data of the electronic noses of the processed products at different processing temperatures are not overlapped under the condition of the same processing time, and the discrimination is better. Further analysis shows that the processed products with different processing time are mainly distributed in three areas, which shows that the volatile smells of the three processed products can be clearly distinguished. This shows that the electronic nose technology can well carry out qualitative identification on the pomegranate rind processed products with different processing temperatures.
3.8.3 analysis of odor change of raw and processed products
After the odor information of the pomegranate rind and the processed pomegranate rind products is measured according to the detection parameters under the item '2.7.2', the main component analysis and the linear discriminant analysis are carried out on the raw pomegranate rind products and the optimized pomegranate rind charcoal products, the PC1 and the LD1 are respectively 88.46 percent and 100 percent, and the analysis results are shown in fig. 11 and fig. 12, which indicate that the raw pomegranate rind products and the charcoal products are not overlapped and have better discrimination. Also shows that the electronic nose technology can well carry out qualitative identification on the pomegranate bark raw product and the processed product. According to the data of the electronic nose detector, the detector for causing the odor change before and after the pomegranate bark is roasted is W5S, the sensitivity of W5S to nitrogen oxides can be high according to the appendix 3 electronic nose sensor array and the main function, and the reason for causing the odor change of raw pomegranate bark and charcoal products is related to the temperature rise in the pomegranate bark roasting process and the generation of nitrogen oxides due to the decomposition of alkaloid components under the high-temperature condition.
4. Results
In the optimal process for processing the pomegranate rind optimized by orthogonal design, the optimal process condition of the pomegranate rind charcoal processing process is A3B3The processing is carried out for 16min at 330 ℃, the comprehensive evaluation obtained by weighting according to the contents of the total polyphenol, the total triterpene, the gallic acid and the ellagic acid is the highest, according to the yield of each weighted index, the main influencing factor is the processing temperature > the processing time, and the processing temperature has significant influence on the quality of the pomegranate rind decoction pieces. In addition, the electronic nose technology can obviously distinguish the raw pomegranate bark products from the processed products, and the main component analysis method and the linear discriminant analysis method can clearly distinguish the raw pomegranate bark products from the charcoal products. The processing property is objective and digitalized by researching the electronic nose technology in the processing process of the traditional Chinese medicine, and the electronic nose technology is applied to the standardization of the traditional Chinese medicine decoction piecesReference is provided therein. At present, the quality evaluation of the traditional Chinese medicine mainly comprises the coexistence of a subjective mode and an objective mode, objective evaluation takes a leading position by virtue of objective data, and only one or more effective components in the traditional Chinese medicine are evaluated as a quality evaluation standard, so that the traditional Chinese medicine quality evaluation is not comprehensive enough, and is time-consuming and labor-consuming. In the traditional quality evaluation of traditional Chinese medicines, the smell is an important evaluation index, each traditional Chinese medicine is strong or light, has unique smell, and the smell is directly related to the content of chemical components and can reflect the internal quality of the medicine, so the smell can be completely used as the external evaluation standard of the quality of the traditional Chinese medicines, and the application of the electronic nose technology in the traditional Chinese medicine quality evaluation is an innovation, and the technical change of the traditional Chinese medicine quality evaluation is brought.
Electronic nose PEN3 standard sensor array and main application thereof
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The processing quality control method of the pomegranate rind is characterized by comprising the following steps:
firstly, repeatedly washing pomegranate rind with tap water to remove impurities adhered to the pomegranate rind, washing with distilled water for 3 times, drying in a 45 ℃ oven, and storing for later use;
step two, selecting three levels of temperature and stir-frying time in the pomegranate bark stir-frying process according to L9(34) Processing pomegranate rind on an orthogonal table;
step three, measuring the moisture content, the total polyphenol content, the total triterpene content and the contents of gallic acid and ellagic acid of the pomegranate peel charcoal;
step four, comprehensively analyzing the water content, the total polyphenol content, the total triterpene content and the determination results of the contents of the gallic acid and the ellagic acid, and determining the processing influence parameters and the optimal processing parameters of the pomegranate rind; analyzing the odor change before and after the pomegranate bark is charred by using a principal component analysis method and a linear discriminant analysis method;
and fifthly, orthogonally optimizing the pomegranate bark carbonizing process based on the optimal processing parameters and the related odor analysis result, and controlling the processing quality of the pomegranate bark.
2. The pomegranate rind processing quality control method of claim 1, wherein in the third step, the method for measuring the moisture content, the total polyphenol content, the total triterpene content and the contents of gallic acid and ellagic acid specifically comprises:
(1) and (3) determination of moisture content: taking the crushed and sieved pomegranate rind and processed pomegranate rind product powder with different degrees to be more than 0.5g, uniformly paving the powder on a sample disc of a rapid moisture tester, closing a sample chamber, and testing the moisture content in the sample according to the operation procedure of the tester;
(2) measuring the content of total polyphenol;
(3) a method for measuring the content of total triterpenoids;
(4) and (4) measuring the content of gallic acid and ellagic acid.
3. The pomegranate rind processing quality control method of claim 2, wherein the method for measuring the content of total polyphenols comprises:
1) preparing a gallic acid standard curve: weighing 25mg of gallic acid standard substance, dissolving with anhydrous ethanol, and metering to 25ml to obtain 1mg/ml gallic acid standard substance solution; precisely absorbing 0.00 ml, 0.20 ml, 0.40 ml, 0.60 ml, 0.80 ml, 1.00 ml and 1.20ml of gallic acid standard solution into a 25ml volumetric flask, adding 6ml of ferrous tartrate solution, shaking uniformly and standing for 10 min; fixing the volume with phosphate buffer solution of pH7.5, shaking, standing for color development, measuring absorbance with ultraviolet-visible spectrophotometer at 540nm wavelength after 30min, repeating for 3 times, and taking average value;
2) preparing a test article: weighing 1g of pomegranate peel raw product and processed product powder, adding 20ml of 40% ethanol solution according to a material-liquid ratio of 1:20, carrying out ultrasonic extraction at 30 ℃ and 250kw for 30min, after the ultrasonic extraction is finished, carrying out centrifugal separation at 8000r/min for 10min, collecting supernatant, and using 40% ethanol solution to fix the volume to 100ml to serve as a test solution; measuring 0.5ml of test solution;
adding 6ml of ferrous tartrate solution, shaking uniformly and standing for 10 min; and (3) adding phosphate buffer solution with the pH value of 7.5 to constant volume, shaking up, standing for color development, measuring the A value by using an ultraviolet-visible spectrophotometer at the wavelength of 540nm after 30min, repeating for 3 times, taking the average value, and calculating the content of the total polyphenol in each sample.
4. The pomegranate rind processing quality control method of claim 2, wherein the method for measuring the total triterpene content comprises the following steps:
1) preparing an ursolic acid standard curve: weighing 5.00mg of ursolic acid standard substance in a 25ml volumetric flask, dissolving with methanol and fixing the volume to obtain 0.2mg/ml ursolic acid standard substance solution; accurately measuring 0.00, 0.20, 0.40, 0.60, 0.80, 1.00, 1.20 and 1.40ml of ursolic acid standard solution respectively, placing the ursolic acid standard solution in a 25ml test tube with a plug scale, heating in a water bath at 70 ℃ to volatilize the solvent, adding 0.6ml of 0.5 percent vanillin-glacial acetic acid solution and 2ml perchloric acid, cooling in an ice bath after 20min in a water bath at 60 ℃, adding glacial acetic acid to 25ml, fully shaking, measuring absorbance at a wavelength of 550nm, repeating for 3 times, and taking an average value;
2) preparing a test sample: weighing 1g of raw pomegranate rind and processed product powder, adding 20ml of ethanol solution with volume fraction of 70% according to a material-liquid ratio of 1:20, carrying out high-power ultrasonic extraction at 50 ℃ for 30min, after the extraction reaction is finished, carrying out centrifugal separation at 10000r/min for 10min, collecting supernatant, evaporating in a water bath, dissolving dry paste with methanol, and fixing the volume to 100ml to obtain a test solution; measuring a sample solution 1ml, placing the sample solution in a test tube with a plug scale, heating in a water bath at 70 ℃ to volatilize the solvent completely, adding 0.6ml of a 0.5% vanillin-glacial acetic acid solution and 2ml perchloric acid, cooling in an ice bath after 20min in a water bath at 60 ℃, adding glacial acetic acid to 25ml, fully shaking, measuring absorbance at a wavelength of 550nm, repeating for 3 times, and taking an average value; calculating the content of the triterpenoid in the sample;
the method for measuring the content of gallic acid and ellagic acid comprises the following steps:
1) preparing a reference solution: weighing 2.00mg of gallic acid, and diluting with ultrapure water to constant volume in a 10ml volumetric flask to obtain gallic acid reference solution with concentration of 0.2000 mg/ml; accurately weighing 2.62mg of ellagic acid, and metering to a 10ml volumetric flask with dimethyl sulfoxide to obtain an ellagic acid reference solution with a concentration of 0.2620 mg/ml; accurately sucking 5ml of gallic acid reference substance solution and ellagic acid reference substance solution respectively, and mixing by vortex shaking to obtain mixed reference substance solution with concentration of gallic acid 0.1mg/ml and ellagic acid 0.131 mg/ml;
2) drawing a standard curve: taking the mixed reference substance solution, respectively injecting 20 μ l, 15 μ l, 10 μ l, 5 μ l and 2 μ l, measuring peak areas under the wavelength conditions of 270nm and 254nm, and drawing a standard curve by taking the peak areas as ordinate and the content unit μ g as abscissa;
3) preparing a test solution: accurately weighing 0.25g of pericarpium Granati crude product and processed product, adding 25ml of distilled water, performing high power ultrasonic extraction for 30min, centrifuging at 10000r/min for 5min after ultrasonic extraction is finished, collecting supernatant, and filtering with 0.45 μm microporous membrane to obtain the final product;
4) determination precision: precisely absorbing a proper amount of a gallic acid and ellagic acid mixed reference solution, carrying out quantitative sample injection for 20 mu l, carrying out continuous sample injection for 6 times, storing the peak area of a target object in an off-line workstation, and calculating an RSD value;
5) and (3) measuring the stability: taking any sample powder, preparing a sample solution, respectively measuring for 0 h, 2h, 4 h, 6h, 8 h and 16h, storing the peak area of a target object in an off-line workstation, and calculating an RSD value;
6) determining the repeatability: sampling sample powder, preparing 6 parts of sample solution in parallel, storing the peak area of a target object in an off-line workstation, and calculating an RSD value;
7) and (3) measuring the content: respectively and precisely sucking the test solution to be tested at a flow rate of 0.8mg/ml for 0-12 min; 1mg/ml for 12-25 min; the column temperature is 30 ℃; the sample amount is 20 mul; detecting the wavelength of 270nm for 0-12 min and the wavelength of 254nm for 12-25 min; the detection time is 25 min; performing chromatographic determination, and determining the contents of gallic acid and ellagic acid simultaneously by the same method.
5. The pomegranate rind processing quality control method of claim 2, wherein the odor analysis: detecting response values of the pomegranate rind on the sensor before and after charring through an electronic nose to serve as processing smell parameters;
1) pretreatment of samples
Crushing and sieving raw pomegranate rind and processed products, weighing 20g of the raw pomegranate rind and the processed products, placing the raw pomegranate rind and the processed products in a dry conical flask, sealing and standing, collecting odor information of a sample by adopting a standing headspace sampling method, wherein the headspace generation time is 120min, namely, the sample is placed in the conical flask and then sealed and kept standing for 2 h;
2) detecting parameters
After the PEN3 electronic nose is connected with a computer, the configuration software Win Muster is operated, and all detection parameters of the electronic nose are set as follows: clean dry air is taken as carrier gas, the pre-sampling preparation time is 8s, the sampling time is 160s, the gas flow is 0.4L/min, the waiting time is 10s, and the cleaning time is 50 s;
3) odor collection
Detecting headspace gas in the conical flask by using an electronic nose, collecting stable data of each sample, and repeatedly measuring each sample for 3 times;
4) data analysis
And a PCA scatter diagram and a linear discriminant analysis LDA projection diagram are adopted to effectively distinguish the processed product from the raw product.
6. A pomegranate rind processing method using the pomegranate rind processing quality control method according to any one of claims 1 to 5, wherein the processing temperature of the pomegranate rind processing method is 330 ℃, and the processing time is 16 min.
7. A pomegranate rind prepared by the pomegranate rind processing method of claim 1.
8. An antidiarrheal drug with astringents made from the pomegranate rind of claim 6.
9. A hemostatic drug made from the pomegranate rind of claim 6.
10. An insect repellent made from the pomegranate rind of claim 6.
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| CN117388187A (en) * | 2023-11-09 | 2024-01-12 | 山东省中医药研究院 | Method for calculating content of active ingredients of common cephalanoplos herb charcoal based on electronic eye chromaticity identification technology and application |
| CN118657258A (en) * | 2024-08-20 | 2024-09-17 | 张家港市绿色中药饮片有限公司 | Optimization method and system for stir-frying process of traditional Chinese medicine decoction pieces |
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| CN117388187A (en) * | 2023-11-09 | 2024-01-12 | 山东省中医药研究院 | Method for calculating content of active ingredients of common cephalanoplos herb charcoal based on electronic eye chromaticity identification technology and application |
| CN118657258A (en) * | 2024-08-20 | 2024-09-17 | 张家港市绿色中药饮片有限公司 | Optimization method and system for stir-frying process of traditional Chinese medicine decoction pieces |
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