CN117316308A - Extraction process for optimizing phyllanthus emblica by combining G1-entropy weight analysis with response surface method - Google Patents
Extraction process for optimizing phyllanthus emblica by combining G1-entropy weight analysis with response surface method Download PDFInfo
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- CN117316308A CN117316308A CN202311143767.5A CN202311143767A CN117316308A CN 117316308 A CN117316308 A CN 117316308A CN 202311143767 A CN202311143767 A CN 202311143767A CN 117316308 A CN117316308 A CN 117316308A
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- phyllanthus emblica
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- ethanol
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- 238000000605 extraction Methods 0.000 title claims abstract description 83
- 235000015489 Emblica officinalis Nutrition 0.000 title claims abstract description 79
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- 240000009120 Phyllanthus emblica Species 0.000 title claims abstract 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 127
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- 244000119298 Emblica officinalis Species 0.000 claims description 64
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 37
- 230000001419 dependent effect Effects 0.000 claims description 28
- 238000011156 evaluation Methods 0.000 claims description 26
- AFSDNFLWKVMVRB-UHFFFAOYSA-N Ellagic acid Chemical compound OC1=C(O)C(OC2=O)=C3C4=C2C=C(O)C(O)=C4OC(=O)C3=C1 AFSDNFLWKVMVRB-UHFFFAOYSA-N 0.000 claims description 18
- 235000004515 gallic acid Nutrition 0.000 claims description 18
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- OHDRQQURAXLVGJ-HLVWOLMTSA-N azane;(2e)-3-ethyl-2-[(e)-(3-ethyl-6-sulfo-1,3-benzothiazol-2-ylidene)hydrazinylidene]-1,3-benzothiazole-6-sulfonic acid Chemical compound [NH4+].[NH4+].S/1C2=CC(S([O-])(=O)=O)=CC=C2N(CC)C\1=N/N=C1/SC2=CC(S([O-])(=O)=O)=CC=C2N1CC OHDRQQURAXLVGJ-HLVWOLMTSA-N 0.000 claims description 12
- TUSDEZXZIZRFGC-XIGLUPEJSA-N corilagin Chemical compound O([C@H]1[C@H](O)[C@H]2OC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC[C@@H](O1)[C@H]2O)C(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-XIGLUPEJSA-N 0.000 claims description 12
- -1 iron ion Chemical class 0.000 claims description 12
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- 229920002786 Corilagin Polymers 0.000 claims description 11
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- ATJXMQHAMYVHRX-CPCISQLKSA-N Ellagic acid Natural products OC1=C(O)[C@H]2OC(=O)c3cc(O)c(O)c4OC(=O)C(=C1)[C@H]2c34 ATJXMQHAMYVHRX-CPCISQLKSA-N 0.000 claims description 11
- CPWYQGWOJMNXGJ-UHFFFAOYSA-N corilagin Natural products OC1C2COC(=O)c3c(O)c(O)c(O)c(O)c3c4c(O)c(O)c(O)c(O)c4C(=O)OC1C(O)C(OC(=O)c5cc(O)c(O)c(O)c5)O2 CPWYQGWOJMNXGJ-UHFFFAOYSA-N 0.000 claims description 11
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- FAARLWTXUUQFSN-UHFFFAOYSA-N methylellagic acid Natural products O1C(=O)C2=CC(O)=C(O)C3=C2C2=C1C(OC)=C(O)C=C2C(=O)O3 FAARLWTXUUQFSN-UHFFFAOYSA-N 0.000 claims description 11
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- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical group [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 claims description 6
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- QKUSRAKPUWQSJS-UHFFFAOYSA-N diazanium 3-ethyl-2H-1,3-benzothiazole-6-sulfonate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)C1=CC=C2N(CC)CSC2=C1.[O-]S(=O)(=O)C1=CC=C2N(CC)CSC2=C1 QKUSRAKPUWQSJS-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/06—Peri-condensed systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- C—CHEMISTRY; METALLURGY
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Abstract
The invention belongs to the technical field of plant extraction, and particularly relates to an extraction process for optimizing phyllanthus emblica by combining G1-entropy weight analysis with a response surface method. The invention utilizes the G1-entropy weight combination weighting method to comprehensively score the total phenol extraction amount, the tannin content, the dry extract rate, the target component content, the antioxidant activity and the glycosylation resisting activity of the phyllanthus emblica on the basis of single factors, optimizes the phyllanthus emblica extraction process by combining a response surface, obtains the optimal process conditions of 56% of ethanol concentration, 8mL/G of volume-mass ratio of ethanol to phyllanthus emblica and 100min of extraction time, and obtains the comprehensive score of 92.03 under the condition that the deviation from model prediction is smaller, thus indicating that the extraction process is reasonable and feasible. In addition, the invention can provide reference for digital extraction of the phyllanthus emblica and theoretical basis for widening the market of the phyllanthus emblica and applying the phyllanthus emblica to production and development of industries such as health preservation, cosmetics and the like.
Description
Technical Field
The invention belongs to the technical field of plant extraction. More particularly, the extraction process of phyllanthus emblica is optimized by combining G1-entropy weight analysis with a response surface method.
Background
Emblic leafflower fruit (Phyllanthus emblica L.) is a dried mature fruit of Euphorbiaceae plant Phyllanthus emblica, also known as African Murraya, fructus Phyllanthi, fructus Canarii albi, and fructus Phyllanthi etc., which is widely distributed in India, nepal, malaysia, china etc., and in Guangdong, guangxi, fujian, yunnan, sichuan etc. places in China.
The emblic leafflower fruit contains various chemical components, mainly comprises tannins, phenolic acids, flavones, terpenes, sterols, fatty acids, amino acids, polysaccharides, vitamins, trace elements and the like, wherein the tannins and the phenolic acids are main active components. Modern researches show that the phyllanthus emblica has certain pharmacological activity in the aspects of antioxidation, anti-tumor, antibiosis, anti-inflammatory, pain relieving, blood sugar reducing, atherosclerosis resisting, liver protecting and the like, and gallic acid and derivatives thereof, namely ellagic acid, myrobalan acid and corilagin, can be used as candidate components of phyllanthus emblica quality markers. The phyllanthus emblica has rich nutritional value and medicinal value, and is widely applied to the fields of food, beverage, cosmetics, medical care and the like in recent years.
At present, the extraction process of phyllanthus emblica is mainly examined by taking the content of total phenols, polysaccharides or main components as indexes, and the extraction process is focused on chemical components (Wei Caicai, li Xueli, hao Lei and the like). However, most of the phyllanthus emblica extraction methods are not combined with related functional activities, evaluation indexes are not comprehensive, and a multi-index evaluation method is needed to optimize the phyllanthus emblica extraction process.
Disclosure of Invention
The invention aims to overcome the defect and the defect that the evaluation index of the existing phyllanthus emblica extraction process is not comprehensive, and provides a G1-entropy weight analysis combined with a response surface method to optimize the phyllanthus emblica extraction process, and the optimal parameters of the phyllanthus emblica extraction process are screened out.
The above object of the present invention is achieved by the following technical scheme:
the extraction process of the phyllanthus emblica is optimized by combining G1-entropy weight analysis with a response surface method, and specifically comprises the following steps of:
s1, adopting an ethanol reflux extraction mode, selecting ethanol concentration and ethanol: carrying out a single factor experiment on the mass-to-volume ratio and the extraction time of the phyllanthus emblica, and taking the total phenol content as an evaluation index;
s2, on the basis of a single factor experiment, selecting the volume-mass ratio of ethanol to phyllanthus emblica and the extraction time as independent variables, taking the total phenol extraction amount, the tannin content, the dry extract rate, the active ingredient content, the antioxidant activity and the anti-glycosylation activity as dependent variable indexes, taking the comprehensive score Y of each dependent variable index as an evaluation index, adopting a three-factor three-level response surface method data analysis method, and optimizing the phyllanthus emblica extraction process;
s3, determining an index importance sequence by adopting a G1 subjective weighting method and an entropy weighting method objective weighting method, and carrying out combined weighting on the indexes;
s4, obtaining a comprehensive score Y according to the combination weighting, analyzing by using Design-Expert software, and drawing a 3D graph and a 2D contour map of the interaction result of the response surface of each factor to obtain the optimal extraction process of the phyllanthus emblica.
Total polyphenols were chosen as a simple and scientific index, and we therefore selected them as relevant index for single factor investigation. According to the related research report, the more the polyphenol content is, the stronger the antioxidant activity is, the polyphenol also has an inhibiting effect on advanced glycosylation end products (advanced glycation end products, AGEs), and the stronger the anti-glycosylation activity is. Therefore, the total polyphenol can be used for initially screening the range of extraction factors and laying a foundation for the subsequent response surface investigation.
Further, in step S2, the active ingredients are gallic acid, corilagin, chebulic acid and ellagic acid.
Further, in step S2, the antioxidant activity is DPPH radical scavenging rate, ABTS + & radical scavenging rate, OH radical scavenging rate and iron ion reducing ability.
Further, in step S2, the anti-glycosylation activity is the inhibition rate of BSA-Flu to AGEs and the inhibition rate of BSA-MGO to AGEs.
The G1 subjective weighting method is a subjective evaluation method which improves the AHP method and has high calculation speed and does not need consistency test, and comprises the following specific steps:
firstly, determining the sequence relation of evaluation indexes, sorting according to the importance degree of each evaluation index in the experiment, and marking as y 1 ＞y 2 ＞…＞y m The order of 13 evaluation indexes determined by the G1 method was in turn the total phenol extraction amount (y 1 ) Content of tannins (y 2 ) Dry paste rate (y) 3 ) Gallic acid (y) 4 ) =corilagin (y) 5 ) =myrobalanLi Leic acid (y) 6 ) Ellagic acid (y) 7 ) Radical scavenging by DPPH (y 8 )＝ABTS +· Radical scavenging rate (y) 9 ) =.oh radical scavenging rate (y 10 ) =iron ion reducing ability (y 11 ) =bsa-Flu inhibition of AGEs (y 12 ) =bsa-MGO inhibition of AGEs (y 13 )；
Next, determining the relative importance between adjacent indexes according to the following formula, wherein y k-1 And y is k For the evaluation index, the ratio of the importance degree between the two is r k ；
Preferably, the weight evaluation scale r 2 ＝1，r 3 ＝1.1，r 4 ＝r 5 ＝r 6 ＝r 7 ＝1.2，r 8 ＝r 9 ＝r 10 ＝r 11 ＝r 12 ＝r 13 ＝1.3。
Further, in step S3, the G1 subjective weighting method calculates each index weight w k The calculation formula is as follows:
wherein w is k-1 ＝r k w k The method comprises the steps of carrying out a first treatment on the surface of the k represents different dependent variable indexes; k=m, m-1 … …,2; m is the index number of dependent variables; r is (r) i Is the ratio of the relative importance between adjacent indexes.
The entropy weight method is an objective weight method for determining the weight of each index according to the information quantity provided by the original data of each index, can avoid the deviation of human factors, improve the accuracy and enhance the objectivity, and can better explain the obtained result, and mainly comprises the following calculation steps:
step 1: data normalization:
Yij＝(xij－min{xij})/(max{xij}－min{xij})
step 2: normalization of normalized data:
step 3: solving the information entropy of each index, and determining the weight of each index:
e is a dependent variable index entropy value; n is the index number of the dependent variables; j is 1-n and represents different dependent variable indexes.
Further, in step S3, the calculation formula of the combined weighting is:
wherein, the subjective weight obtained by the G1 method is expressed as w 1 The objective weight obtained by the entropy weight method is expressed as w 2 The method comprises the steps of carrying out a first treatment on the surface of the j is 1-m and represents different dependent variable indexes; m is the index number of the dependent variable.
Further, in step S4, the calculation formula of the composite score Y is as follows:
wherein y is j Data results which are dependent variable indexes; y is j max Representing the maximum value of a certain index in all group detection; j is 1-m and represents different dependent variable indexes; m is the index number of the dependent variable.
Further, in the step S1, the concentration of the ethanol is 20% -100%; the volume-mass ratio of the ethanol to the phyllanthus emblica is 4-12 mL/g; the extraction time is 30-150 min.
Preferably, in the step S1, the concentration of the ethanol is 56%, the volume-mass ratio of the ethanol to the phyllanthus emblica is 8mL/g, and the extraction time is 100min; under the condition of the extraction process, the comprehensive score is 92.03, the difference from the predicted value (94.91) is 3.03 percent, the RSD is less than 5 percent, and the extraction process is reasonably feasible.
The invention has the following beneficial effects:
the invention adopts an ethanol reflux extraction mode, combines chemical component content indexes with biological activity indexes by a digital technology on the basis of single factors, and utilizes a G1-entropy weight combination weighting method to extract total phenols of phyllanthus emblica, tannin content, dry extract rate, target component (gallic acid, corilagin, myrobalan acid and ellagic acid) content and antioxidant activity (DPPH free radical clearance rate, ABTS) +· The free radical clearance, OH free radical clearance, iron ion reducing capability) and the anti-glycosylation activity (the AGEs inhibition rate by BSA-Flu and the AGEs inhibition rate by BSA-MGO) are comprehensively scored, and the extraction condition of the phyllanthus emblica is optimized by combining a response surface method, wherein the obtained optimal process condition is that the ethanol concentration is 56%, the feed-liquid ratio is 1:8, and the extraction time is 100min. Compared with the prior art, the method has the advantages that the experimental system is perfect and reliable, the extraction process is scientific and reasonable, the cost is low, and compared with the prior art for extracting the phyllanthus emblica, the method only has chemical component indexes, and the evaluation indexes are incomplete, the biological activity index is increased, so that the phyllanthus emblica can be further explained to have certain development potential as a raw material of cosmetics and health products. The optimization method can provide reference for digital extraction of the phyllanthus emblica, and simultaneously provides theoretical basis for widening the market of the phyllanthus emblica and applying the phyllanthus emblica to production and development of industries such as health preservation, cosmetics and the like.
Drawings
FIG. 1 is a statistical graph of the effect of ethanol concentration, the volume to mass ratio of ethanol to phyllanthus emblica, and the extraction time on total phenol extraction.
FIG. 2 shows the liquid chromatography (a) of gallic acid, corilagin, chebular acid and ellagic acid standard substances, and the high performance liquid chromatography (b) of gallic acid, corilagin, chebular acid and ellagic acid in the extract of fructus Phyllanthi.
FIG. 3 is a 3D plot and 2D contour plot of response surface interactions for various factors.
Fig. 4 is a diagram of model diagnosis results, in which, (a) is a diagram of predicted composite score and actual composite score response, (b) is a normal distribution diagram of residual error, (c) is a diagram of predicted value and residual error, and (d) is a diagram of residual error and test operation sequence.
Detailed Description
The invention is further illustrated in the following drawings and specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
Reagents and materials used in the following examples are commercially available unless otherwise specified.
(1) Medicinal materials and reagents
Emblic leafflower fruit (produced in Guangdong Chaoshan region); gallic acid control (CAS: 149-91-7, lot number: CHB-M-037, chengdu Ke Loma Biotech Co., ltd.); corilagin reference (CAS: 23094-69-1, lot number: CHB-K-004, chengdu Keloma Biotechnology Co., ltd.); chebular acid control (CAS: 23094-71-5, lot number: CHB-H-114, chengdu Ke Loma Biotechnology Co., ltd.); ellagic acid control (CAS: 476-66-4, lot number: CHB-R-039, chengdu Keloma Biotechnology Co., ltd.); methanol (analytically pure, available from Tianjin far chemical agents Co., ltd.); absolute ethanol (analytically pure, available from Guangdong Guanghua technologies Co., ltd.); anhydrous sodium carbonate (analytically pure, available from the company of the company Tianjin far chemical agents, inc.); 30% hydrogen peroxide (analytically pure, available from guangzhou chemical reagent plant); disodium hydrogen phosphate (analytically pure, available from Jiangsu-strongness chemical Co., ltd.); sodium dihydrogen phosphate (analytically pure, available from Shanghai chemical agents Co., ltd.); PBS pH7.4 buffer (available from gibco, U.S.A.); formic acid (chromatographic purity, available from Tianjin Miou reagent Co.); phosphomolybdic tungstic acid (available from Xiamen sea mark technologies Co., ltd.); acetonitrile (chromatographic purity, available from the company euron barker chemical, sweden); fu Lin Fen, salicylic acid, ferrous sulfate, potassium persulfate, trichloroacetic acid, ferric trichloride, 1-diphenyl-2-trinitro-base-hydrazine (DPPH), 2-diaza-bis (3-ethylbenzothiazole-6-sulfonic acid) diammonium salt (ABTS), all available from Shanghai Milin Biochemical technologies, inc.; potassium ferricyanide (analytically pure, available from Jiangsu-chong chemical Co., ltd.), 40% pyruvaldehyde (MGO) solution (available from German Sigma reagent Co., ltd.), fructose (Fru) (available from Beijing Soy Bao technology Co., ltd.), bovine Serum Albumin (BSA) (available from Guangzhou Ruisha biosciences Co., ltd.).
(2) Instrument for measuring and controlling the intensity of light
TECAN Spark multifunctional microplate detector (switzerland imperial); shimadzu LC-20AT high performance liquid chromatograph (Shimadzu corporation); electrothermal blowing drying oven (Shanghai-constant scientific instruments Co., ltd.).
Example 1 single factor investigation
(1) Drawing gallic acid standard curve
Gallic acid 10mg was weighed, dissolved in distilled water and fixed to a volume of 20mL volumetric flask as a mother liquor (0.5 mg/mL). The standard solution was diluted with water to a concentration of 12.5, 25, 50, 100, 200, 400 μg/mL.
Accurately weighing 10.0g of anhydrous sodium carbonate, dissolving the anhydrous sodium carbonate by distilled water, and fixing the volume to 100mL to obtain 10% Na2CO3 solution.
The Folin-Ciocalteu colorimetric method is slightly modified, 10 mu L of standard solution with different concentrations is sucked into a 96-well plate, 20 mu L of Fu Lin Fen is added, the reaction is carried out for 5min in a dark place, and 170 mu L of 10% Na is added 2 CO 3 The solution is mixed evenly and reacted for 2 hours, and the absorbance value is measured at 765nm by an enzyme-labeled instrument, and meanwhile, the reagent blank is prepared. The concentration gradient (X) and absorbance value (Y) of gallic acid reference substance are used as standard curves.
(2) Testing of different factors
Extracting the phyllanthus emblica polyphenol by adopting a reflux extraction mode under the conditions of different concentrations, different volume-to-mass ratios of ethanol and phyllanthus emblica and different extraction times.
Effect of ethanol concentration on total polyphenol extraction: weighing 20g of phyllanthus emblica, respectively adding ethanol solution with volume concentration of 20%, 40%, 60%, 80% and 100% into the phyllanthus emblica at volume-mass ratio of 8mL/g, refluxing and heating to boiling point of ethanol, recording 60min when a condenser tube starts dripping liquid drops, keeping the temperature constant, and determining the ethanol concentration range according to the total polyphenol extraction amount of phyllanthus emblica.
Influence of the volume-mass ratio of ethanol to phyllanthus emblica on total polyphenol extraction: weighing 20g of phyllanthus emblica, adding 60% ethanol solution according to the volume-mass ratio of 4,6,8,10 and 12mL/g of the ethanol to the phyllanthus emblica, refluxing and heating until the ethanol reaches the boiling point, recording for 60 minutes when a condensing tube starts dripping liquid drops, keeping the temperature constant, and determining the volume-mass ratio range of the ethanol to the phyllanthus emblica according to the total polyphenol extraction amount of the phyllanthus emblica.
Effect of extraction time on total polyphenol extraction: weighing 20g of phyllanthus emblica, adding 60% ethanol solution at a volume-mass ratio of 8mL/g of ethanol to phyllanthus emblica, refluxing and heating to boiling point, and recording 30min, 60min, 90min, 120min and 150min when a condenser tube starts dripping liquid drops, and determining the extraction time range according to the total polyphenol extraction amount of phyllanthus emblica.
(3) Determination of total Polyphenol content
Adding 10 μl of the extract (diluted with appropriate multiple) into 96-well plate, adding 20 μl of Fu Lin Fen, standing in dark place for reaction for 5min, and adding 170 μl of 10% Na 2 CO 3 The solution was mixed well and reacted for 2 hours, and the absorbance was measured at 765nm with an enzyme-labeled instrument. And calculating the total polyphenol extraction amount under different conditions according to a standard curve.
Wherein: c-polyphenol concentration, mg/mL; v-volume of extract, mL; n-dilution factor; m is the mass of phyllanthus emblica, g.
2. Experimental results
Total polyphenols were chosen as a simple and scientific index, and we therefore selected them as relevant index for single factor investigation. According to the related research report, the more the polyphenol content is, the stronger the antioxidant activity is, the polyphenol also has an inhibiting effect on advanced glycosylation end products (advanced glycation end products, AGEs), and the stronger the anti-glycosylation activity is. Therefore, the total polyphenol can be used for initially screening the range of extraction factors and laying a foundation for the subsequent response surface investigation.
Gallic acid standard curve regression equation y=0.0023x+0.0772, r 2 =0.9998. As can be seen from fig. 1, as the ethanol concentration increases, the total phenol extraction amount of emblic leafflower fruit increases and then decreases, and when the ethanol concentration is 60%, the total phenol extraction amount reaches the maximum, so that three concentrations of 40%, 60% and 80% are selected as the treatment levels for response surface test optimization. As the volume-to-mass ratio of ethanol to emblic leafflower fruit increases, the total phenol extraction of emblic leafflower fruit gradually increases, tends to peak at 8mL/g, continues to increase the volume-to-mass ratio of ethanol to emblic leafflower fruit (i.e., the feed liquid ratio mL/g as shown in fig. 1), the total phenol extraction increases slowly, and too much solvent is detrimental to recovery, and can increase residual dissolution and production energy consumption. Considering comprehensively, the volume-mass ratio of the ethanol to the phyllanthus emblica is 6,8 and 10mL/g for subsequent experiments. The extraction time is within 30-90 min, the total phenol extraction amount is continuously increased, but when the extraction time is>At 90min, the total phenol extraction amount is slightly reduced, and if the extraction time is too long, the condensation of polyphenol substances or the oxidation of the polyphenol substances by oxygen can be possibly caused, so that the reaction is economical and reasonable for extracting the total polyphenol at about 90 min.
Example 2 response surface optimization and Combined weighting evaluation
1. Experimental method
Based on single factor experimental results, the volume-mass ratio (B) of ethanol concentration (A), ethanol and phyllanthus emblica and the extraction time (C) are selected as independent variables, and the total phenol extraction amount, the tannin content, the dry extract rate, the target component content (gallic acid, corilagin, chebular acid and ellagic acid), the antioxidant activity (DPPH free radical clearance, ABTS+ & free radical clearance, OH free radical clearance and iron ion reducing capability), the anti-glycosylation activity (BSA-Flu inhibition rate to AGEs and BSA-MGO inhibition rate to AGEs) are selected as dependent variables by adopting a three-factor three-level response surface method data analysis method, and the phyllanthus emblica extraction process is optimized, and the factors and the levels are shown in Table 1. The response surface Design using Design-Expert 13 software is shown in table 2.
TABLE 1Box-Behnken experiment design factors and levels
TABLE 2 response surface Experimental design
(1) Determination of total Polyphenol content
And (3) measuring the total phenol content of each group of extracting solutions under the extracting conditions designed according to Design-Expert 13 software, and calculating the total polyphenol extracting amount under different conditions according to a standard curve.
(2) Determination of tannin content
Reference is made to the "content determination method of tannin" 2202 in 2020 edition of Chinese pharmacopoeia "with slight modification.
Preparation of control solution
Precisely weighing gallic acid reference substance 10mg, placing into 200mL brown measuring flask, adding water for dissolving and diluting to scale, and preparing into 0.05mg/mL reference substance solution.
Preparation of a Standard Curve
Precisely measuring 0.5mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL, 6.0mL, 7.0mL and 8.0mL of the reference substance solution, respectively placing the reference substance solution into 25mL brown measuring flasks, respectively adding 1mL of the phosphomolybdic tungstic acid test solution, respectively adding 11.5mL, 11mL, 10mL, 9mL, 8mL, 7mL, 6mL, 5mL and 4mL of water, diluting to a scale with 29% sodium carbonate solution, shaking uniformly, standing for 30 minutes, taking the corresponding reagent as a blank, measuring absorbance at a wavelength of 760nm according to ultraviolet-visible spectrophotometry (general rule 0401), taking absorbance as a ordinate and taking concentration as a abscissa, and drawing a standard curve.
Total phenol amount: precisely measuring each group of extracting solutions, diluting by proper times, taking 2mL of each group of diluting solutions, placing into a 25mL brown measuring flask, adding 10mL of water from the step of adding 1mL of phosphomolybdic tungstic acid test solution according to the method under the preparation item of a standard curve, measuring absorbance according to the method, reading the amount (mg) of gallic acid in the test solution from the standard curve, and calculating to obtain the product.
Amount of non-adsorbed polyphenols: precisely measuring each group of extracting solutions, diluting by proper times, taking 25mL of each group of diluting solutions, adding into a 100mL conical flask with a plug which is filled with 0.6g of casein, sealing, preserving heat for 1 hour in a water bath at 30 ℃, shaking constantly, taking out, cooling, shaking uniformly, filtering, discarding the primary filtrate, precisely measuring 2mL of the secondary filtrate, placing into a 25mL brown measuring flask, adding 10mL of water from the step of adding 1mL of phosphomolybdic tungstic acid test solution according to the method under the preparation of a standard curve, measuring absorbance according to the law, reading the amount (mg) of gallic acid in the test solution from the standard curve, and calculating to obtain the product. And during measurement, simultaneously performing a casein adsorption blank test, and calculating a blank deduction value.
The content of tannins was calculated as follows:
tannin content = total phenol amount-amount of non-adsorbed polyphenols
(3) Dry paste rate determination
Precisely sucking 20mL of each group of extracting solution, placing into an evaporation dish with constant mass, evaporating in water bath, drying at 105 ℃ for 3h, taking out, cooling in a dryer for 30min, precisely weighing the mass, and calculating the dry paste rate.
Wherein: m-dry mass, g; v-total volume of extract, mL; m is crude drug mass, g.
(4) Determination of the content of target Components
Chromatographic conditions: the column was an Ecosil C18 column (250 mm. Times.4.6 mm,5 μm); mobile phase is 0.1% formic acid water (A) -acetonitrile (B); gradient elution: 0-10min,5% -10% B;10-15min,10% -15% of B;15-20min,15% -18% of B;20-30min,18% -23% of B;30-40min,23% -30% of B;40-50min,30% -60% of B;50-55min,60% -5% of B;55-60min,5% B; flow rate: 1mL/min; detection wavelength: 270nm; column temperature: 30 ℃; sample injection amount: 10 mu L.
Preparation of a mixed control solution: precisely weighing gallic acid, corilagin, chebular acid and ellagic acid reference substances, and adding methanol to dissolve to obtain mixed reference substance solutions with concentration of 1.068, 1.017, 1.095 and 1.022 mg/mL. The mixed reference substance solution is taken in proper amount, and diluted with methanol to the concentration of 0.267, 0.254, 0.274 and 0.256mg/mL.
Preparation of test solution: and diluting each group of extracting solutions under the extraction condition according to software design by a proper multiple, and filtering by a microporous filter membrane with the thickness of 0.22 mu m to obtain a sample solution.
Linear relation investigation: the mixed control solutions (0.267, 0.254, 0.274, 0.256 mg/mL) were sampled at 1,2,4,6,8,10,12. Mu.L and assayed as described above under chromatographic conditions. And drawing a standard curve by taking the sample injection amount as an abscissa and the peak area as an ordinate.
Precision test: the mixed reference solution was measured under the above chromatographic conditions, the peak area of each target component was recorded 6 times successively, and the Relative Standard Deviation (RSD) value was calculated.
Stability test: sample solutions of design scheme test number 1 are taken, 10 mu L of sample is injected for 0, 2,4, 8, 12 and 24 hours after sample preparation, measurement is carried out, the variation condition of peak areas of all components is examined, and the peak area RSD value is calculated.
Repeatability test: taking the design scheme test number 1 extracting solution, preparing 6 parts of sample solution in parallel, sampling according to the chromatographic conditions, measuring the content of 4 target components and calculating the RSD value.
Sample recovery rate test: sample solution 1 of test number 1 of known content was precisely measured in 6 parts and control solution approximately equal to the sample amount was precisely added, respectively. The chromatographic measurement was performed, and the sample recovery rate and RSD value of each component were calculated.
Sample measurement: taking each sample solution, sampling according to chromatographic conditions, and calculating the content of the target component according to an external standard method by determining the peak area of the sample solution and a linear equation of a reference substance.
(5) Antioxidant Activity assay
Determination of DPPH radical scavenging Rate
Taking 50 mu L of sample solution diluted by proper times in each group under the design scheme, adding 150 mu L of 0.2mmol/L DPPH solution, uniformly mixing, carrying out light-shielding reaction for 30min, measuring absorbance (Ai) at 517nm, using absolute ethyl alcohol to replace the DPPH solution, measuring absorbance (Aj), using the same volume of absolute ethyl alcohol to replace the sample solution, and measuring absorbance (A0).
ABTS +· Determination of radical scavenging Rate
Mixing the solution of 7mmol/L ABTS with the solution of 2.45mmol/L potassium persulfate in equal volume, reacting for 12-16 h at the dark room temperature, and diluting with Phosphate Buffer Solution (PBS) of pH7.4 before use to enable the absorbance value to reach 0.70+/-0.02 at 734nm wavelength, thus obtaining the ABTS working solution. After the sample solutions of each group were properly diluted, 50. Mu.L of each group was aspirated into a 96-well plate, 150. Mu.L of an ABTS working solution was added, the mixture was allowed to stand at room temperature in a dark place for 6 minutes, the absorbance value (Ai) was measured at a wavelength of 734nm, the control absorbance (Aj) was measured by using a PBS buffer instead of the ABTS working solution, and the blank absorbance value (A0) was measured by using ultrapure water instead of the sample.
Determination of OH radical scavenging Rate
Adding salicylic acid 9mmol/L and FeSO 9mmol/L into 2mL of each group of extracting solution by salicylic acid titration 4 1mL each, and finally 1mL of H was added at a concentration of 9.8mmol/L 2 O 2 Performing color reaction, mixing, shaking, performing water bath reaction at 37deg.C for 30min, collecting 200 μl of the reaction solution, measuring absorbance (Ai) at 510nm wavelength, and replacing H with ultrapure water 2 O 2 The solution was measured for a control absorbance (Aj) and the blank absorbance was (A0).
Iron ion reducing ability
The method is characterized by adopting a potassium ferricyanide reduction method. Diluting each group with 1mL of the extractive solution with proper ratio, adding pH6.6 phosphate buffer solution and 1% K 3 [Fe(CN) 6 ]2.5mL each of the solutions was subjected to a water bath at 50deg.C for 20min, followed by addition of 2.5mL of 10% trichloroacetic acid solution, centrifugation at 4000r/min for 10min, taking 2.5mL of supernatant, and adding 2.5mL of deionized water and 2.5mL of 0.1% FeCl 3 Mixing the solutions, standing for 10min, and collecting 200 μl of the reaction solutionAbsorbance was measured at 700 nm. During this reaction, fe 3+ Can be reduced into Fe by antioxidant substances 2+ And then has strong absorption at 700nm wavelength. Therefore, the larger the absorbance, the stronger the sample reducing ability, and the stronger the antioxidant ability.
(6) Anti-glycosylation activity assay
A bovine serum albumin-fructose glycosylation reaction system (BSA-Fru) and a bovine serum albumin-acetone aldolization reaction system (BSA-MGO) were established. In the BSA-Fru model, 1g of BSA and 45.05g of fructose were dissolved in 100mL of PBS to give a control solution containing 10mg/mL BSA and 2.5M fructose. In the BSA-MGO model, 0.1g BSA and 90.9. Mu.L MGO (40% solution) were dissolved in 100mL PBS to give 1mg/mL BSA and 5mM MGO control solution. 2.25mL of the model solution was incubated at 37℃for 5d, and 0.75mL of each set of extracts in phosphate buffer (pH 7.4) was added. The same volume of model solution was also used as a control. The test solution was added with a diabody to ensure aseptic conditions. Determining fluorescence value of glycosylated end products (AGEs) at excitation wavelength of 370nm and emission wavelength of 440nm, and calculating inhibition rate of phyllanthus emblica polyphenol on AGEs according to a formula:
wherein: f (F) e -testing the fluorescence intensity of the solution; f (F) c Model fluorescence intensity.
(7) Comprehensive weighting of evaluation indexes
Subjective weighting by G1 method
The G1 method is a subjective evaluation method which improves the AHP method and has high calculation speed and does not need consistency test, and the method comprises the following specific steps.
Firstly, determining the sequence relation of evaluation indexes, sorting according to the importance degree of each evaluation index in the experiment, and marking as y 1 ＞y 2 ＞…＞y m 。
And secondly, determining the relative importance degree between adjacent indexes. According to the formula, wherein y k-1 And y is k For the evaluation index, the importance degree ratio rk between the two is calculated.
Finally, calculating the weight coefficient w of each index k 。
Wherein: w (w) k-1 ＝r k w k K=m, m-1 … …,2 (m is the number of evaluation indexes).
Objective weighting by entropy weighting method
The entropy weighting method is an objective weighting method for determining the weights of the indexes according to the information quantity provided by the original data of the indexes, so that deviation of human factors can be avoided, the accuracy is improved, the objectivity is enhanced, and the obtained result can be better explained.
Step 1: data normalization:
Yij＝(xij－min{xij})/(max{xij}－min{xij})
step 2: normalization of normalized data:
step 3: solving the information entropy of each index, and determining the weight of each index:
determination of combining weights and composite scores
The subjective weight obtained by the G1 method is w 1 The objective weight obtained by the entropy weight method is w 2 The combined weight calculation formula is as follows:
further obtaining an index comprehensive score Y of each test condition:
2. experimental results
The HPLC methodology investigation result shows that the method has good linear relation, good instrument precision, certain stability of the test sample solution, good repeatability and high accuracy, and can be used for detecting the contents of four target components in phyllanthus emblica. The high performance liquid chromatogram of the fructus Phyllanthi extract is shown in figure 2.
Table 34 results of linear relationship investigation of target components
Table 44 results of precision, stability and reproducibility of target ingredients
Table 54 results of sample recovery of target components
Response surface analysis comprehensive evaluation: the evaluation index weight value obtained by subjective weighting according to the G1 method is subjective and reasonable, but the corresponding subjective randomness is larger, and objective change cannot be reflected; according to objective weighting of the entropy weight method, extensive research based on the original data is objective and reasonable, but expert experience is ignored. Therefore, after the subjective weight value and the objective weight value are respectively determined, the subjective weight value and the objective weight value are combined, and the method not only can consider the expertise and experience of an expert, but also can explain the related information of the actual situation, so that the evaluation result is more scientific and reasonable. The combined weight values of the evaluation indexes are shown in table 6, and the response surface results are shown in table 7.
Table 6 extraction process evaluation index weight values
Model building and analysis of variance the Design-Expert 13 software was used to perform multiple regression fitting and significance testing on the table 7 data, and the results are shown in table 8. The quadratic polynomial regression equation between factors A, B, C and Y, y=93.49-4.05a+1.97b+4.24c-2.86ab+2.71ac+1.28bc-8.64A2-7.88B2-5.11C2. Analysis of variance of the model shows that the model is extremely remarkable (P is less than 0.01), the mismatching term F=0.7437, P= 0.5794 is more than 0.05, the mismatching is not remarkable, and R 2 ＝0.9718，Radj 2 ＝0.9356，Rpred 2 ＝0.8103，Radj 2 And Rred 2 The difference is smaller than 0.2,Adeq Precision (signal-to-noise ratio) 14.8779, is far larger than 4, and the coefficient of variation CV is smaller than 10%, so that the fitting degree and the reliability of the regression equation are high, and the experimental model can be used for analysis and prediction. The F value result shows that the influence degree of each factor on the phyllanthus emblica extraction process is as follows: extraction time (C) > ethanol concentration (A) > volume to mass ratio (B).
Interaction impact significance analysis: and analyzing interaction of all factors according to the three-dimensional response curved surface diagram and the contour diagram of the response surface obtained by the regression model. The effect of the two is observed with a slope, the higher the slope, the more pronounced the interaction of the two is demonstrated, and the more pronounced the interaction is. The interaction of the two factors can be obtained through the contour lines, the contour lines are elliptical, the interaction of the 2 factors is obvious, and the contour lines are circular, the interaction of the 2 factors is not obvious. As can be seen from fig. 3, the factors of the ratio of ethanol concentration to volume mass, ethanol concentration and extraction time are in an elliptical shape, so the influence on the extraction process is significant; the interaction between the volume and mass ratio and the extraction time is not obvious, so the influence on the extraction process is not obvious.
Model diagnosis: the diagnostic chart (fig. 4) shows a high correlation between the predicted outcome and the experimental outcome. The comparison graph of the predicted value and the actual value shows that the correlation between the predicted value and the actual value is higher, and the difference is smaller. The response residual map is normally distributed. The built secondary model can accurately predict experimental data.
TABLE 7Box-Behnken response surface design experiment scheme and results
TABLE 8 multiple regression model analysis of variance
Note that: * Extremely significant (P < 0.01), significant (P < 0.05)
Example 3 extraction Process validation
1. Experimental method
The optimal extraction process of phyllanthus emblica selected according to Design-Expert 13 software analysis is that the ethanol concentration is 55.880%, the volume-mass ratio is 8.387 (mL/g), and the time is 101.496min (in the embodiment 2, each index is required to be optimized in the experiment, the comprehensive score is highest, the corresponding level of the highest point of the curved surface is selected as the optimal experimental parameter, and the optimal extraction process is obtained by using Design-Expert 13 software). In view of the operability of the test, the process parameters were adjusted to an ethanol concentration of 56%, a volume to mass ratio of 8 (mL/g), and a time of 100min.
2. Experimental results
Under this condition, the results of 3 parallel experiments are shown in Table 9. The average value of the comprehensive scores is 92.03, the average value is 3.03 percent different from the predicted value (94.91), the average value is less than 5 percent, and the RSD is 1.61 percent, so that the extraction process is reasonable and feasible, has strong operability and practical value.
Table 9 results of process verification
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The extraction process for optimizing phyllanthus emblica by combining G1-entropy weight analysis with a response surface method is characterized by comprising the following steps of:
s1, extracting phyllanthus emblica by adopting an ethanol reflux extraction mode, selecting the ethanol concentration, the volume-mass ratio of the ethanol to the phyllanthus emblica, and carrying out a single factor experiment on the extraction time, wherein the total phenol content is used as an evaluation index;
s2, on the basis of a single factor experiment, selecting the volume-mass ratio of ethanol to phyllanthus emblica and the extraction time as independent variables, taking the total phenol extraction amount, the tannin content, the dry extract rate, the active ingredient content, the antioxidant activity and the anti-glycosylation activity as dependent variable indexes, taking the comprehensive score Y of each dependent variable index as an evaluation index, adopting a three-factor three-level response surface method data analysis method, and optimizing the extraction process of the phyllanthus emblica;
s3, determining the importance sequence of the dependent variable indexes by adopting a G1 subjective weighting method and an entropy weighting method objective weighting method, and carrying out combined weighting on the indexes;
s4, obtaining a comprehensive score Y according to the combination weighting, analyzing by using Design-Expert software, and drawing a 3D graph and a 2D contour map of the interaction result of the response surface of each factor to obtain the optimal extraction process of the phyllanthus emblica.
2. The process according to claim 1, wherein in step S2, the active ingredients are gallic acid, corilagin, chebulic acid and ellagic acid.
3. The process for extracting fructus Phyllanthi according to claim 1, wherein in step S2, the antioxidant activity is DPPH free radical scavenging rate, ABTS +· Radical scavenging rate, OH radical scavenging rate and iron ion reducing ability.
4. The process for extracting emblic leafflower fruit according to claim 1, wherein in step S2, the anti-glycosylation activity is a BSA-Flu inhibition rate against AGEs and a BSA-MGO inhibition rate against AGEs.
5. The process for extracting emblic leafflower fruit according to claim 1, wherein in step S3, the subjective weighting method of G1 calculates each index weight w k The calculation formula is as follows:
wherein w is k-1 ＝r k w k The method comprises the steps of carrying out a first treatment on the surface of the k represents different dependent variable indexes; k=m, m-1 … …,2; m is the index number of dependent variables; r is (r) i Is the ratio of the relative importance between adjacent indexes.
6. The process for extracting emblic leafflower fruit according to claim 1, wherein in step S3, the entropy weighting method objectively weights each index weight w j The calculation formula is as follows:
e is a dependent variable index entropy value; n is the index number of the dependent variables; j is 1-n and represents different dependent variable indexes.
7. The process for extracting emblic leafflower fruit according to claim 1, wherein in step S3, the calculation formula of the combination weighting is:
wherein in step S3 of claim 1, the subjective weight obtained by the G1 subjective weighting method represents w 1 The objective weight obtained by the entropy weight objective weighting method is expressed as w 2 The method comprises the steps of carrying out a first treatment on the surface of the j is 1-m and represents different dependent variable indexes; m is the index number of the dependent variable.
8. The process for extracting emblic leafflower fruit according to claim 1, wherein in step S4, the comprehensive score Y is calculated as follows:
wherein y is j Data results which are dependent variable indexes; y is j max Representing the maximum value of a certain dependent variable index in all group detection; j is 1-m and represents different dependent variable indexes; m is the index number of the dependent variable.
9. The process according to claim 1, wherein in step S3, the index importance order of the dependent variables is total phenol extraction (y 1 ) Content of tannins (y 2 ) Dry paste rate (y) 3 ) Gallic acid (y) 4 ) =corilagin (y) 5 ) =myrtillus acid (y) 6 ) Ellagic acid (y) 7 ) Radical scavenging by DPPH (y 8 )＝ABTS +· Radical scavenging rate (y) 9 ) =.oh radical scavenging rate (y 10 ) =iron ion reducing ability (y 11 ) =bsa-Flu inhibition of AGEs (y 12 ) =bsa-MGO inhibition of AGEs (y 13 )。
10. The process for extracting emblic leafflower fruit according to claim 1, wherein in step S1, the concentration of ethanol is 20% -100%; the volume-mass ratio of the ethanol to the phyllanthus emblica is 4-12 mL/g; the extraction time is 30-150 min.
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