CN109147894A - A kind of method of Extraction Process of Volatile Oil parameter in the preferred energy-stagnation stomachache of multi objective - Google Patents
A kind of method of Extraction Process of Volatile Oil parameter in the preferred energy-stagnation stomachache of multi objective Download PDFInfo
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 60
- 238000000605 extraction Methods 0.000 title claims abstract description 54
- 206010000087 Abdominal pain upper Diseases 0.000 title description 7
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002791 soaking Methods 0.000 claims abstract description 26
- 238000012360 testing method Methods 0.000 claims abstract description 25
- 238000004458 analytical method Methods 0.000 claims abstract description 20
- RTBLDXVIGWSICW-JMSVASOKSA-N (1R,7R,10R)-4,10,11,11-tetramethyltricyclo[5.3.1.01,5]undec-4-ene Chemical compound C[C@@H]1CC[C@@H]2CC3=C(C)CC[C@]13C2(C)C RTBLDXVIGWSICW-JMSVASOKSA-N 0.000 claims abstract description 16
- 238000013461 design Methods 0.000 claims abstract description 16
- 238000002474 experimental method Methods 0.000 claims abstract description 16
- 229940087305 limonene Drugs 0.000 claims abstract description 15
- 235000001510 limonene Nutrition 0.000 claims abstract description 15
- 235000021419 vinegar Nutrition 0.000 claims abstract description 12
- 239000000052 vinegar Substances 0.000 claims abstract description 12
- YALFFHSIVPCNLF-QPSCCSFWSA-N Cyperolone Chemical compound C1[C@H](C(=C)C)CC[C@@]2(C)CC[C@H](O)[C@]21C(C)=O YALFFHSIVPCNLF-QPSCCSFWSA-N 0.000 claims abstract description 10
- YALFFHSIVPCNLF-UHFFFAOYSA-N Cyperolone Natural products C1C(C(=C)C)CCC2(C)CCC(O)C21C(C)=O YALFFHSIVPCNLF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008187 granular material Substances 0.000 claims abstract description 10
- 239000009737 qizhiweitong Substances 0.000 claims abstract description 10
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 238000005211 surface analysis Methods 0.000 claims abstract description 3
- GIGKXOAUYMWORB-OSQNNJELSA-N isopatchoulenone Chemical compound C[C@@H]1CC[C@@H]2CC3=C(C)C(=O)C[C@]13C2(C)C GIGKXOAUYMWORB-OSQNNJELSA-N 0.000 claims description 20
- 239000000284 extract Substances 0.000 claims description 13
- GIGKXOAUYMWORB-UHFFFAOYSA-N alpha-cyperotundone Natural products CC1CCC2CC3=C(C)C(=O)CC13C2(C)C GIGKXOAUYMWORB-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 8
- 238000013401 experimental design Methods 0.000 claims description 4
- 239000003814 drug Substances 0.000 abstract description 9
- 230000003993 interaction Effects 0.000 description 10
- 239000000843 powder Substances 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 7
- 230000000844 anti-bacterial effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000470 constituent Substances 0.000 description 5
- 230000036407 pain Effects 0.000 description 5
- 230000003110 anti-inflammatory effect Effects 0.000 description 4
- 230000000857 drug effect Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 241000372132 Hydrometridae Species 0.000 description 2
- 206010062717 Increased upper airway secretion Diseases 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 2
- 208000036029 Uterine contractions during pregnancy Diseases 0.000 description 2
- 230000036592 analgesia Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 201000011510 cancer Diseases 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 208000026435 phlegm Diseases 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 241000218176 Corydalis Species 0.000 description 1
- 208000015220 Febrile disease Diseases 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000003694 hair properties Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- VYQNWZOUAUKGHI-UHFFFAOYSA-N monobenzone Chemical compound C1=CC(O)=CC=C1OCC1=CC=CC=C1 VYQNWZOUAUKGHI-UHFFFAOYSA-N 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
A kind of method of the preferred qizhi weitong granules Extraction Process of Volatile Oil parameter of multi objective, belongs to technical field of traditional Chinese medicine pharmacy.Single factor experiment is carried out first, determines final factor level scheme.On the basis of single factor experiment result, using 3 amount of water, soaking time, extraction time factors as variable, using Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil recovery rate, limonene content, cyperolone content and cyperene content as response, it designs the response surface analysis test (12 factorial experiments and 3 multi-center trials) of horizontal totally 15 testing sites of 3 factor 3 and carries out volatile oil extracting one by one according to the test of 15 group analysis, each index result of gained is recorded into table.Application message entropy method carries out weight analysis to index result each in 15 groups of schemes of gained, assigns each index weights coefficient w, calculates overall target M.Polynary bout Fitting Analysis is carried out to data M, and carries out variance analysis and significance test, finally determines optimum extraction process.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicine pharmacy, and in particular to volatile oil mentions in a kind of preferred energy-stagnation stomachache of multi objective
The method of taking technique parameter.
Background technique
Qizhi weitong granules agent is clinically used for stagnation of QI due to depression of the liver, feeling of stuffiness in chest turgor, gastral cavity pain.By radix bupleuri, Fructus Aurantii, Radix Paeoniae Alba,
The composition such as Radix Glycyrrhizae, rhizoma cyperi, rhizoma corydalis, " Sini San " of the prescription in treatise on Febrile Diseases.Perhaps cloud tints cloud tints et al. is by studying
Conclusion out, thousands of of the whole nation, clinical application applied for more than 20 years to the medicine, efficient up to 85% or more.Wherein touch it is inorganic from
Son, involatile constituent, volatile component etc., chemical composition is extremely complex.Zhang Chunyan et al. is by waving qizhi weitong granules
Hair property ingredient characterization and medicinal material ownership research, it was therefore concluded that, the major volatile constituents of the medicine are from Fructus Aurantii and 2 taste of rhizoma cyperi
Simple, wherein Fructus Aurantii has the effects of qi-regulating, antibacterial, eliminating the phlegm, antibechic, stagnant row, and limonene is as the main volatilization of Fructus Aurantii
Property ingredient have and subtract pain, antibacterial, anti-inflammatory, the effect for preventing and treating cancer, rhizoma cyperi has the benefits of dispersing stagnated hepatoqi, menstruction regulating and pain relieving,
α-cyperolone and cyperotundone are the main components of volatile oil in rhizoma cyperi, there is antibacterial anti-inflammatory, analgesia, inhibit uterine contraction etc.
Effect is widely used in treatment gynecological disease.
The extracting method of common volatile oil are as follows: weigh a certain amount of medicinal material in prescription ratio, justify being added after pulverizing medicinal materials
Suitable water is added in the flask of bottom and impregnates certain time, connects volatile oil extractor and reflux condensing tube, is placed in electric jacket
It is middle first by electric jacket modulation maximum temperature make its boil after adjust electric heating sleeving temperature to 100 DEG C, make its keep slight boiling condition heating
Extract certain time.The extraction of volatile oil is mainly by pulverizing medicinal materials granularity, soaking time, amount of water and extraction in this method
The influence of time factor.Raise volatile oil more, preferably playing its drug effect is a critical problem.At present about
It is preferred that the research report of volatile oil optimum extraction process mostly uses orthogonal experiment and is to comment with the single index of volatile oil extracting rate
Sentence standard.Volatile oil constituent is complicated, and principle active component is the key that play drug effect, main in qizhi weitong granules
Volatile component is from Fructus Aurantii and 2 taste simple of rhizoma cyperi, and wherein Fructus Aurantii has qi-regulating, antibacterial, eliminating the phlegm, antibechic, stagnant etc. make that go
With limonene has as the main volatile component of Fructus Aurantii subtracts pain, antibacterial, anti-inflammatory, the effect for preventing and treating cancer, fragrant
The benefits of having attached dispersing stagnated hepatoqi, menstruction regulating and pain relieving, α-cyperolone and cyperotundone are the main components of volatile oil in rhizoma cyperi, are had
Antibacterial anti-inflammatory, inhibits the effects of uterine contraction at analgesia.These active constituent contents number have directly with the performance of drug effect
Connection, Gu the content of volatile oil principle active component also should be used as screening volatile oil optimum extraction work in addition to waving oil extract rate
The index of skill, it should more acurrate in the method that volatile oil extracting rate and volatile oil active constituent content size establish overall target
Preferred volatile oil optimum extraction process.
Summary of the invention
For the deficiency of existing method, Extraction Process of Volatile Oil parameter in a kind of preferred energy-stagnation stomachache of multi objective is now invented
Method, it is intended to more effectively extract Chinese medicine in volatile component.
The method of Extraction Process of Volatile Oil parameter, the steps include: in a kind of preferred energy-stagnation stomachache of multi objective
(1) it carries out single factor experiment: weighing a certain amount of medicinal material in prescription ratio, connect volatile oil extractor and return
Condenser pipe is flowed, sets and adjusts electric heating sleeving temperature to 100 DEG C after first so that it is boiled electric jacket modulation maximum temperature in electric jacket, make
It is kept for slight boiling condition heating extraction certain time.Respectively to pulverizing medicinal materials granularity, amount of water, soaking time, extraction time four
A influence factor carries out single factor exploration, and final factor level scheme is determined according to the result of single factor exploration；
Under general actual conditions, the level of pulverizing medicinal materials granularity can be fixed, so determining amount of water, soaking time, extraction
Time is final factor level；
(2) experimental design is carried out using response surface software: using software such as Design Expert10 software, selecting step
(1) determine factor level scheme i.e.: amount of water, soaking time, 3 factors of extraction time be variable, 3 water of each factor
It is flat；Using Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil recovery rate, limonene content, cyperolone content and cyperene content as response, fortune
(12 factorial experiments are tested with the design a model response surface analysis of horizontal totally 15 testing sites of design 3 factor 3 of Box-Behnken
And 3 multi-center trials) and carry out volatile oil extracting one by one according to the test of 15 group analysis, each index result of gained is recorded to table
In lattice；
(3) application message entropy method calculates overall target；According to each index in step (2) 15 groups of schemes of middle gained as a result, answering
With information Entropy Method, the weight coefficient w of each index is calculatedi, i=1,2,3,4, successively respectively correspond total volatile oil recovery rate, lemon
The weight coefficient of alkene content, cyperolone content, cyperene content；
(4) overall target M is calculated；Each index weights coefficient w acquired according to step (3)i, using formula M=(volatilization
Oil extract rate/volatile oil extracting rate max) × w1+ (limonene content/limonene content max) × w2+ (cyperolone content/rhizoma cyperi
Ketone content max) × w3+ (cyperotundone content/cyperotundone content max) × w4, overall target M is calculated, and record to test
As a result in table；
(5) foundation and variance analysis of model equation；Application software such as Design Expert10 software are in step (4)
The data obtained overall target M carries out polynary bout Fitting Analysis, obtains overall target M to adding water multiple A soaking time B and extract
The secondary multinomial regression model of C3 variable of time and variance analysis and significance test result；
(6) determination and verifying of optimised process；Using software such as Design Expert10 software to gained in step (5)
Secondary multinomial regression model is analyzed, and the optimum extraction process of volatile oil extracting and the best M value of model prediction are obtained；To sieve
The optimised process selected carries out verifying and seeks its M value, and is compared in the best M value of model prediction.
Compared with prior art, the invention has the following advantages that
1. the extraction of volatile oil is influenced by three extraction time, soaking time and amount of water factors, orthogonal experiment is only
It can be carried out linear mathematical model fitting, determine that single factors and test result influence, and then determine optimum extraction process, obtain
Result often have larger difference with true value.And response phase method passes through 10 software of Design Expert, it can be more intuitive
Analyze each interaction factor to the 3 dimensional drawing and contour map of test result, by binomial model equation model, as a result
It is smaller with true value difference.
2. mostly using volatile oil extracting rate single factors as sieve at present about the research of volatile oil optimum extraction process
The judgment criteria of choosing, and the content size of each effective component is also an important factor for it plays drug effect in volatile oil.This method is first
Single factor experiment, then comprehensive volatile oil yield, limonene, rhizoma cyperi are carried out using Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil yield as index
The content multi objective of ketone and cyperotundone carries out the screening of optimised process, improves its accuracy.Because of limonene and cyperotundone
And the content of cyperene is variant, the method for being easy to extract limonene is not necessarily suitble to cyperotundone and cyperene.In view of this,
Using each index weights coefficient of the imparting of information Entropy Method science and then its comprehensive score M is calculated, by analyzing comprehensive score M,
The optimised process filtered out is more rigorous, can effectively improve the content of volatile oil in energy-stagnation stomachache, is energy-stagnation stomachache into one
Step exploitation provides scientific basis.
3. this method records result by response phase method contrived experiment scheme；Each index weights coefficient is assigned by information Entropy Method,
Calculate comprehensive score；It is analyzed as response phase method comprehensive score to obtained by, determines optimum extraction process.With existing side
Method is compared to more science, rigorous, and simple possible, is convenient for experimental study.
Detailed description of the invention
The response surface figure of Fig. 1 amount of water (A) and soaking time (B) interaction factor；
The contour map of Fig. 2 amount of water (A) and soaking time (B) interaction factor；
The response surface figure of Fig. 3 amount of water (A) and extraction time (C) interaction factor；
The contour map of Fig. 4 amount of water (A) and extraction time (C) interaction factor；
The response surface figure of Fig. 5 soaking time (B) and extraction time (C) interaction factor；
The contour map of Fig. 6 soaking time (B) and extraction time (C) interaction factor；
Specific embodiment
Illustrating the present invention referring to specific embodiment, these specific embodiments are further elaborated the present invention, but
It is not as a limitation of the invention.
Embodiment 1
Based on Extraction Process of Volatile Oil in response phase method and the preferred qizhi weitong granules of information Entropy Method multi objective.
1.1 single factor experiments determine each factor level
1) 4 parts of sample are weighed, wherein 3 parts are respectively prepared coarse powder, middle powder and fine powder by 2015 editions Chinese Pharmacopoeias regulation, another 1
Part holding medicine materical crude slice is constant, and fixed soaking time 3h, extraction time 3h and 7 times of amount of water are extracted by 2.1 methods and calculate volatilization
Oil extract rate investigates influence of the medicine materical crude slice granularity to volatile oil extracting, as a result are as follows: 0.25%, 0.5%, 0.45%, 0.3%.Slightly
The mentioned volatile oil content highest of powder, Gu medicine materical crude slice partial size is set to coarse powder；5 parts of sample are weighed, is made slightly by 2015 editions States Pharmacopoeia specifications
Powder, fixed soaking time 3h, 7 times of amount of water extract 2,4,6,8,10h respectively.The accurate amount calculating for reading mentioned volatile oil is waved
Hair oil recovery rate investigates influence of the extraction time to volatile oil extracting, as a result are as follows: and 0.45%, 0.6%, 0.7%, 0.7%,
0.7%.Volatile oil extracting amount reaches peak value when being 6h between at the extraction, admittedly 5 are chosen, 6,7h tri- levels；5 parts of sample are weighed,
Coarse powder is made by 2015 editions States Pharmacopoeia specifications, fixed soaking time 3h and extraction time 3h is separately added into 7 times, and 9 times, 11 times, 13
Times, 15 times of water is ibid investigated and adds influence of the water multiple to volatile oil extracting, as a result are as follows: and 0.5%, 0.6%, 0.65%,
0.8%, 0.8% plus water multiple be 13 times when volatile oil extracting amount reach peak value, admittedly choose 12,13,14h tri- levels；It weighs
5 part of sample, coarse powder is made by 2015 editions States Pharmacopoeia specifications, fixes 7 times of amount of water and extraction time 3h, impregnates 0h, 1h respectively,
2h, 3h, 4h are same as above, and investigate influence of the soaking time to volatile oil extracting, as a result are as follows: and 0.3%, 0.35%, 0.35%,
0.3%, 0.3%.When soaking time is 1h, volatile oil extracting amount reaches peak value, is finally set to 0.5,1,1.5h.
2) according to single factor experiment as a result, determining final factor level table, is shown in Table 1；
1 experimental design factor level table of table
1.2 application response surface softwares carry out experimental design:
On the basis of single factor experiment result, using Design Expert10 software, when choosing amount of water, impregnating
Between, 3 factors of extraction time be variable, with Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil recovery rate, limonene content, cyperolone content and
Cyperene content is response, designs a model with Box-Behnken and designs the response surface of 3 factor, 3 15 testing sites of level
Analysis test (12 factorial experiments and 3 multi-center trials) simultaneously extracts volatile oil to according to 15 groups of schemes, by each index knot of gained
Fruit records into table, and B-B testing program and each index the results are shown in Table 2
2 B-B testing program of table and each index Test result
Analysis of 1.3 information Entropy Methods to data
In one evaluation criteria system, there are m evaluation object, n evaluation index, the original index data square formed
Battle array is Y=(yij)mn.For a certain index i, index yijGap it is bigger, then show that this index is in " unordered " state,
Then effect of the index played in evaluation is bigger；If a certain index value is equal (can be of equal value think that the value of pi is equal),
Then illustrate that this index is in " orderly " state, this index does not work in overall merit.Each finger is calculated using comentropy
Target weight, the overall merit for traditional Chinese medicine extraction multi objective provide foundation.It calculates step are as follows:
1) iotave evaluation index matrix (Xij) mn is established:
2) initial data battle array (Xij) mn is switched into " index probability " matrix (pij) mn:
Note: Pi is the probability of some information, and 0≤pi≤1, thus matrix (Xij) mn should be normalized index is " general
Rate " matrix.Pij indicates " probability " of j-th of test under i-th of evaluation index.
3) indices comentropy (H is calculatedi), obtain HiAre as follows:
[0.9992 0.9943 0.9949 0.9943]。K=1/lnn
4) weight coefficient for calculating each index, obtains final data result.Formula and result are as follows.
Obtain Wi are as follows: [0.0411 0.3312 0.2985 0.3292]；
I.e. volatile oil extracting rate, limonene content, cyperolone content, each index of cyperotundone content weight coefficient be
[0.0411、0.3312、0.2985、0.3292]
1.4 response phase methods carry out data to analyze preferred optimum extraction process
Comprehensive evaluation index M is sought by formula.Data M (overall target) is carried out through Design Expert10 software polynary
Bout Fitting Analysis, when obtaining Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil recovery rate (Y) to adding water multiple (A) soaking time (B) and extracting
Between (C) 3 variables secondary multinomial regression model are as follows: Y=0.91+0.029A+0.049B+0.037C-0.036 AB+
0.061AC+0.035BC-0.061A2-0.088B2-0.070C2. variance analysis and significance test are shown in Table 3.
1)
3 variance analysis of table and significance test
2) as seen from the results in Table 3: this test model (p=0.0061 < 0.01) conspicuousness is extremely significant, the quasi- item (p=of mistake
0.5700 > 0.05) conspicuousness be it is not significant, show that the model is true and reliable.Because to consolidate three factors (comprehensive to M by PA > PC > PB
Close scoring) influence degree are as follows: A, B, C, which all have conspicuousness and A, C, in B > C > A. first order has extremely significant property；It is secondary
A2, B2, C2 all have conspicuousness in；Interaction factor AC has conspicuousness.R2=0.9579, R2adj=0.8820 show
The model can explain the variation of 88.20% response；Correlation coefficient r=0.11/0.12=0.91.67, shows response
Variation has 91.67% to derive from selected variable, it was demonstrated that the models fitting degree is preferable, can be used for analyzing and predicting that Fructus Aurantii, vinegar are fragrant
The extraction of attached total volatile oil.
3) the secondary multinomial regression model of gained in 1.4 is analyzed through Design Expert10 software, obtains volatile oil
The optimum extraction process of extraction and the best M value of model prediction.Finally obtain the optimum extraction of Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil
Technique are as follows: 13.418 times of amount of water, soaking time 1.149h, each influence factor of extraction time 6.518h. are comprehensive to volatile oil extracting
Two-dimentional contour and the 3 dimensional drawing for closing scoring M are as follows: by Fig. 53 dimensional drawing it is found that be between upon extracting it is theoretical most
When good extraction time 6.518h, add that water measures (A) again and curved surface corresponding to soaking time (B) is steeper, show plus water measure again, with soak
Steeping the influence that the time extracts comprehensive score M to Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil has conspicuousness；The contour map of two factor of Fig. 6
It is rounded to show that two interaction factors do not have conspicuousness.By 3 dimensional drawing it is found that when soaking time is theoretical optimal value
When 1.149h, extraction time (C) and curved surface corresponding to amount of water (A) are more gentle, show it for the response surface of comprehensive score M
It is not high that the gradient influences conspicuousness.The color of two factor contour maps from outside to inside color gradually deepen to show its response by
It is cumulative to add, maximum response is obtained in the center point, and contour map is oval and density is larger, shows between two factors
Reciprocation has conspicuousness.By 3 dimensional drawing it is found that when amount of water is best 13.418 times theoretical, extraction time (C)
The corresponding curved surface gradient is steeper, shows that the factor extracts the influence factor of composite factor M to Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil
Significantly；The curved surface gradient corresponding to soaking time (B) is relatively slow, is not so good as to mention to the influence that total volatile oil extracts comprehensive score M
Take the time.The contour map of two factors is rounded to show that two interaction factors do not have conspicuousness.
1.5 the verifying of optimised process
Finally obtain the optimum extraction process of Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil are as follows: 13.418 times of amount of water, soaking time
1.149h, extraction time 6.518h. consider to be adjusted to 13 times of amount of water convenient for practical operation, soaking time 1.1h, extract
Time 6.5h.
It is extracted 3 times using gained optimum extracting method, obtains Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil overall target M value are as follows:
0.9316,0.912,0.923. average value are as follows: 0.9222, the bias ratio with model predication value 0.9322 is 1%, shows this reality
Test predictive preferable, model reliability height.
Claims (5)
1. a kind of based on Extraction Process of Volatile Oil parameter in response phase method and the preferred qizhi weitong granules of information Entropy Method multi objective
Method, which comprises the following steps:
(1) carry out single factor experiment: connection volatile oil extractor extracts the volatile oil in medicinal material, respectively to granularity plus water times
Four number, soaking time, extraction time influence factors carry out single factor exploration, are determined finally according to the result of single factor exploration
Factor level scheme；
(2) experimental design is carried out using response surface software: on the basis of step (1) single factor experiment result, using software, choosing
Taking 3 amount of water, soaking time, extraction time factors is variable, is contained with Fructus Aurantii, prepared RHIZOMA CYPERI with vinegar total volatile oil recovery rate, limonene
Amount, cyperolone content and cyperene content are response, totally 15 horizontal with Box-Behnken 3 factor of design 3 that designs a model
The response surface analysis of testing site is tested and carries out volatile oil extracting one by one according to the test of 15 group analysis, and each index result of gained is remembered
Record is into table；
(3) application message entropy method calculates overall target；According to each index in step (2) 15 groups of schemes of middle gained as a result, application letter
Entropy method is ceased, the weight coefficient w of each index is calculatedi, i=1,2,3,4, successively respectively correspond total volatile oil recovery rate, limonene contains
The weight coefficient of amount, cyperolone content, cyperene content；
(4) overall target M is calculated；Each index weights coefficient w acquired according to step (3)i, using formula M=(volatile oil extracting
Rate/volatile oil extracting rate max) × w1+ (limonene content/limonene content max) × w2+ (cyperolone content/cyperolone content
max)×w3+ (cyperotundone content/cyperotundone content max) × w4, overall target M is calculated, and record to test result table
In；
(5) foundation and variance analysis of model equation；Application software carries out the data obtained overall target M in step (4) polynary
Bout Fitting Analysis obtains secondary multinomial recurrence of the overall target M to water multiple A soaking time B Yu C3 variable of extraction time is added
Model and variance analysis and significance test result；
(6) determination and verifying of optimised process；The secondary multinomial regression model of gained in step (5) is analyzed using software,
Obtain the optimum extraction process of volatile oil extracting and the best M value of model prediction；Verifying is carried out to the optimised process filtered out and seeks its M
Value, and be compared in the best M value of model prediction.
2. one kind described in accordance with the claim 1 is based on waving in response phase method and the preferred qizhi weitong granules of information Entropy Method multi objective
The method of hair oil Extraction technique, which is characterized in that the software is Design Expert10 software.
3. one kind described in accordance with the claim 1 is based on waving in response phase method and the preferred qizhi weitong granules of information Entropy Method multi objective
The method of hair oil Extraction technique, which is characterized in that step (2) designs the response surface point of horizontal totally 15 testing sites of 3 factor 3
Analysis test is 12 factorial experiments and 3 multi-center trials.
4. one kind described in accordance with the claim 1 is based on waving in response phase method and the preferred qizhi weitong granules of information Entropy Method multi objective
The method of hair oil Extraction technique, which is characterized in that using response surface software to gained M carry out polynary bout Fitting Analysis and
Variance analysis and significance test result.
5. one kind described in accordance with the claim 1 is based on waving in response phase method and the preferred qizhi weitong granules of information Entropy Method multi objective
The method of hair oil Extraction technique, which is characterized in that need to verify it after preferably going out optimised process, and and model prediction
Value compares.
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