CN109223881A - A method of optimization Taohe Chengqi decoction decoction preparation process - Google Patents
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Abstract
A method of optimization Taohe Chengqi decoction decoction preparation process belongs to Pharmaceutical Analysis technical field.Using high performance liquid chromatography, the best preparation process of Taohe Chengqi decoction decoction is obtained by the screening of response surface combining information entropy method.Rhein, glycyrrhizic acid and amarogentin, cinnaldehydrum chromatographic condition are determined first, and carry out methodological study for following assay；Determine investigation factor and level, it is tested using response phase method arrangement, by the content results of measured Rhein, glycyrrhizic acid, four kinds of amarogentin, cinnaldehydrum ingredients, carry out data processing, obtain entropy, for the screening of best preparation method, the best preparation method finally determined, and carry out best verification experimental verification.
Description
Technical field
The invention belongs to herbal pharmaceutical analysis technical fields, and in particular to a kind of optimization Taohe Chengqi decoction decoction preparation process
Method.
Background technique
Taohe Chengqi decoction comes from the 106th article of treatise on Febrile Diseases written by Chinese Zhang Zhongjing: " Taiyin diseases is not understood, bladder heat stagnation, people
As mad, blood under, be cured by lower person.Its outer puzzled person, can not yet attack, solve outside it in the ban, and, but hypogastric pain person is that can attack to outer solution
It, suitable Taohe Chengqi decoction." be made of peach kernel, rheum officinale, ramulus cinnamomi, saltcake, Radix Glycyrrhizae, effect is blood-breaking stagnation resolvation, and stasis eliminatings are raw new, main
Controlling card is stagnated blood syndrome symptoms include fever and delirium, difficult urination, the hypogastric pain etc. caused by hemostasis and heat symptoms caused by an exopathgen are mutually tied in lower coke.
There is drug for invigorating blood circulation and eliminating stasis to have peach kernel in prescription, softening hard masses of purging heat dissolving stasis medicine has rheum officinale, saltcake, and scattered stasis of blood of stimulating the menstrual flow medicine has ramulus cinnamomi,
Resistance and supplementing qi medicine has Radix Glycyrrhizae.Peach kernel and ramulus cinnamomi in side, belonging to mutually makes compatibility, blood-breaking promoting menstruation；Rheum officinale and saltcake belong to mutual reinforcement between compatibility, rush down
Hot dissolving stasis；Peach kernel and rheum officinale, saltcake, belonging to mutually makes compatibility, and peach kernel helps rheum officinale, saltcake softening hard masses dissolving stasis, and rheum officinale, saltcake help peach kernel broken
Blood stagnation resolvation；Peach kernel and Radix Glycyrrhizae, belonging to phase reverse phase makes compatibility, and opposite, reinforcing and reducing methods is same to be used, peach kernel blood-breaking, Radix Glycyrrhizae QI invigorating, phase envoy,
QI invigorating general's blood stasis of blood.Recipe is refinforced each other, to play dissolving stasis of purging heat, the benefits of promoting menstruation QI invigorating.
Modern research shows that the application of Taohe Chengqi decoction clinically has been not limited only to lower burnt stagnated blood syndrome, can also be widely applied
In the treatment of multisystem disease.Wang Li etc. is the study found that Taohe Chengqi decoction has centainly to pelvic inflammatory disease rat local immunity is improved
Effect；Repair can be played to its impaired institutional framework, promote its metabolism, restore its normal morphosis, in turn
Promote the recovery of cell function.Tang Zhonghua is sick on the basis of regular western medicine treatment plus with Taohe Chengqi decoction treatment post operation of hypertensive cerebral hemorrhage
People 62, as a result total effective rate 95%.Luo Zhenghou application Taohe Chengqi decoction plus-minus treats demented (lower energizer retention of heat card), produces effects good.
The decocting method of modern Taohe Chengqi decoction are as follows: with water decoct recipe about 25min, remove slag, then be included in saltcake decoct 2~
3min, the method can not extract the effective component in this decoction complete.Influence three key factors that decoction extracts are as follows: leaching
Time, amount of water, extraction time are steeped, how effective component more completely to be extracted, is the key that decoction preparation process skill
Art.Chinese prescription complicated component, research report mostly uses orthogonal experiment and about optimization decoction preparation process with single at present
Effective component is that index is evaluated.The method is excessively unilateral, therefore the present invention uses response phase method contrived experiment, and with rheum officinale
The content of the multiple effective components of acid, amarogentin, glycyrrhizic acid, cinnaldehydrum is index, using information Entropy Method Objective Weight, and then
To the preparation process of optimization.
Summary of the invention
For the deficiency of existing method, the present invention is to establish a kind of side for optimizing the best preparation process of Taohe Chengqi decoction decoction
Method.
A method of optimization Taohe Chengqi decoction decoction preparation process, which is characterized in that using high performance liquid chromatography into
Row active constituent content measuring obtains the best preparation work of Taohe Chengqi decoction decoction by the screening of response surface combining information entropy method
Skill, comprising the following steps:
(1) medicine materical crude slice sorting: identification meets and providing under 2015 editions pharmacopeia, one continuous item, weighs 60 grams of rheum officinale, and 15 grams of peach kernel,
30 grams of ramulus cinnamomi, 30 grams of Radix Glycyrrhizae, 30 grams of saltcake；
(2) preparation of Taohe Chengqi decoction Aqueous extracts: using medicine materical crude slice in step (1), impregnating certain time, add water a certain amount of,
Certain time is extracted, 50mL is concentrated into, prepares the Aqueous extracts of Taohe Chengqi decoction.
(3) high effective liquid chromatography for measuring target Rhein, amarogentin, glycyrrhizic acid, osmanthus the determination of liquid-phase condition: are used
Skin aldehyde, using the Aqueous extracts prepared in step (2), for determining liquid-phase condition；Determining measurement Rhein, glycyrrhizic acid
Chromatographic condition: Diamonsil C18 (5 μm, 250 × 4.6mm), mobile phase be -0.1% phosphate aqueous solution of acetonitrile, gradient elution:
0-20min, 10%-40% acetonitrile；20-30min, 40%-50% acetonitrile；30-70min, 50%-10% acetonitrile；Volume flow
1.0ml/min；10 μ L of sample volume；30 DEG C of column temperature；Detection wavelength 250nm, during above-mentioned gradient elution in each period
The volumn concentration that acetonitrile accounts for overall flow rate phase is at the uniform velocity promoted, and such as 0-20min, 10%-40% acetonitrile is indicated: in 0-
In 20min, the volumn concentration of acetonitrile is gradually increased from 10% in mobile phase 40%；Be calculated corresponding Rhein,
The content of glycyrrhizic acid；
Determining measurement amarogentin, cinnaldehydrum chromatographic condition: chromatographic column: Diamonsil C18 (5 μm, 250 ×
4.6mm), mobile phase is acetonitrile-water, gradient elution: 0-10min, 10% acetonitrile；10-20min, 10%-20% acetonitrile；20-
30min, 20% acetonitrile；30-60min, 20%-45% acetonitrile, 60-70min, 45%-10% acetonitrile；Volume flow 1.0ml/
min；10 μ L of sample volume；30 DEG C of column temperature；Detection wavelength 210nm measures amarogentin, and 290nm measures cinnaldehydrum.Above-mentioned gradient is washed
The volumn concentration that acetonitrile during de- in each period accounts for overall flow rate phase is at the uniform velocity promoted, such as 0-10min, 10%
Acetonitrile；10-20min, 10%-20% acetonitrile；Indicate: the volumn concentration of acetonitrile is constant in 0-10min, in mobile phase is
10%, in 10-20min, the volumn concentration of acetonitrile is gradually increased from 10% in mobile phase 200%；Phase is calculated
The content of the amarogentin, cinnaldehydrum answered.
Rhein, amarogentin, glycyrrhizic acid, the corresponding peak area of content of cinnaldehydrum and standard in solution to be tested is molten
The peak area ratio of liquid is compared with being calculated the content of Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum；
(4) response phase method experimental design: software such as Design Expert10 software is used, it is first determined three in step (2)
A investigation factor: soaking time, amount of water, extraction time, three levels of each factor, with Rhein, amarogentin, Radix Glycyrrhizae
Acid, Determination of Cinnamaldehyde are response, are designed a model the response of horizontal totally 17 testing sites of design 3 factor 3 with Box-Behnken
Surface analysis test, and the preparation for carrying out Taohe Chengqi decoction decoction one by one is tested according to 17 group analysis, use chromatostrip in step (3)
Part carries out assay, and each index result of gained is recorded into table；
(5) application message entropy method obtains weight coefficient: converting probability square for the obtained 17 groups of test results of step (4)
Battle array calculates indices comentropy, obtains weight coefficient wi, i=1,2, and 3,4, successively respectively correspond Rhein Content, semen armeniacae amarae
Glycosides content, glycyrrhizic acid content, Determination of Cinnamaldehyde weight coefficient；
(6) it calculates overall target M: according to weight coefficient obtained by step (5), calculating every group analysis test overall target Mm=
(Rhein Contentm/ Rhein Content max) × w1+ (amarogentin contentm/ amarogentin content max) (glycyrrhizic acid contains × w2+
Amountm/ glycyrrhizic acid content max) × w3+ (Determination of Cinnamaldehydem/ Determination of Cinnamaldehyde max) × w4, calculate the overall target of 17 groups of tests
Mm, m=1,2,3,4...17, and record into test result table；Rhein Content max indicates Rhein in 17 groups of experimental datas
The greatest measure of content, amarogentin content max indicate the greatest measure of amarogentin content in 17 groups of experimental datas, glycyrrhizic acid
Content max indicates that the greatest measure of glycyrrhizic acid content in 17 groups of experimental datas, Determination of Cinnamaldehyde max indicate in 17 groups of experimental datas
The greatest measure of Determination of Cinnamaldehyde.
(7) determination of best preparation process: application software such as Design Expert10 software is to institute's total in step (6)
Polynary bout Fitting Analysis is carried out according to overall target M, overall target M is obtained and (B) extraction time is measured again to soaking time (A) plus water
(C) the secondary multinomial regression model of 3 variables and variance analysis and significance test result；Using software such as Design
Expert10 software multinomial regression model secondary to gained is analyzed, and the best preparation process and mould of Taohe Chengqi decoction decoction are obtained
The best M value of type prediction；Verifying is carried out to the optimised process filtered out and seeks its M value, and is compared in the best M value of model prediction
Compared with.
Compared with the prior art, the present invention has the following advantages:
Taohe Chengqi decoction is that the important foundation side of representative for controlling stagnant heat card is distinguished in " Treatise on Febrile and Miscellaneous Disease ", cure mainly " bladder heat stagnation,
People is for example mad ... but hypogastric pain person." according to original text spirit in syndrome differentiation, not only pointed out diseased region in bladder, but also point out disease show
In the heart.Drug for invigorating blood circulation and eliminating stasis has peach kernel in Taohe Chengqi decoction composition, and softening hard masses of purging heat dissolving stasis medicine has rheum officinale, saltcake, and scattered stasis of blood of stimulating the menstrual flow medicine has
Ramulus cinnamomi, resistance and supplementing qi medicine have Radix Glycyrrhizae.Recipe is refinforced each other, to play dissolving stasis of purging heat, the benefits of promoting menstruation QI invigorating.In recent years, it is held with to peach-pit
Gas soup main sick position, syndrome, interpretation of the cause, onset and process of an illness understanding deepen continuously, the party is in a variety of diseases especially in some difficult and complicated cases and anxious critical
It is used widely in the treatment of disease, obtains relatively satisfactory curative effect.For the modern Application for further speeding up Taohe Chengqi decoction, using existing
Generation technique screens to obtain the best preparation method of Taohe Chengqi decoction.
Using response phase method in such a way that information Entropy Method combines, screening technology research is carried out.Response phase method by pair
The set of sample point in specified design space carries out limited experimental design, fits the overall situation of output variable (system response)
It approaches to replace true response surface.In Optimum design of engineering structure, using response phase method not only available response target and design
Variation relation between variable, and available prioritization scheme, the i.e. optimum combination of design variable, reach objective function most
It is excellent.Due to traditional Chinese medicine ingredients complexity, index components are more, and being investigated using single index has certain one-sidedness, and mostly basis is ground at present
Study carefully basis or documents and materials determine the multiple index components of Chinese medicine, and subjective weighting method is to directly give preference information based on researcher
Method, it is big by main body subjective impact, using information entropy theory to data carry out Objective Weight, weight coefficient is entirely from right
The analysis of experimental data clearly reflects the objective law that index components change under various extracting conditions, while also avoiding
Influencing each other between each achievement data, also reduces interference of the subjective factor to experimental result to a certain extent, improves
The science and preciseness of this experimental study.More may be used using the best preparation method that information Entropy Method and response phase method screen
It leans on, accurately.
Detailed description of the invention
Fig. 1 sample and reference substance high-efficient liquid phase chromatogram
A: Rhein reference substance figure；B: amarogentin reference substance figure；C: glycyrrhizic acid reference substance figure；D: cinnaldehydrum reference substance
Figure；E:250nm sample drawing；F:210nm sample drawing；G:290nm sample drawing；
1: Rhein；2: amarogentin；3: glycyrrhizic acid；4: cinnaldehydrum
Specific embodiment
Below with reference to embodiment, the invention will be further described, but the present invention is not limited to following embodiments.
The best preparation method of 1 Taohe Chengqi decoction of embodiment
1. the investigation of methodology
The preparation of 1.1 Taohe Chengqi decoction Aqueous extracts
Peach kernel, rheum officinale, ramulus cinnamomi, the radix glycyrrhizae preparata, saltcake gomi herbs of certain batch of material, preceding four taste are weighed in original side's prescription ratio
The water that certain solid-liquid ratio is added in medicine, which impregnates, to be decocted, and medicine materical crude slice water absorption is supplied, and decocts filtration three times, and saltcake is added in merging filtrate,
50ml is concentrated the filtrate to, Taohe Chengqi decoction Aqueous extracts are obtained, it is spare.
1.2 chromatographic condition
1.2.1 Rhein, glycyrrhizic acid chromatographic condition
Chromatographic column: Diamonsil C18 (5 μm, 250 × 4.6mm), mobile phase are -0.1% phosphate aqueous solution of acetonitrile, ladder
Degree elution: 0-20min, 10%-40% acetonitrile；20-30min, 40%-50% acetonitrile；30-70min, 50%-10% acetonitrile；Body
Product flow 1.0ml/min；10 μ L of sample volume；30 DEG C of column temperature；Detection wavelength 250nm.
1.2.2 amarogentin, cinnaldehydrum chromatographic condition
Chromatographic column: Diamonsil C18 (5 μm, 250 × 4.6mm), mobile phase are acetonitrile-water, gradient elution: 0-
10min, 10% acetonitrile；10-20min, 10%-20% acetonitrile；20-30min, 20% acetonitrile；30-60min, 20%-45% second
Nitrile, 60-70min, 45%-10% acetonitrile；Volume flow 1.0ml/min；10 μ L of sample volume；30 DEG C of column temperature；Detection wavelength 210nm
Amarogentin is measured, 290nm measures cinnaldehydrum.
The preparation of 1.3 reference substance solutions
Precision weighs Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum 6.70,2.30,4.40,1.45mg respectively, is placed in
In 5ml volumetric flask, methanol dissolves and is settled to scale, shakes up, be made mass concentration be respectively 1340.00,460.00,
880.00, the reference substance stock solution of 290.00 μ g/ml.Each 2.5ml of reference substance stock solution is taken, is placed in same 5ml volumetric flask, i.e.,
Obtain mixed reference substance solution.
The preparation of 1.4 test solutions
The Aqueous extracts 1ml that precision draws after concentration shakes up quiet until methanol dissolves and be settled to scale in 5ml volumetric flask
It sets, is filtered through 0.45 μm of miillpore filter, take subsequent filtrate up to test solution.
1.5 system suitability test
Take reference substance solution, test solution by above-mentioned chromatographic condition sample introduction, the result is shown in Figure 1.1.6 linear relationships are investigated
Precision measures 1,5,10,15,20 μ l of Rhein reference substance stock solution, is measured by identified chromatographic condition,
Record peak area.
Precision measures 5,10,20,30,40,50 μ l of amarogentin reference substance stock solution, carries out by identified chromatographic condition
Measurement records peak area.
Precision measures 1,5,10,20,30 μ l of glycyrrhizic acid reference substance stock solution, is measured by identified chromatographic condition,
Record peak area.
Precision measures 3,10,20,30,40,50 μ l of cinnaldehydrum reference substance stock solution, is surveyed by identified chromatographic condition
It is fixed, record peak area.
With sample volume (x, μ g) for abscissa, peak area (y) is ordinate, draws standard curve, regression equation and linear
Range is shown in Table 1.
1 regression equation of table and the range of linearity
Then by the corresponding peak area of content and mark of Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum in solution to be tested
The peak area ratio of quasi- solution is compared with being calculated the content of Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum；
1.7 precision test
Precision draws mixed reference substance solution, repeats sample introduction 6 times under determining chromatographic condition respectively, records peak area.
Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum peak area RSD be respectively 0.79%, 0.77%, 0.92%, 0.87% (n=
6), surface instrument precision is good.1.8 stability test
Same test solution is taken, respectively at being placed at room temperature for 0,2,4,6,8,12h, by identified chromatographic condition sample introduction,
Record peak area.As a result Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum peak area RSD be respectively 1.32%, 2.12%,
1.66%, 2.84%, show that test sample is stablized in 12h.
1.9 repetitive test
Same test solution is taken, prepares 6 parts in parallel by identified method, the sample introduction under determining chromatographic condition, note
Record peak area.As a result Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum peak area RSD be respectively 2.21%, 1.46%,
0.87%, 1.61%, show that this method repeatability is good.
1.10 being loaded recovery test
Precision measures 6 parts of known content test solution, and every part of 1ml is separately added into a certain amount of Rhein, semen armeniacae amarae
Glycosides, glycyrrhizic acid, cinnaldehydrum reference substance solution prepare test solution, then are measured by above-mentioned chromatographic condition, record peak face
Product, and sample recovery rate is calculated, it the results are shown in Table 2.
2 sample recovery rate test result (n=6) of table
2 extraction process by water based on the preferred Taohe Chengqi decoction of information entropy theory
The design of 2.1 response surface experiments
Based on single factor exploration test result, Combination Design principle is tested in interview according to response, determines soaking time
(A), solid-liquid ratio (B), extraction time (C) are investigation factor, are to refer to Rhein, amarogentin, glycyrrhizic acid, Determination of Cinnamaldehyde
Mark, and Assignment Analysis is carried out to the above index using entropy assessment, comprehensive evaluation index is calculated, is tested by the interview of 3 factor, 3 horizontal respone
It is designed, factor level is shown in Table 6.
6 factor level table of table
2.2 data process&analysis
The matrix (X) of iotave evaluation index is established according to document, it is as follows.
Calculate Pij, " probability " matrix (P) is converted by original matrix.
Formula are as follows:I=1,2,3,4；J=1,2,3,4...17, n=17
Calculate the comentropy (H of each indexi), obtain the H of evaluation indexi。
H=[0.9924 0.9715 0.9864 0.9072]
Calculate i-th index coefficient Wi。
W=[0.0537 0.1997 0.0954 0.6512]
For the probability matrix of 1 m row n column, comprehensive evaluation index Mm=P1mW1+P2mW2+P3mW3+…+PnmWn, i.e. rheum officinale
Acid, amarogentin, glycyrrhizic acid, cinnaldehydrum weight coefficient be respectively 0.0537,0.1997,0.0954,0.6512.
Data weighting in probability matrix is handled, comprehensive evaluation index (M) is obtained, variance analysis is carried out to it, is established best
Extraction process.Response surface experiments the results are shown in Table 7, and variance analysis is shown in Table 8.
7 response surface experiments result of table
8 analysis of variance table of table
Experimental result is analyzed by Design-Expert software, using overall merit as response, obtains quadratic polynomial recurrence
Fit equation Y=0.053-5.238 × 10-3A+0.020B-6.750 × 10-4C+0.012AB+7.100 × 10-3AC-1.350
× 10-3BC+0.012A2-4.275 × 10-4B2-7.453 × 10-3C2, Y is overall merit in formula, and A is soaking time, and B is
Solid-liquid ratio, C are extraction time.By analysis of variance table it is found that regression equation model P=0.0322 < 0.05 established, illustrates model
Significantly, quasi- item P=0.4205 > 0.05 is lost, not significantly, shows that the model has referential, can be used for Taohe Chengqi decoction water and propose work
Skill theoretical prediction.It influences the extraction process by water factor size and is followed successively by B > A > C, is i.e. solid-liquid ratio > soaking time > extraction time, feed liquid
Than for significant factor, soaking time, extraction time influence test result without conspicuousness.
2.3 verification test
It is analyzed by Design-Expert software, obtains optimum extraction condition are as follows: soaking time 60.00min, solid-liquid ratio 1:
10.00, extraction time 130.25min, overall merit 0.092, it is contemplated that experiment operability optimizes it are as follows: leaching
Steep time 60.00min, solid-liquid ratio 1:10.00, extraction time 130.00min.
Claims (4)
1. a kind of method for optimizing Taohe Chengqi decoction decoction preparation process, which is characterized in that carried out using high performance liquid chromatography
Active constituent content measuring obtains the best preparation work of Taohe Chengqi decoction decoction by the screening of response surface combining information entropy method
Skill, comprising the following steps:
(1) 60 grams of rheum officinale, 15 grams of peach kernel, 30 grams of ramulus cinnamomi, 30 grams of Radix Glycyrrhizae, 30 grams of saltcake medicine materical crude slice sorting: are weighed；
(2) preparation of Taohe Chengqi decoction Aqueous extracts: using medicine materical crude slice in step (1), certain time is impregnated, adds water a certain amount of, extracted
Certain time is concentrated into 50mL, prepares the Aqueous extracts of Taohe Chengqi decoction；
(3) determination of liquid-phase condition, using high effective liquid chromatography for measuring target Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum
Content；
(4) response phase method experimental design: software such as Design Expert10 software is used, it is first determined examine for three in step (2)
Examine factor: soaking time, amount of water, extraction time, three levels of each factor, with Rhein, amarogentin, glycyrrhizic acid, osmanthus
Skin aldehyde is response, is designed a model the response surface point of horizontal totally 17 testing sites of design 3 factor 3 with Box-Behnken
Analysis test, and according to 17 group analysis test one by one carry out Taohe Chengqi decoction decoction preparation, using chromatographic condition in step (3) into
Row assay records each index result of gained into table；
(5) application message entropy method obtains weight coefficient: probability matrix is converted by the obtained 17 groups of test results of step (4),
Indices comentropy is calculated, obtains weight coefficient wi, i=1,2,3,4, successively respectively correspond Rhein Content, amarogentin
Content, glycyrrhizic acid content, Determination of Cinnamaldehyde weight coefficient；
(6) it calculates overall target M: according to weight coefficient obtained by step (5), calculating every group analysis test overall target Mm=(rheum officinale
Acid contentm/ Rhein Content max) × w1+ (amarogentin contentm/ amarogentin content max) × w2+ (glycyrrhizic acid contentm/ sweet
Oxalic acid content max) × w3+ (Determination of Cinnamaldehydem/ Determination of Cinnamaldehyde max) × w4, calculate the overall target M of 17 groups of testsm, m=
1,2,3,4...17, and record into test result table；Rhein Content max indicates Rhein Content in 17 groups of experimental datas
Greatest measure, amarogentin content max indicate the greatest measure of amarogentin content in 17 groups of experimental datas, glycyrrhizic acid content
Max indicates that the greatest measure of glycyrrhizic acid content in 17 groups of experimental datas, Determination of Cinnamaldehyde max indicate cassia bark in 17 groups of experimental datas
The greatest measure of aldehyde.
(7) determination of best preparation process: it is quasi- that application software carries out polynary bout to the data obtained overall target M in step (6)
Analysis is closed, the secondary multinomial recurrence mould that overall target M measures 3 variables of (B) extraction time (C) to soaking time (A) plus water again is obtained
Type and variance analysis and significance test result；It is analyzed using software multinomial regression model secondary to gained, obtains peach-pit and hold
The best preparation process of gas rushing agent and the best M value of model prediction；Verifying is carried out to the optimised process filtered out and seeks its M value,
And it is compared in the best M value of model prediction.
2. according to the method for claim 1, which is characterized in that the determination of step (3) liquid-phase condition: using in step (2)
The Aqueous extracts of preparation, for determining liquid-phase condition；The chromatographic condition of determining measurement Rhein, glycyrrhizic acid: Diamonsil C18
(5 μm, 250 × 4.6mm), mobile phase are -0.1% phosphate aqueous solution of acetonitrile, gradient elution: 0-20min, 10%-40% acetonitrile；
20-30min, 40%-50% acetonitrile；30-70min, 50%-10% acetonitrile；Volume flow 1.0ml/min；10 μ L of sample volume；Column
30 DEG C of temperature；Detection wavelength 250nm, the acetonitrile during above-mentioned gradient elution in each period account for the volume basis of overall flow rate phase
Content is at the uniform velocity promoted, and the content of corresponding Rhein, glycyrrhizic acid is calculated；
Determining measurement amarogentin, cinnaldehydrum chromatographic condition: chromatographic column: Diamonsil C18 (5 μm, 250 × 4.6mm), stream
Dynamic is mutually acetonitrile-water, gradient elution: 0-10min, 10% acetonitrile；10-20min, 10%-20% acetonitrile；20-30min, 20%
Acetonitrile；30-60min, 20%-45% acetonitrile, 60-70min, 45%-10% acetonitrile；Volume flow 1.0ml/min；Sample volume 10
μL；30 DEG C of column temperature；Detection wavelength 210nm measures amarogentin, and 290nm measures cinnaldehydrum.It is each during above-mentioned gradient elution
The volumn concentration that acetonitrile in period accounts for overall flow rate phase is at the uniform velocity promoted, and corresponding amarogentin, osmanthus is calculated
The content of skin aldehyde.
3. according to the method for claim 1, which is characterized in that step (7) is using Design Expert10 software to step
(6) the data obtained overall target M carries out polynary bout Fitting Analysis in.
4. according to the method for claim 1, which is characterized in that measurement target Rhein, amarogentin, glycyrrhizic acid, cassia bark
The method of aldehyde: by Rhein in solution to be tested, amarogentin, glycyrrhizic acid, cinnaldehydrum the corresponding peak area of content with
The peak area ratio of standard solution is compared with being calculated the content of Rhein, amarogentin, glycyrrhizic acid, cinnaldehydrum.
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| CN110118846A (en) * | 2019-03-26 | 2019-08-13 | 河北中医学院 | The method for building up of Taohe Chengqi decoction matter basis |
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