CN102106892B - Process for preparing Chinese herbal slices of dogwood fruit pulp prepared for decoction - Google Patents
Process for preparing Chinese herbal slices of dogwood fruit pulp prepared for decoction Download PDFInfo
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Abstract
The invention discloses a process for preparing Chinese herbal slices of dogwood fruit pulp prepared for decoction, which comprises the following steps: taking crude dogwood fruit pulp; adding water of 0.2 to 4 times by weight; moistening for 1 to 3h, heating to 80 to 100DEG C and boiling for 30min to 6h and then cooling; taking out liquid medicine until the liquid medicine is completely absorbed for later use; adding yellow wine accounting for 20 to 30 percents of the boiled dogwood fruit pulp by weight and uniformly stirring; and heating and steaming by spacing out water for 0.5 to 4h and drying to obtain the Chinese herbal slices of dogwood fruit pulp prepared for decoction. According to the process for preparing the Chinese herbal slices of dogwood fruit pulp prepared for decoction, provided by the invention, plenty of experiment researches are carried out on the basis of the traditional process for preparing the dogwood fruit pulp; and the process of steaming before boiling is applied to the process for preparation, the contents of active components in the dogwood fruit pulp, such as iridoid glycoside, polyose, and the like can be improved, so that the processed dogwood fruit pulp product has better clinical curative effect, which provides stronger scientific basis for the novel process for preparing the Chinese herbal slices of dogwood fruit pulp prepared for decoction. The invention has broad application prospect.
Description
Technical field
The present invention relates to a kind of process of preparing Chinese medicine new method of the prepared slices of Chinese crude drugs, be specifically related to a kind of concocting method of the Fructus Corni prepared slices of Chinese crude drugs, belong to technical field of traditional Chinese medicine pharmacy.
Background technology
The Chinese medicine Fructus Corni is the drying and ripening sarcocarp of Cornaceae plant Fructus Corni Cornus officinalis Sieb.et Zucc..These article sour in the mouth, puckery; Slightly warm in nature is returned liver, kidney channel, and function liver and kidney tonifying, arresting seminal emission reducing urination, arresting sweating only collapse; Cure mainly caused by liver and kidney deficiency, have a dizzy spell, card such as Hiccough and deaf, soreness of the waist and knees, impotence and premature ejaculation, the seminal emission enuresis, incessant sweating due to debility, menorrhagia, bleeding not during menses, interior-heat are quenched one's thirst; It is main that the article of giving birth to take off with arresting sweating admittedly, and the goods benefiting action strengthens, and is one of tcm clinical practice rare Chinese medicine very commonly used.Fructus Corni mainly contains compositions such as iridoid glycoside, polysaccharide, organic acid, tannin; Wherein iridoid glycoside, polysaccharide are its important active substances of generally acknowledging; And morroniside, loganin are the main matter of Fructus Corni iridoid glycoside; Research at present confirms that it has effects such as immunosuppressant, the protection of many-sided kidney, neuroprotective, and polysaccharide has significant immunomodulating, defying age and antioxidation in the Fructus Corni.At present Fructus Corni is clinical is used to treat diseases such as diabetes, coronary heart disease, hypertension and hepatic and renal YIN deficiency in a large number.
The modern method of concocting of Fructus Corni has enucleation, wine to steam, steam in clear soup; Have also that steaming with vinegar, vinegar are mixed, method such as processed with salt, honey are mixed, honey steams; " mostly the concocting method of Chinese pharmacopoeia, " national Chinese medicine processing standard " and each province and city concocted specification regulation is that enucleation, stewed with wine, wine steam, steam in clear soup; The concocting method of Fructus Corni is the most commonly used with processed with wine at present, but existing concocting method, the part important activity composition that Fructus Corni contained in concocting process; As: the morroniside content of iridoid glycosides reduces, and causes the clinical efficacy of Fructus Corni to reduce.
Summary of the invention
Goal of the invention: the objective of the invention is provides a kind of and can improve active component in the Fructus Corni in order to overcome the deficiency of prior art, the process of preparing Chinese medicine new method of iridoid glycoside, polyoses content, and the Fructus Corni active component after the process of preparing Chinese medicine improves, and clinical efficacy is better.
Technical scheme: in order to realize above purpose, the technical scheme that the present invention takes is:
A kind of concocting method of the Fructus Corni prepared slices of Chinese crude drugs, it comprises the steps:
(1) get Fructus Corni and give birth to article, add the water of 0.2 to 4 times of amount, first moistening 1 to 3 hour, reheat boiled 30 minutes to 6 hours, put coldly after boiling, and it is subsequent use to treat that medicinal liquid blots the back taking-up;
(2) get the boiling Fructus Corni that step (1) obtains, add the yellow wine of boiling Fructus Corni weight 20% to 30%, stir, the water proof heating was steamed 0.5 to 4 hour, and drying promptly gets.
As preferred version, the concocting method of the above-described Fructus Corni prepared slices of Chinese crude drugs, step (1) cooking method are concocted in the Fructus Corni process, and amount of water is 2 times that Fructus Corni is given birth to article weight, and the moistening time is 2 hours, and the temperature of boiling is 80 to 100 ℃, and the boiling time is 6 hours.
As preferred version, the concocting method of the above-described Fructus Corni prepared slices of Chinese crude drugs, step (2) wine steams to be concocted in the Fructus Corni process; The yellow wine addition is 20% of a boiling Fructus Corni weight; The heating steaming temperature is 100 to 120 ℃, and the heating steaming time is 2 hours, steams the back and promptly gets in 60 ℃ of oven dry.
As preferred version, the concocting method of the Fructus Corni prepared slices of Chinese crude drugs provided by the invention, step (1) cooking method are concocted in the Fructus Corni process, and regulating pH value of aqueous solution is 1 to 6; As preferred technical method, step (1) cooking method is concocted in the Fructus Corni process, and regulating pH value of aqueous solution is 1 to 2.
One, Fructus Corni prepared slices of Chinese crude drugs processing procedure is preferred
1, instrument and reagent
Waters-e2695 type high performance liquid chromatograph, 2998 PDA detectors (U.S. Waters company); BP-211D type electronic analytical balance (Sartorius AG); The temperature adjustable electrically heated device of DW (Shanghai flat ring combustion apparatus Engineering Co., Ltd); 101-1A type digital display electric drying oven with forced convection (Shanghai Hu Nan scientific instrument related factory); HH-4 digital display thermostat water bath (state China Electrical Appliances Co., Ltd).
The loganin reference substance is available from Nat'l Pharmaceutical & Biological Products Control Institute (lot number: 111640-200604, assay with), the morroniside reference substance available from Shanghai hundred million glad bio tech ltds (lot number: 091018, assay with).
2, method and result
2.1 morroniside, loganin assay
2.1.1 chromatographic condition chromatographic column Waters-C
18Chromatographic column (4.6 mm * 250 mm, 5 μ m), mobile phase methanol-water (30: 70), flow velocity 0.8 mLmin
-1, detect wavelength 240 nm, 30 ℃ of column temperatures.
2.1.2 the preparation precision of reference substance solution takes by weighing the morroniside reference substance, the loganin reference substance is an amount of, adds 80% methanol respectively and processes the stock solution that per 1 mL contains morroniside 460 μ g, loganin 416 μ g.
2.1.3 the preparation of need testing solution: get Fructus Corni respectively, press the boiling of orthogonal array rated condition water, treat that medicinal liquid blots the back and takes out, according to 10 editions pharmacopeia it is carried out wine and steam, get each processed product after the oven dry, beat powder, cross 60 mesh sieves.Respectively get 0.1g respectively, accurate claim surely, add 25 ml, 80% methanol, claim to decide weight, reflux 1h is put and is supplied weightlessness, 0.45 μ m filtering with microporous membrane after cold.
2.1.4 morroniside, loganin reference substance stock solution are got in the drafting of standard curve; Add 80% methanol and be diluted to the mixing reference substance solution of getting loganin (16.64 μ g/mL), morroniside (36.8 μ g/mL), sample introduction 3,5,10,15,20,25 μ L are vertical coordinate with the peak area that records respectively; Loganin, morroniside sample size are abscissa; The drawing standard curve gets loganin regression equation: Y=1E+06 X – 16584, r=1.0000; Morroniside regression equation: Y=2E+06 X-10873, r=1.0000.Show that loganin is good in 0.04992～0.416 μ g scope internal linear relation, morroniside is good in 0.1104～0.92 μ g scope internal linear relation.
2.1.5 same mixing reference substance solution (loganin 16.64 μ g/mL, morroniside 36.8 μ g/mL) is got in the precision test, continuous sample introduction 6 times, and the RSD value of calculating morroniside and loganin peak area is respectively 1.24% and 1.61%.
2.1.6 stability test is got same need testing solution, respectively at 0,2,4,8, and l2,24 h measure the peak area of morroniside and loganin, and morroniside and loganin peak area RSD value are respectively 1.78% and 0.99% as a result, show that need testing solution is stable in 24 h.
2.1.7 replica test is pressed test sample preparation item test sample method for preparing down, parallel preparation 5 duplicate samples liquid, and microporous filter membrane filters, and measures, and the RSD of morroniside, loganin content is respectively 2.15%, 1.88%.
2.1.8 accurate sample 0.05g (morroniside 7.53 mg/g that take by weighing known content of average recovery test; Loganin 5.47mg/g) 6 parts, puts in the 25 mL volumetric flasks accurate morroniside reference substance solution (the 460.00 μ g mL that add
-1) 1 mL, loganin reference substance solution (416 μ g mL
-1) 0.5 mL, add 80% methanol to scale, shake up, 0.45 μ m filtering with microporous membrane is measured by chromatographic condition under " 2.1.1 " item.Morroniside and loganin average recovery rate are respectively 99.76% and 98.96% as a result, and the RSD value is respectively 1.98% and 1.61%.
2.2 content Determination of Polysaccharide
2.2.1 it is an amount of that 105 ℃ of glucose reference substances that are dried to constant weight are got in the preparation of reference substance solution, the accurate title, decide, and processes the reference substance solution that per 1 mL contains 144.3 μ g glucoses, promptly gets.
2.2.2 the preparation of test liquid is got respectively by the 2.1.3 method and is prepared process of preparing Chinese medicine Fructus Corni 3 g, places tool plug conical flask, adds ultrasonic 30 min of 30 mL, 80% ethanol, centrifugalize (3 000 r/min; 15 min), residue volatilizes in the rearmounted tool plug of the ethanol conical flask and adds 30 mL water, puts in the water bath with thermostatic control agitator 80 ℃ of vibration 2 h; Centrifugalize, and, merge washing liquid and supernatant with washing with alcohol residue 3 times; After it was concentrated, adding ethanol to concentration of alcohol was 80%, placed centrifugalize behind refrigerator 24 h; With ethanol and ether washing precipitation for several times, volatilize behind the ether and to get 1 mL to 25mL again after being settled to 50 mL with water dissolution, subsequent use.
2.2.3 the drafting of standard curve accurately pipettes 144.3 μ g/mL glucose reference substance solution, 0.1,0.2,0.3,0.4,0.5,0.6 mL in 10 mL scale test tubes, adds water to 1 mL, adds 5% phenol solution, 1 mL; Add concentrated sulphuric acid 7 mL after shaking up again, shake up, heat in 100 ℃ of boiling water baths among 30 min; Being cooled to room temperature in the ice-water bath, measuring absorbance in 480 nm wavelength, is abscissa with the reference substance micrograms; Light absorption value is a vertical coordinate, and regression equation is Y=0.0063X-0.0004, r=0.9995; Be illustrated in, be good linear relationship in 14.43 ~ 86.58 μ g scopes.
2.2.4 accurate reference substance diluent 0.5 mL that draws of precision test measures RSD=0. 65% (n=5) by the assay method under the drafting item of standard curve
2.2.5 replica test is got same Asiatic Cornelian Cherry Fruit, and 5 parts, be equipped with need testing solution by a test sample preparation below legal system, measure, RSD is 1. 90%.
2.2.6 stability test is got with a polysaccharide need testing solution and measured, every in 1 h at a distance from 10min mensuration once per 20 min measure once behind 1 h, and 2 h internal absorbance substantially constants, RSD are 2. 17% (n=9).
2.2.7 the average recovery test adds the reference substance solution of 0. 5 mL (72.15 μ g/mL) in each polysaccharide test liquid of 0. 5 mL known content, the average recovery rate that records polysaccharide is: 101.69 %, RSD=2. 87%.
2.3 the cooking technology orthogonal experiment is investigated
Consumption (A), boiling time (B), the moistening time (C) of selecting water, each influence factor respectively selected 3 levels to make an experiment as main investigation factor, adopted L
9(3
4) orthogonal table, serve as to investigate index to experimentize with morroniside, loganin, polyoses content, design factor and level are seen table 1, and experimental result is seen table 2, and table 3 ~ 5 are seen in variance analysis.
Table 1 factor level table
Table 2 L
9(3
4) test arrangement and result
The variance analysis of table 3 morroniside
The variance analysis of table 4 loganin
The variance analysis of table 5 polysaccharide
Carry out intuitive analysis by table 2 and can know that each factor is followed successively by the influence degree of morroniside: B>A>C, the influence degree of loganin is followed successively by: C>B>A, the influence degree of polysaccharide is followed successively by: B>A>C, i.e. the boiling time has the greatest impact to each index, is amount of water and moistening time secondly; Variance analysis by table 3 ~ 5 can be known; Boiling time, amount of water contain the influence of measurer significance to morroniside; The results of analysis of variance by polysaccharide can know that the content of boiling time to polysaccharide has the significance influence, and can be known by the The results of analysis of variance of loganin; Each factor does not have significance to the content of loganin influences comprehensive intuitive analysis and variance analysis, can get preferred extraction process and be: A
2B
3C
2, promptly adding 2 times of water gagings, moistening 2h boils 6h.
2.5 demonstration test is got with 3 parts of batch Fructus Corni medical materials, every part 200 g.Make an experiment according to selection process respectively.So concrete outcome is seen like table 6.
Table 6 demonstration test
The result shows; The processing procedure conditional stability that is screened is feasible; And show by the result; Fructus Corni through after the present invention preferred process conditions boiling again wine steam the processed product that obtains, can obviously improve the content of Fructus Corni iridoid glycoside active component morroniside and polysaccharide, the Fructus Corni clinical effectiveness that the process of preparing Chinese medicine obtains is better.
Two, influence factor's investigation in the Fructus Corni boiling process
1, method and result
1.1 the assay of morroniside, loganin (with above orthogonal experiment)
1.2 different brew temperatures are to the influence of the content of morroniside, loganin
Get Fructus Corni decoction pieces coarse powder 2g, put in the 500 mL measuring bottles, add water to scale; Put (40 ℃ ~ 100 ℃ are adopted heating in water bath, and 120 ℃ are adopted the pressure steam sterilizer heating) heat treated 60 min under 40,60,70,80,90,100,120 ℃ of temperature respectively, take out back cooling rapidly; Supply weightlessness; Microporous filter membrane filters, and high performance liquid chromatogram is measured the content of morroniside, loganin, and concrete outcome is as shown in table 7.
The assay result of morroniside, loganin under table 7 different temperatures
Shown that by table 7 experimental result the content of morroniside and loganin is closely related with temperature, temperature is less than under 80 ℃ the situation; The changes of contents of morroniside and loganin is less; After temperature was greater than 80 ℃, morroniside along with increasing of temperature, and loganin content increases less.Therefore brew temperatures is controlled at more than 80 ℃ in the actual boiling process.
1.3 the different heating time is to the content influence of morroniside and loganin
Get Fructus Corni decoction pieces coarse powder 2 g, put in the 500 mL measuring bottles, add water to scale; 100 ℃ of difference reflux 10,20,30,60,120,240,480,720 min take out back cooling rapidly, supply weightlessness; Microporous filter membrane filters; Sample introduction, high performance liquid chromatogram is measured the content of morroniside, loganin, and concrete outcome is as shown in table 8.
The assay result of morroniside, loganin under the table 8 different heating time
Show by table 8 experimental result; The content of morroniside and loganin is closely related with heat time heating time, and after 10 minutes heat time heating times, the content of morroniside is with increasing gradually heat time heating time; Content at 2 to 8 hours morronisides of heating increases at most, and loganin content increases less.Therefore can be controlled at 2 to 8 hours heat time heating time in the actual boiling process.
1.4 different pH are to the content influence of morroniside and loganin
Get Fructus Corni decoction pieces coarse powder 2 g, put in the 500 mL measuring bottles, add water to scale; Transfer pH to 0.5,1,2,4,6,8,10,100 ℃ of heating 60 min with dilute hydrochloric acid and 0.5 %NaOH respectively, take out back cooling rapidly; Be settled to 10 mL, microporous filter membrane filters, sample introduction; High performance liquid chromatogram is measured the content of morroniside and loganin, and concrete outcome is as shown in table 9.
The assay result of morroniside and loganin under the different pH value of table 9
Shown that by table 9 experimental result it is bigger that the content of morroniside and loganin is influenced by pH value, when pH was 0.5, the content of morroniside was starkly lower than normal contents; When pH was 1～6, its content was increase trend, but was that 2 o'clock content is the highest with pH value, and as separation, and pH was obvious increase trend at 1～2 o'clock, and 2～6 are increase trend.The changes of contents of morroniside is less when neutral and alkaline (Ph>6).Loganin Ph 1 o'clock, content is lower than normal measured value, all the other content are constant basically.Therefore in order to improve the content of active component morroniside and loganin in the boiling process, the pH value of in boiling process, controlling solution is between 1 ~ 6, and the best is between 1 ~ 2.
Beneficial effect: the concocting method of the Fructus Corni prepared slices of Chinese crude drugs provided by the invention is compared with prior art and had the following advantages: the present invention is with the active component of Fructus Corni clinical practice; Like compositions such as morroniside, polysaccharide is evaluation index, on the basis of the traditional concocting method of Fructus Corni, through lot of experiments, draws and can improve the Fructus Corni active component; The new processing procedure of composition such as morroniside, polysaccharide; Make the Fructus Corni goods after the process of preparing Chinese medicine have better clinical effect, the present invention at first adopts the boiling method of optimizing technology to concoct Fructus Corni, obtain the boiling Fructus Corni after; Adopting wine steaming method to concoct again obtains; Concocting method provided by the invention adopts to boil earlier afterwards to steam and combines, and can overcome existing concocting method, concocts the shortcoming that Fructus Corni brings active component iridoid glycoside content to reduce as single with the processed with wine method; For setting up the new concocting method of the Fructus Corni prepared slices of Chinese crude drugs stronger scientific basis is provided, has important application prospects.
The specific embodiment
According to following embodiment, can understand the present invention better.Yet, those skilled in the art will readily understand that the described concrete material proportion of embodiment, process conditions and result thereof only are used to explain the present invention, and the present invention that should also can not limit in claims to be described in detail.
Embodiment 1
A kind of concocting method of the Fructus Corni prepared slices of Chinese crude drugs, it comprises the steps:
(1) get Fructus Corni and give birth to article, add the water of 2 times of amounts, first moistening 2 hours, 100 ℃ of heating were boiled 6 hours again, put coldly after boiling, and it is subsequent use to treat that medicinal liquid blots the back taking-up;
(2) get the boiling Fructus Corni that step (1) obtains, add the yellow wine of boiling Fructus Corni weight 20%, stir, 120 ℃ of heating of water proof were steamed 2 hours, steamed the back and promptly got in 60 ℃ of oven dry.
Embodiment 2
A kind of concocting method of the Fructus Corni prepared slices of Chinese crude drugs, it comprises the steps:
(1) get Fructus Corni and give birth to article, add the water of 3 times of amounts, first moistening 2 hours, 80 ℃ of heating were boiled 4 hours again, put coldly after boiling, and it is subsequent use to treat that medicinal liquid blots the back taking-up;
(2) get the boiling Fructus Corni that step (1) obtains, add the yellow wine of boiling Fructus Corni weight 20%, stir, 100 ℃ of heating of water proof were steamed 4 hours, steamed the back and promptly got in 60 ℃ of oven dry.
Embodiment 3
A kind of concocting method of the Fructus Corni prepared slices of Chinese crude drugs, it comprises the steps:
(1) get Fructus Corni and give birth to article, add the water of 1 times of amount, first moistening 3 hours, 100 ℃ of heating were boiled 2 hours again, put coldly after boiling, and it is subsequent use to treat that medicinal liquid blots the back taking-up;
(2) get the boiling Fructus Corni that step (1) obtains, add the yellow wine of boiling Fructus Corni weight 30%, stir, 120 ℃ of heating of water proof were steamed 1 hour, steamed the back and promptly got in 60 ℃ of oven dry.
Embodiment 4
A kind of concocting method of the Fructus Corni prepared slices of Chinese crude drugs, it comprises the steps:
(1) get Fructus Corni and give birth to article, add the water of 2 times of amounts, using hydrochloric acid to transfer the solution pH value is 2, first moistening 2 hours, and 100 ℃ of heating were boiled 6 hours again, put coldly after boiling, and it is subsequent use to treat that medicinal liquid blots the back taking-up;
(2) get the boiling Fructus Corni that step (1) obtains, add the yellow wine of boiling Fructus Corni weight 20%, stir, 120 ℃ of heating of water proof were steamed 2 hours, steamed the back and promptly got in 60 ℃ of oven dry.
Embodiment 5
A kind of concocting method of the Fructus Corni prepared slices of Chinese crude drugs, it comprises the steps:
(1) get Fructus Corni and give birth to article, add the water of 3 times of amounts, using hydrochloric acid to transfer the solution pH value is 1, first moistening 2 hours, and 80 ℃ of heating were boiled 4 hours again, put coldly after boiling, and it is subsequent use to treat that medicinal liquid blots the back taking-up;
(2) get the boiling Fructus Corni that step (1) obtains, add the yellow wine of boiling Fructus Corni weight 20%, stir, 120 ℃ of heating of water proof were steamed 1 hour, steamed the back and promptly got in 60 ℃ of oven dry.
Embodiment 6 Fructus Corni are given birth to article, traditional wine is steamed article and boiled the comparison of afterwards steaming loganin in the processed product, morroniside, 5 hydroxymethyl furfural and polyoses content earlier
1, the content assaying method of loganin, morroniside, 5 hydroxymethyl furfural
1.1 the preparation of reference substance solution
It is an amount of to take by weighing loganin reference substance, morroniside reference substance, 5 hydroxymethyl furfural, accurately claims surely, adds 80% methanol and processes the mixed solution that per 1 mL contains loganin 16.64 μ g, morroniside 36.8 μ g, 5 hydroxymethyl furfural 46.4 μ g, promptly gets.
1.2 the preparation of test liquid
Get Fructus Corni respectively and give birth to article, traditional wine steaming article, the about 0.1g of the processed product powder that embodiment 1 prepares (crossing sieve No. three), the accurate title, decide, and puts in the tool plug conical flask; Accurate 80% methanol, 25 mL that add claim to decide weight, supersound extraction 1 hour; Put coldly, claim again to decide weight, supply the weight that subtracts mistake with 80% methanol; Shake up, filter, get subsequent filtrate and promptly get.
1.3 chromatographic condition
Waters C18 post (5 μ m, 4. 6mm * 250mm); Mobile phase is acetonitrile: 0.1% phosphoric acid water (0 ~ 12min, 5:95; 12 ~ 15min, 10:90; 15-40min, 10:90); Detect wavelength: 240 nm; Column temperature: 30 ℃; Flow velocity is 1.0 mL/min.
1.4 the drafting of standard curve
Get the mixing reference substance solution of loganin (16.64 μ g/mL), morroniside (36.8 μ g/mL), 5 hydroxymethyl furfural (46.4 μ g), sample introduction 3,5,10,15,20,25 μ L are vertical coordinate with the peak area that records respectively; Loganin, morroniside sample size are abscissa; The drawing standard curve gets loganin regression equation: Y=1E+06 X-16584, r=1.0000; Morroniside regression equation: Y=2E+06 X-10873; R=1.0000,5 hydroxymethyl furfural regression equation: Y=7E+06x+23433, r=0.999 9.Show that loganin is good in 0.04992～0.416 μ g scope internal linear relation, morroniside is good in 0.1104～0.92 μ g scope internal linear relation, and 5 hydroxymethyl furfural is good in 0.0928～1.16 μ g scope internal linear relation.
2, measurement of the polysaccharide content method
2.1 the preparation of reference substance solution
It is an amount of that precision takes by weighing 105 ℃ of glucose reference substances that are dried to constant weight, and accurate the title decides, and processes the reference substance solution that per 1 mL contains 144.3 μ g glucoses, promptly gets.
2.2 the preparation of test liquid
Precision takes by weighing Fructus Corni and gives birth to article, wine product, boils and steam combination processed product (embodiment 1) coarse powder (crossing 60 mesh sieves) 3 g, places tool plug conical flask, adds ultrasonic 30 min of 30 mL, 80% ethanol, centrifugalize (3 000 r/min; 15 min), residue volatilizes in the rearmounted tool plug of the ethanol conical flask and adds 30 mL water, puts in the water bath with thermostatic control agitator 80 ℃ of vibration 2 h; Centrifugalize, and, merge washing liquid and supernatant with washing with alcohol residue 3 times; After it was concentrated, adding ethanol to concentration of alcohol was 80%, placed centrifugalize behind refrigerator 24 h; With ethanol and ether washing precipitation for several times, volatilize behind the ether and to get 1 mL to 25mL again after being settled to 50 mL with water dissolution, subsequent use.
2.3 the drafting of standard curve
Accurately pipette 144.3 μ g/mL glucose reference substance solution, 0.1,0.2,0.3,0.4,0.5,0.6 mL in 10 mL scale test tubes, add water to 1 mL, add 5% phenol solution, 1 mL; Add concentrated sulphuric acid 7 mL after shaking up again, shake up, heat in 100 ℃ of boiling water baths among 30 min; Being cooled to room temperature in the ice-water bath, measuring absorbance in 480 nm wavelength, is abscissa with the reference substance micrograms; Light absorption value is a vertical coordinate, and regression equation is Y=0.0063X-0.0004, r=0.9995; Be illustrated in, be good linear relationship in 14.43 ~ 86.58 μ g scopes.
3, assay result
Fructus Corni is given birth to article, traditional wine steaming article and provided by the invention and is boiled earlier that afterwards to steam loganin in the processed product, morroniside, 5 hydroxymethyl furfural and polyoses content as shown in table 10:
The comparison of the different goods loganins of table 10, morroniside, 5 hydroxymethyl furfural and polyoses content
Assay result by table 10 shows; Fructus Corni is given birth to article, traditional wine and is steamed article and provided by the invention and boil earlier and afterwards steam loganin in the processed product, morroniside, 5 hydroxymethyl furfural and polyoses content and have notable difference, and especially the present invention boils afterwards wine earlier and steams article and traditional wine and steam article and compare the main active of Fructus Corni; Compositions such as morroniside, 5 hydroxymethyl furfural and polysaccharide have obvious raising; Especially after this important activity composition of morroniside was concocted through concocting method of the present invention, its content had obvious raising, and its content steams the method goods with traditional wine and compares; Its content increases more than 1 times, therefore has better medicinal curative effect.
Above embodiment only is explanation technical conceive of the present invention and characteristics; Its purpose is to let the people that is familiar with this technology understand content of the present invention and implements; Can not limit protection scope of the present invention with this; All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (5)
1. the concocting method of Fructus Corni prepared slices of Chinese crude drugs is characterized in that, comprises the steps:
(1) get Fructus Corni and give birth to article, add the water of 0.2 to 4 times of amount, first moistening 1 to 3 hour, reheat boiled 30 minutes to 6 hours, put coldly after boiling, and it is subsequent use to treat that medicinal liquid blots the back taking-up;
(2) get the boiling Fructus Corni that step (1) obtains, add the yellow wine of boiling Fructus Corni weight 20% to 30%, stir, the water proof heating was steamed 0.5 to 4 hour, and drying promptly gets.
2. the concocting method of the Fructus Corni prepared slices of Chinese crude drugs according to claim 1 is characterized in that, step (1) cooking method is concocted in the Fructus Corni process; Amount of water is 2 times that Fructus Corni is given birth to article weight; The moistening time is 2 hours, and the temperature of boiling is 80 to 100 ℃, and the boiling time is 6 hours.
3. the concocting method of the Fructus Corni prepared slices of Chinese crude drugs according to claim 1 is characterized in that, step (2) wine steams to be concocted in the Fructus Corni process; The yellow wine addition is 20% of a boiling Fructus Corni weight; The heating steaming temperature is 100 to 120 ℃, and the heating steaming time is 2 hours, steams the back in 60 ℃ of oven dry.
4. according to the concocting method of each described Fructus Corni prepared slices of Chinese crude drugs of claim 1 to 3, it is characterized in that step (1) cooking method is concocted in the Fructus Corni process, regulating pH value of aqueous solution is 1 to 6.
5. the concocting method of the Fructus Corni prepared slices of Chinese crude drugs according to claim 4 is characterized in that, step (1) cooking method is concocted in the Fructus Corni process, and regulating pH value of aqueous solution is 1 to 2.
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| CN103446432A (en) * | 2013-07-17 | 2013-12-18 | 当涂县黄池蔬菜产销专业合作社 | Cornus officinalis decoction piece for treating kidney deficiency and preparation method of cornus officinalis decoction piece |
| CN104586919A (en) * | 2015-02-04 | 2015-05-06 | 安徽省万生中药饮片有限公司 | Method for processing dogwood with wine |
| CN104940271A (en) * | 2015-06-19 | 2015-09-30 | 亳州市永刚饮片厂有限公司 | Manufacture method of cornus officinalis decoction pieces |
| CN109966334A (en) * | 2017-12-28 | 2019-07-05 | 九芝堂股份有限公司 | A kind of wine-prepared fructus corni and its processing procedure |
| CN111280284A (en) * | 2020-03-31 | 2020-06-16 | 河南中医药大学 | Black bean juice and dogwood preserved fruit and preparation method thereof |
| CN115645449B (en) * | 2022-12-06 | 2024-04-30 | 北京橘井健康科技集团有限公司 | Processing method and application of double-auxiliary wine honey pulp |
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