CN102106892A - 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 percent 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..This product sour in the mouth, puckery, slightly warm in nature, return liver, kidney channel, 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, the product of giving birth to take off admittedly based on arresting sweating, and the goods benefiting action strengthens, and are 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; studies confirm that at present; 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.The present clinical diseases such as diabetes, coronary heart disease, hypertension and hepatic and renal YIN deficiency that are used for the treatment of in a large number of Fructus Corni.
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, " concocting method of Chinese pharmacopoeia, " national Chinese medicine processing standard " and each province and city concocted specification regulation mostly is enucleation, stewed with wine, wine steaming, steamed, 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 deficiencies in the 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 product, 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 standby 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, drying, promptly.
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 product 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 in 60 ℃ of oven dry promptly.
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 makes 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), difference sample introduction 3,5,10,15,20,25 μ L, with the peak area that records is vertical coordinate, loganin, morroniside sample size are abscissa, the drawing standard curve, get 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 method under the test sample preparation, 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 makes the reference substance solution that per 1 mL contains 144.3 μ g glucoses, promptly.
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, place tool plug conical flask, add 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 is concentrated, adding ethanol to concentration of alcohol is 80%, and centrifugalize behind placement refrigerator 24 h is with ethanol and ether washing precipitation several, volatilize behind the ether and to get 1 mL to 25mL again after being settled to 50 mL with water dissolution, standby.
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, add water to 1 mL, add 5% phenol solution, 1 mL, add concentrated sulphuric acid 7 mL after shaking up again, shake up, heat among 30 min in 100 ℃ of boiling water baths, being cooled to room temperature in the ice-water bath, measuring absorbance at 480 nm wavelength places, is abscissa with the reference substance micrograms, light absorption value is a vertical coordinate, and regression equation is
Y=0.0063
X-0.0004, r=0.9995 is illustrated in, and is 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 Fructus Corni powder, and 5 parts, be equipped with need testing solution by 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, and measures once every 10min in 1 h, 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 test 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 see Table 1, and experimental result sees Table 2, and variance analysis sees Table 3 ~ 5.
Table 1 factor level table
Table 2 L
9(3
4) test arrangement and result
The variance analysis of table 3 morroniside
| Soruces of variation | Sum of deviation square | Degree of freedom | FValue | P |
| A | 21.58 | 2 | 138.88 | <0.05 |
| B | 39.05 | 2 | 251.27 | <0.01 |
| C | 0.78 | 2 | 5.03 | >0.05 |
| D | 0.16 | 2 | ? |
The variance analysis of table 4 loganin
| Soruces of variation | Sum of deviation square | Degree of freedom | FValue | P |
| A | 0.002 | 2 | 0.295 | >0.05 |
| B | 0.009 | 2 | 1.448 | >0.05 |
| C | 0.030 | 2 | 5.030 | >0.05 |
| D | 0.006 | 2 | ? | ? |
The variance analysis of table 5 polysaccharide
| Soruces of variation | Sum of deviation square | Degree of freedom | FValue | P |
| A | 4.396 | 2 | 5.994 | >0.05 |
| B | 46.246 | 2 | 63.057 | <0.05 |
| C | 0.421 | 2 | 0.575 | >0.05 |
| D | 0.733 | 2 | ? | ? |
Carry out intuitive analysis as can be known by table 2, 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,Being the boiling time each index to be had the greatest impact, is amount of water and moistening time secondly; By the variance analysis of table 3 ~ 5 as can be known, boiling time, amount of water contain the influence of measurer significance to morroniside, by the The results of analysis of variance of polysaccharide as can be known, the content of boiling time to polysaccharide has the significance influence, and as 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 2 B 3 C 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.Test according to selection process respectively.So concrete outcome is seen as table 6.
Table 6 demonstration test
| Group | Morroniside content/mgg -1 | Loganin content/mgg -1 | Polyoses content/mgg -1 |
| 1 | 16.18 | 5.03 | 52.29 |
| 2 | 16.33 | 5.12 | 51.36 |
| 3 | 16.07 | 5.17 | 53.33 |
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, it is better to concoct the Fructus Corni clinical effectiveness that obtains.
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 increased 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 is in Ph＜1 o'clock, and content is lower than normal measured value, and all the other content are constant substantially.Therefore in order to improve the content of active component morroniside and loganin in the boiling process, the pH value of control solution is between 1 ~ 6 in boiling process, 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, as morroniside, compositions such as polysaccharide are evaluation index, on the basis of the traditional concocting method of Fructus Corni, pass through lot of experiments, draw and to improve the Fructus Corni active component, morroniside, the new processing procedure of compositions such as 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, after obtaining the boiling Fructus Corni, adopting wine steaming method to concoct again obtains, concocting method provided by the invention adopts to boil earlier afterwards to steam and combines, can overcome existing concocting method, concoct the shortcoming that Fructus Corni brings active component iridoid glycoside content to reduce as single with the processed with wine method, provide stronger scientific basis for setting up the new concocting method of the Fructus Corni prepared slices of Chinese crude drugs, have important application prospects.
The specific embodiment
According to following embodiment, the present invention may be better understood.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 illustrate the present invention, and should also can not limit the present invention described in detail in claims.
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 product, 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 standby 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 in 60 ℃ of oven dry promptly.
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 product, 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 standby 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 in 60 ℃ of oven dry promptly.
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 product, 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 standby 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 in 60 ℃ of oven dry promptly.
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 product, add the water of 2 times of amounts, transferring the solution pH value with hydrochloric acid is 2, first moistening 2 hours, and 100 ℃ of heating were boiled 6 hours again, put coldly after boiling, and it is standby 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 in 60 ℃ of oven dry promptly.
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 product, add the water of 3 times of amounts, transferring the solution pH value with hydrochloric acid is 1, first moistening 2 hours, and 80 ℃ of heating were boiled 4 hours again, put coldly after boiling, and it is standby 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 in 60 ℃ of oven dry promptly.
Embodiment 6 Fructus Corni are given birth to product, traditional wine is steamed product 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 makes 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.
1.2 the preparation of test liquid
Get Fructus Corni respectively and give birth to product, traditional wine steaming product, the about 0.1g of the processed product powder that embodiment 1 prepares (crossing sieve No. three), the accurate title, decide, put in the tool plug conical flask, accurate 80% methanol, 25 mL that add claim to decide weight, supersound extraction 1 hour, put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 80% methanol, filter, get subsequent filtrate promptly.
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), difference sample introduction 3,5,10,15,20,25 μ L, with the peak area that records is vertical coordinate, loganin, morroniside sample size are abscissa, the drawing standard curve, get 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 makes the reference substance solution that per 1 mL contains 144.3 μ g glucoses, promptly.
2.2 the preparation of test liquid
Precision takes by weighing Fructus Corni and gives birth to product, wine product, boil steaming in conjunction with processed product (embodiment 1) coarse powder (crossing 60 mesh sieves) 3 g, place tool plug conical flask, add 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 is concentrated, adding ethanol to concentration of alcohol is 80%, and centrifugalize behind placement refrigerator 24 h is with ethanol and ether washing precipitation several, volatilize behind the ether and to get 1 mL to 25mL again after being settled to 50 mL with water dissolution, standby.
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 among 30 min in 100 ℃ of boiling water baths, be cooled to room temperature in the ice-water bath, measuring absorbance at 480 nm wavelength places, is abscissa with the reference substance micrograms, and light absorption value is a vertical coordinate, regression equation is Y=0.0063X-0.0004, r=0.9995 is illustrated in, and is good linear relationship in 14.43 ~ 86.58 μ g scopes.
3, assay result
Fructus Corni is given birth to product, traditional wine steaming product and is provided by the inventionly 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 product, traditional wine is steamed product and provided by the invention boiling earlier afterwards steamed loganin in the processed product, morroniside, 5 hydroxymethyl furfural and polyoses content have notable difference, especially the present invention boils back wine earlier and steams product and traditional wine and steam product and compare, the main active of Fructus Corni, morroniside, composition such as 5 hydroxymethyl furfural and polysaccharide has obvious raising, especially after this important activity composition of morroniside is concocted through concocting method of the present invention, its content has obvious raising, 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 allow the people that is familiar with this technology understand content of the present invention and is implemented; 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 product, 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 standby 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, drying, promptly.
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 product 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 |
| CN103446222A (en) * | 2013-07-17 | 2013-12-18 | 当涂县黄池蔬菜产销专业合作社 | Liver nourishing and eyesight improving cornus decoction piece and preparation method thereof |
| 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 |
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| CN103446222A (en) * | 2013-07-17 | 2013-12-18 | 当涂县黄池蔬菜产销专业合作社 | Liver nourishing and eyesight improving cornus decoction piece and preparation method thereof |
| 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 |
| CN115645449A (en) * | 2022-12-06 | 2023-01-31 | 北京橘井健康科技集团有限公司 | Method for processing cornus officinalis with double auxiliary materials, wine and honey and application of cornus officinalis |
| 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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