CN105193741A - Preparation method for honeysuckle flower-fructus forsythia powder solid decoction - Google Patents

Preparation method for honeysuckle flower-fructus forsythia powder solid decoction Download PDF

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CN105193741A
CN105193741A CN201510708399.3A CN201510708399A CN105193741A CN 105193741 A CN105193741 A CN 105193741A CN 201510708399 A CN201510708399 A CN 201510708399A CN 105193741 A CN105193741 A CN 105193741A
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decoction
lonicerae
powder solid
preparation
forsythiae
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CN105193741B (en
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林渊
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Fujian University of Traditional Chinese Medicine
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Fujian University of Traditional Chinese Medicine
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Abstract

The invention provides a preparation method for a honeysuckle flower-fructus forsythia powder solid decoction. The preparation method comprises the following steps: (1) preparing medicinal materials consisting of 30 g of honeysuckle flower, 12 g of Herba Lopatheri, 30 g of fructus forsythia, 12 g of herba schizonepetae, 15 g of fermented soybean, 18 g of arctium fruit, 15 g of raw licorice, 18 g of mint, 18 g of balloonflower root and 18 g of reed rhizome; and (2) crushing the medicinal materials, combining the crushed medicinal materials to obtain coarse grains with diameters no more than 1 cm, placing the coarse grains in a drug decocting machine with a power of 1200 W, adding 90 mL of water, preheating the drug decocting machine for 2 min, then carrying out heating and decocting for 3 min so as to obtain coarse medicinal material grains with soup, drying the soup and the medicinal materials, filling a filter paper bag with a drying product and directly packaging the drying product with a transparent plastic bag so as to obtain the honeysuckle flower-fructus forsythia powder solid decoction. The honeysuckle flower-fructus forsythia powder solid decoction provided by the invention has the advantages of short decoction time, a small amount of added water, easiness in preparation and convenience in carrying and administration.

Description

A kind of preparation method of Lonicerae and Forsythiae Powder solid decoction
Technical field
The present invention is specifically related to a kind of preparation method of Lonicerae and Forsythiae Powder solid decoction.
Background technology
Solid decoction is reform on decoction and decoction made from powder agent basis, it is one novel dosage forms easily and efficiently, be the improvement that a kind of that traditional decoction decoction method and modern mechanical automated production be combined with each other carries, the solid preparation of taking convenience, it not only has traditional decoction to absorb fast, drug effect feature rapidly, according to the change of the state of an illness with card plus-minus flavour of a drug dose, can also can take into account the feature in different patient or different lesions stage neatly comparatively comprehensively; And carry, taking convenience, mechanization automatic production process can reduce the time of boiling medicine significantly, improves the fried efficiency of medicine.
Lonicerae and Forsythiae Powder is made up of Flos Lonicerae, Fructus Forsythiae, Radix Glycyrrhizae, Fructus Arctii, Herba Menthae, Herba Schizonepetae, Semen Sojae Preparatum, Herba Lophatheri, Radix Platycodonis, Rhizoma Phragmitis ten taste medicine, and wherein Flos Lonicerae, Fructus Forsythiae are monarch drug.Flos Lonicerae main component has chlorogenic acid compound, flavone compound and triterpene saponin componds and volatilization wet goods; The main component of Fructus Forsythiae is lignanoid and its glycosides compound, phenethyl alcohol glycoside compounds and pentacyclic triterpenoid and the wet goods that volatilizees.Chlorogenic acid is the principle active component of Flos Lonicerae, have blood pressure lowering, function of gallbladder promoting, antibacterial, rise white effect, also have antioxidative activity, be promising antioxidant simultaneously.Phillyrin is active substance important in Fructus Forsythiae, is also one of index composition of Fructus Forsythiae.In side, ministerial drug Fructus Arctii, Herba Menthae etc. are containing arctiin, Hesperidin, are not only effective ingredient but also be the index composition detected.Therefore the present invention measures these the four kinds of amount of substances in Lonicerae and Forsythiae Powder and it can be used as Con trolling index.
Summary of the invention
The technical problem to be solved in the present invention, is the preparation method providing a kind of Lonicerae and Forsythiae Powder solid decoction.
The present invention is achieved in that a kind of preparation method of Lonicerae and Forsythiae Powder solid decoction, comprises the following steps:
(1) each medical material is prepared by following formula:
Flos Lonicerae 30g, Herba Lophatheri 12g, Fructus Forsythiae 30g, Herba Schizonepetae 12g, Semen Sojae Preparatum 15g, Fructus Arctii 18g, Radix Glycyrrhizae 15g, Herba Menthae 18g, Radix Platycodonis 18g and Rhizoma Phragmitis 18g;
(2) each medical material merging in (1) is ground into coarse granule, diameter is not more than 1cm, is placed in boiling machine, and add water 90mL, and boiling machine power is 1200W, and after first preheating 2min, heating decocts 3min again, obtains the medical material coarse granule adsorbing medicinal liquid; By medicinal liquid together with medical material after drying, load in filter paper bag, outer transparent plastic bag is directly packed, and obtains Lonicerae and Forsythiae Powder solid decoction.
Further, the method for pouring of described Lonicerae and Forsythiae Powder solid decoction is as follows:
Brew 2 times with boiling water 200mL, each brewing time is 5min.
The invention has the advantages that: Lonicerae and Forsythiae Powder solid decoction of the present invention has that decocting time is shorter, amount of water is less, manufacture method be simple, carry, the advantage of taking convenience.
Detailed description of the invention
A preparation method for Lonicerae and Forsythiae Powder solid decoction, comprises the following steps:
(1) each medical material is prepared by following formula:
Flos Lonicerae 30g, Herba Lophatheri 12g, Fructus Forsythiae 30g, Herba Schizonepetae 12g, Semen Sojae Preparatum 15g, Fructus Arctii 18g, Radix Glycyrrhizae 15g, Herba Menthae 18g, Radix Platycodonis 18g and Rhizoma Phragmitis 18g;
(2) each medical material merging in (1) is ground into coarse granule, diameter is not more than 1cm, is placed in boiling machine, and add water 90mL, and boiling machine power is 1200W, and after first preheating 2min, heating decocts 3min again, obtains the medical material coarse granule adsorbing medicinal liquid; By medicinal liquid together with medical material after drying, load in filter paper bag, outer transparent plastic bag is directly packed, and obtains Lonicerae and Forsythiae Powder solid decoction.
The method for pouring of described Lonicerae and Forsythiae Powder solid decoction is as follows:
Brew 2 times with boiling water 200mL, each brewing time is 5min.
1, the preparation of Lonicerae and Forsythiae Powder solid decoction test sample
Above-mentioned obtained Lonicerae and Forsythiae Powder solid decoction boiling water 200mL is brewed rear filtration, is settled to 250mL, then evaporate to dryness, add supersound extraction 30min after methanol 25mL, after filtering, precision measures 15mL filtrate, adds methanol constant volume to 50mL, shake up, with syringe by microporous filter membrane and get final product.
High performance liquid chromatography testing conditions:
Chromatographic column: UltimateXB-C18 (4.6mm × 250mm, 5 μm), determined wavelength: 279nm, column temperature is 30 DEG C, and mobile phase is methanol: phosphate aqueous solution, type of elution: gradient elution, and flow velocity is 0.8mL/min, and sample size is 10 μ L.
Table 1 gradient elution program
The assay of 1.1 phillyrins, chlorogenic acid, arctiin, Hesperidin
1.1.1 the configuration of reference substance solution
Phillyrin, chlorogenic acid, arctiin and Hesperidin reference substance precision take in right amount, and add methanol standardize solution respectively, make reference substance solution, concentration is respectively: 0.1428mg/mL, 0.1309mg/mL, 0.1536mg/mL and 0.1686mg/mL.
1.1.2 linear relationship is investigated
Accurate draw in the measuring bottle of each reference substance solution 0.2mL, 0.6mL, 1.0mL, 1.5mL, 2.0mL, 3.0mL to 10mL and to add methanol constant volume.Draw 20 μ L more respectively and inject high performance liquid chromatograph, the integrating peak areas value that record chromatogram measures, and with reference substance sample introduction quality solubility (μ g/mL) for abscissa x, reference substance peak area is that vertical coordinate y carries out linear regression, result is: the regression equation of phillyrin is y=6900.6x+4356.9, r=0.9994 (n=6), prove that sample size relation within the scope of 1.3 μ g ~ 45.4 μ g of phillyrin is good, the regression equation of chlorogenic acid is y=82104x-54858, r=0.9998 (n=6), prove that sample size relation within the scope of 2.6 μ g ~ 39.4 μ g of chlorogenic acid is good, the regression equation of arctiin is y=7214x-1532.3, r=0.9996 (n=6), prove that sample size relation within the scope of 3.2 μ g ~ 44.0 μ g of arctiin is good, the regression equation of Hesperidin is y=7411.5x-2013.5, r=0.9998 (n=6), prove that sample size relation within the scope of 3.4 μ g ~ 51.0 μ g of Hesperidin is good.
The linear relationship of table 2 phillyrin
The linear relationship of table 3 chlorogenic acid
The linear relationship of table 4 arctiin
The linear relationship of table 5 Hesperidin
1.1.3 Precision Experiment
Get Lonicerae and Forsythiae Powder solid decoction need testing solution continuous sample introduction 5 times, and calculate phillyrin, chlorogenic acid, arctiin, Hesperidin peak area RSD%, result is respectively: 0.29%, 0.97%, 0.64% and 1.02%, shows that instrument precision is good.
Table 6 Precision Experiment result
1.1.4 repeated experiment
Prepare Lonicerae and Forsythiae Powder solid decoction test sample 5 parts of sample introductions, and calculate phillyrin, chlorogenic acid, arctiin and Hesperidin peak area RSD%, result is respectively: 1.04%, 0.33%, 0.84% and 1.17%, shows that method repeatability is good.
Table 7 repeated experiment result
1.1.5 stability test
When 0h, 2h, 4h, 6h, 8h, 12h, 24h, sample introduction is once respectively to get Lonicerae and Forsythiae Powder solid decoction need testing solution, and calculate the RSD of chlorogenic acid, phillyrin, arctiin and Hesperidin peak area, result is respectively 0.82%, 0.59%, 0.34% and 0.54%, shows: sample is stable in 24h.
Table 8 stability experimental result
1.1.6 recovery test
Get the Lonicerae and Forsythiae Powder solid decoction 6 parts with a collection of known content, it is appropriate and by " 1.1.3 " operation, measure content that precision adds reference substance.The average recovery rate of result phillyrin, chlorogenic acid, arctiin and Hesperidin be respectively 97.50%, 99.44%, 100.67% and 100.56%, RSD be respectively 4.29%, 1.37%, 2.71% and 2.50%.
Table 9 phillyrin determination of recovery rates result
Table 10 chlorogenic acid determination of recovery rates result
Table 11 arctiin determination of recovery rates result
Table 12 Hesperidin determination of recovery rates result
1.2 affect the investigation of Lonicerae and Forsythiae Powder solid decoction preparation factor
Because Lonicerae and Forsythiae Powder includes volatile oil, former side's decoction made from powder decocting time is also shorter, and also needs boiled water to brew when taking.Therefore setting decocting time is 3min, because boiling machine power is fixed as 1200W, therefore probe into the impact of amount of water on each main component and yield of extract at this.Consider to decoct rear residue medicinal liquid speed drying time comprehensive descision preferred plan simultaneously, the results are shown in Table 2-13.
1.2.1 yield of extract calculates
Lonicerae and Forsythiae Powder solid decoction 90 DEG C of tap water 200mL are brewed, after filtering, standardize solution is in 250mL, measures filtrate 20mL and is placed in the evaporating dish water bath method of dry constant temperature, being positioned over dry 3h in 105 DEG C of vacuum drying ovens after evaporate to dryness, exsiccator 30min is put into after taking-up, and precise weighing.
(for recording extractum weight, M is pharmaceutical decocting piece gross weight to m)
Table 13 Lonicerae and Forsythiae Powder solid decoction amount of water investigation table
As shown in Table 13 under the condition of fixing decoction power and decocting time, because amount of water only differs 5mL, affect little on each component content and soft extracts yield, but consider to decoct overdrying whether to have medicinal liquid and do on the bottom of a pan and the length of drying time, show that best decoction scheme is: decoct 3 minutes, decoct temperature (power 1200W), amount of water 90mL.
The confirmatory experiment of 1.3 optimum conditions
Take pharmaceutical decocting piece by recipe quantity and be ground into the coarser powder of 1cm size, under optimum process condition, preparing Lonicerae and Forsythiae Powder solid decoction, repeat preparation 3 times, measure according to the method described above, average, the results are shown in Table 14.
Table 14 optimised process the result
1.4 molding research
Prepare Lonicerae and Forsythiae Powder solid decoction according to preferred the best conditions of preparation pr ocess, put in filter paper bag, and pack.
1.4.1 orthogonal experiment optimization solid decoction brews technique
Because solid decoction is through decocting and pharmaceutical decocting piece dry together with medicine juice, and need using mixing in water for oral taking, therefore do simple optimizing to the method for pouring of solid decoction, as solid decoction medication guide.Be 2 times according to the decoction number of times of traditional decoction, the number of times that brews of fixed solid decoction is twice, uses water to be 90 DEG C (consider different regions height above sea level difference cause the boiling point of water different), investigating, the results are shown in Table 15 with amount of water for probing into factor.
Table 15 solid decoction brews process results
As shown in Table 15, amount of water when brewing affects to some extent on brewing effect, and it is 200mL that the best brews amount of water.The best brews scheme: water temperature 90 DEG C, 200mL brew 2 times.
1.4.2 the confirmatory experiment of optimum condition
Take pharmaceutical decocting piece by recipe quantity and be ground into the coarser powder of 1cm size, under optimum process condition, preparing Lonicerae and Forsythiae Powder solid decoction, and brew under optimum brewing conditions, repeat experiment 3 times and measure, averaging, the results are shown in Table 16.
Table 16 optimised process the result
2. Lonicerae and Forsythiae Powder and solid decoction yield of extract thereof compare
2.1 assay method
According to Pharmacopoeia of the People's Republic of China version water-soluble extractives assay method in 2010: draw Lonicerae and Forsythiae Powder by pipet precision and decoct gained medicinal liquid 10mL, be placed in the evaporating dish of dry constant temperature, put into vacuum drying oven 105 DEG C of drying under reduced pressure 3h after water bath method, put into precise weighing after exsiccator 0.5h.Calculate total extractum to weigh and yield of extract.
2.2 leaching rate computational methods
By Lonicerae and Forsythiae Powder solid decoction of the present invention from add 200mL water brew respectively the 1st, 2,3,5,10,20,30,60min interval time accurately draw 20mL, each water 20mL is centrifugal after supplementing, draw the evaporating dish that the 10mL supernatant is placed in dry constant temperature, after water bath method in vacuum drying oven 105 DEG C of drying under reduced pressure 3h, weigh after being placed in exsiccator 0.5h.
m for record the heavy g of solid (the value first time of m is m1, and second time is m1+m2, by that analogy), mL alwaysthe total amount (mL) of volume, mL inspectionbe the liquid measure to be checked (mL) carrying out measuring, W is example weight (g), m (1 ~ 8)always thing weight (g) is measured for m.
2.3 sample preparation
2.3.1 the sample preparation of Lonicerae and Forsythiae Powder decoction made from powder
Take pharmaceutical decocting piece by recipe quantity and be ground into the coarser powder of 1cm size, being placed in boiling machine and decocting 2 times (first time adds water 300mL, decocts 3mim, obtain decocting liquid and be about 200mL, the 2nd 300mL that adds water, obtains decocting liquid and is about 200mL), merge twice decocting liquid, after filtration, be settled to 400mL.Getting 20mL in the evaporating dish of dry constant temperature, after water bath method, puts exsiccator 0.5h, precise weighing after putting into infrared drying oven 105 DEG C of dry 3h.And prepare 3 parts by above method.
2.3.2 Lonicerae and Forsythiae Powder brews loose preparation
Take pharmaceutical decocting piece by recipe quantity and be ground into the coarser powder of 1cm size, filtering after brewing 2 times with 200mL90 DEG C of tap water, be settled to 400mL.Getting 20mL in the evaporating dish of dry constant temperature, after water bath method, puts exsiccator 0.5h, precise weighing after putting into infrared drying oven 105 DEG C of dry 3h.3 parts are prepared by above method.
2.3.3 prepared by Lonicerae and Forsythiae Powder solid decoction
Take pharmaceutical decocting piece by prescription and be ground into the coarser powder of 1cm size, in boiling machine, add water 90mL, decocts 3 minutes, filters, be settled to 400mL after dry 12 minutes with 200mL90 DEG C of tap water after brewing 2 times.Getting 20mL in the evaporating dish of dry constant temperature, after water bath method, puts exsiccator 0.5h, precise weighing after putting into infrared drying oven 105 DEG C of dry 3h, prepares 3 parts.
2.3.4 measurement result
The yield of extract measurement result of table 17 Lonicerae and Forsythiae Powder and solid decoction thereof
The leaching rate measurement result of table 18 Lonicerae and Forsythiae Powder solid decoction
2.3.5 statistical disposition result
Use SPSS10.0 statistical software to carry out t inspection (getting significance α=0.05) to the yield of extract of Lonicerae and Forsythiae Powder and solid decoction thereof, result is as follows:
Homogeneity test of variance F=2.1683<F0.5/2 (2,2) i.e. P>0.05, then variance is neat
Average t two-tailed test t0.1/2.2<t=2.5348<t0.2/2.2 and P>0.05 not statistically significant, can think that the yield of extract of Lonicerae and Forsythiae Powder solid decoction of the present invention and the former side's decoction made from powder of Lonicerae and Forsythiae Powder does not have difference, extractum is total material base of clinical practice, can reflect the basic difference of the two.
In sum, the factor affecting Lonicerae and Forsythiae Powder solid decoction preparation technology mainly contains and decocts temperature, amount of water, because boiling machine used is constant power, therefore temperature factor is not discussed, the optimum process condition that goes out by experiment is: amount of water 90mL, decocting time 3min, the best brews technique and brews 2 times for adding boiling water (being the water of 90 DEG C) 250mL herein.
Experimental result shows the preparation technology of Lonicerae and Forsythiae Powder solid decoction and brews process stabilizing, convenient, the Lonicerae and Forsythiae Powder solid decoction yield of extract prepared with this understanding and Lonicerae and Forsythiae Powder there was no significant difference.
Lonicerae and Forsythiae Powder solid decoction of the present invention has that decocting time is shorter, amount of water is less, manufacture method is simple, carry, the advantage of taking convenience, the present invention improves on traditional decoction and decoction made from powder agent preparation method, the preparation method of Lonicerae and Forsythiae Powder solid decoction is identical with traditional decoction, just dosage form and decocting condition difference to some extent, the chemical composition for solid decoction and former side's slice decoction contrasts and lays the foundation with study on the efficiency.

Claims (2)

1. a preparation method for Lonicerae and Forsythiae Powder solid decoction, is characterized in that: comprise the following steps:
(1) each medical material is prepared by following formula:
Flos Lonicerae 30g, Herba Lophatheri 12g, Fructus Forsythiae 30g, Herba Schizonepetae 12g, Semen Sojae Preparatum 15g, Fructus Arctii 18g, Radix Glycyrrhizae 15g, Herba Menthae 18g, Radix Platycodonis 18g and Rhizoma Phragmitis 18g;
(2) each medical material merging in (1) is ground into coarse granule, diameter is not more than 1cm, is placed in boiling machine, and add water 90mL, and boiling machine power is 1200W, and after first preheating 2min, heating decocts 3min again, obtains the medical material coarse granule adsorbing medicinal liquid; By medicinal liquid together with medical material after drying, load in filter paper bag, outer transparent plastic bag is directly packed, and obtains Lonicerae and Forsythiae Powder solid decoction.
2. as claimed in claim 1, it is characterized in that: the method for pouring of described Lonicerae and Forsythiae Powder solid decoction is as follows:
Brew 2 times with boiling water 200mL, each brewing time is 5min.
CN201510708399.3A 2015-10-27 2015-10-27 A kind of preparation method of Yinqiao San solid decoction Expired - Fee Related CN105193741B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108607046A (en) * 2016-12-13 2018-10-02 河南后羿实业集团有限公司 A kind of animal compound Lonicera and Forsythia oral solution and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JPS5959158A (en) * 1982-09-29 1984-04-04 Kinichi Hayashi Preparation of herb syrup
CN1150900A (en) * 1995-11-22 1997-06-04 张维安 Production technology of traditional Chinese medicine solid decoction

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Publication number Priority date Publication date Assignee Title
JPS5959158A (en) * 1982-09-29 1984-04-04 Kinichi Hayashi Preparation of herb syrup
CN1150900A (en) * 1995-11-22 1997-06-04 张维安 Production technology of traditional Chinese medicine solid decoction

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Publication number Priority date Publication date Assignee Title
CN108607046A (en) * 2016-12-13 2018-10-02 河南后羿实业集团有限公司 A kind of animal compound Lonicera and Forsythia oral solution and preparation method thereof

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