CN102406760A - Herba verbenae officinalis fluid decoction pieces and preparation method thereof - Google Patents
Herba verbenae officinalis fluid decoction pieces and preparation method thereof Download PDFInfo
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Abstract
The invention discloses herba verbenae officinalis fluid decoction pieces and a preparation method thereof. The decoction pieces are suitable for standardized production and mechanized packaging, and have high decocting rate and less effective component loss. The invention aims to make standardized production and mechanized packaging easier under the premise of maintaining original medicine components, reaches stable and reliable quality and automatic packaging of Chinese herbal pieces, and meets the industrialization requirement of Chinese herbal pieces. The herba verbenae officinalis fluid decoction pieces are prepared by the following method: a. medicinal material crushing: crushing traditional herba verbenae officinalis decoction pieces or finished and selected herba verbenae officinalis, conducting sieving through a sieve of 75-85 meshes, thus obtaining medicinal powder; b. enzyme killing of the medicinal powder: subjecting the medicinal powder to drying treatment in a baking oven at a temperature of 95-105DEG C for more than 4h; c. blast shot preparation: mixing the treated medicinal powder with a proper amount of water so as to obtain a soft material, carrying out granulation, putting wet particles in a shot blasting machine for shot blasting, and drying the obtained wet blast shots at a temperature lower than or equal to 80DEG C, taking the blast shots out and placing them under room temperature, performing sieving, and taking blast shots of 10-24 meshes, thus obtaining the herba verbenae officinalis fluid decoction pieces.
Description
Technical field
The present invention relates to a kind of prepared slices of Chinese crude drugs, mobile decoction pieces of particularly a kind of Herba Verbenae and preparation method thereof belongs to technical field of Chinese medicines.
Background technology
The prepared slices of Chinese crude drugs are Chinese crude drugs through by Chinese medical theory, Chinese medicine processing method, after concocting through processing, can directly be used for the Chinese medicine of tcm clinical practice.The prepared slices of Chinese crude drugs have comprised the Chinese medicine section (comprising cutting, piece, lobe) of part processing through the place of production, original shape pharmaceutical decocting piece and the decoction pieces of processing through cutting (at source on the basis of processing), big gun.Herba Verbenae, Latin formal name used at school are Herba Verbenae Officinalis, and the purple top of another name Agrimony, wild catmint, Agrimony, phoenix neck grass, Aeschna melanictera are careless, TUIXUECAO, Herba Passiflorae Cupiformis, are the medicines of removing heat from blood removing blood stasis, have the effect of anti-inflammatory analgesic.Herba Verbenae tradition decoction pieces is to remove undesirable root and impurity via the Herba Verbenae medical material, cleans, moisten slightly, and cutting, exsiccant step is concocted and is formed, and the small product size of preparation is huge, and is fluffy, is difficult to store and packing.Application number is that 01100033.3 Chinese invention patent discloses a kind of nanometer prepared slices of Chinese crude drugs and preparation method thereof; Be that Chinese medicine powder is broken into the superfines below 500 nanometers; The preparation cost of this superfines is too high; Owing to smashed the cell wall of plant, with traditional Chinese medicines decoction pieces structure again than big difference, so do not possess the equity with the prepared slices of Chinese crude drugs on the drug effect.Therefore; Under the prerequisite that keeps original medicinal ingredient; Produce and mechanical packaging for the ease of standardization, reach that prepared slices of Chinese crude drugs steady quality is reliable, automatic packaging, satisfy the requirement of prepared slices of Chinese crude drugs industrialization, need improve the method for preparing of existing decoction pieces.
Summary of the invention
The object of the invention is to provide a kind of be suitable for standardizing production and mechanical packaging, decocting rate is high, loss of effective components the is few mobile decoction pieces of Herba Verbenae.
The present invention provides the method for preparing of the mobile decoction pieces of this Herba Verbenae.
The technical solution adopted for the present invention to solve the technical problems is:
The mobile decoction pieces of a kind of Herba Verbenae is prepared from following method:
A, pulverizing medicinal materials: the Herba Verbenae after Herba Verbenae tradition decoction pieces or arrangement selected is pulverized, and crosses 75～85 mesh sieves, obtains medicated powder;
B, medicated powder enzyme denaturing: medicated powder is dried in 95～105 ℃ of baking ovens and is handled more than 4 hours;
The preparation of c, ball blast: with the medicated powder after the pre-treatment with must soft material after an amount of water mixes, granulation, wet granular is ball blast in finisher,pill; The wet ball blast that makes is dry under≤80 ℃ of temperature, is placed to room temperature after the taking-up, sieves; Get 10 ~ 24 purpose ball blasts, get the mobile decoction pieces of Herba Verbenae.
The mobile decoction pieces of Herba Verbenae of the present invention (ball blast) changes its physical aspect through operations such as pulverizing, enzyme denaturing, mixing, molding, dryings, and the ball shape flowable decoction pieces that combines the modern pharmaceutical technology to process.
The method for preparing of the mobile decoction pieces of a kind of described Herba Verbenae, this method may further comprise the steps:
A, pulverizing medicinal materials: the Herba Verbenae after Herba Verbenae tradition decoction pieces or arrangement selected is pulverized, and crosses 75～85 mesh sieves, obtains medicated powder;
B, medicated powder enzyme denaturing: medicated powder is dried in 95～105 ℃ of baking ovens and is handled more than 4 hours;
The preparation of c, ball blast: with the medicated powder after the pre-treatment with must soft material after an amount of water mixes, granulation, wet granular places the finisher,pill ball blast; The wet ball blast that makes is dry under≤80 ℃ temperature, is placed to room temperature after the taking-up, sieves; Get 10 ~ 24 purpose ball blasts, get the mobile decoction pieces of Herba Verbenae.
As preferably, b is in the step, and medicated powder enzyme denaturing in 95～105 ℃ of baking ovens was handled 4～5 hours.After undressed Herba Verbenae medicated powder was prepared into ball blast, chemical constituent had significantly sacrificing, and phenylpropyl alcohol glucosides class material damage is more, and is wherein obvious with the loss of verbascoside.For reducing the loss of chemical constituent as far as possible, each step of technical process is investigated, find that the loss of chemical constituent mostly occurs at initial blend step.Mostly the chemical constituent of loss is the glycoside material; Doubting to due to the effect of glycosides enzyme, is the loss that reduces chemical constituent, guarantees the equity of chemical constituent before and after the ball blast preparation; So the used medicated powder of preparation ball blast has been carried out pre-treatment, has promptly adopted 4～5 hours deactivation glycosides of 95～105 ℃ of hyperthermia dryings enzyme.
As preferably, c goes on foot medicated powder and water after the described pre-treatment by the mixed of 1:2～2.2.The medicated powder of this mixed helps the formation of soft material and follow-up pelletization.
As preferably, c goes on foot described ball blast process parameter for throwing circle rotating speed 500rpm, throws 20～25min between bowlder.This condition makes that ball blast product roundness is good, and hardness is moderate, big or small homogeneous, and density is even, has good fluidity, is beneficial to industrialized great production, automatic packaging, the convenient storage.
The advantage of the more traditional decoction pieces of the mobile decoction pieces (ball blast) of Herba Verbenae of the present invention is:
1, traditional decoction pieces is bulky, and is fluffy, is difficult to store and packing.The present invention follows traditional Chinese medicine theory according to prepared slices of Chinese crude drugs production actual demand, in conjunction with modern pharmaceutical technology development a kind of new medicine decoction pieces (mobile decoction pieces).The mobile decoction pieces of Herba Verbenae of the present invention (ball blast) only is adhesive with water; Roundness is good, and hardness is moderate, big or small homogeneous; Density is even; Good fluidity is convenient to that standardization is produced, mechanical packaging, and prepared slices of Chinese crude drugs steady quality is reliable to reach, automatic packaging, satisfy the requirement of prepared slices of Chinese crude drugs industrialization.
2, method for preparing of the present invention can be preserved the main component in the Herba Verbenae to greatest extent.
3, the present invention adopts the method for high temperature enzyme denaturing effectively to keep the glycoside composition in the Herba Verbenae.
4, the decocting rate of the mobile decoction pieces of product Herba Verbenae is higher than traditional decoction pieces.The mobile decoction pieces of ball shape is beneficial to the fried of composition more.
Description of drawings
Fig. 1 is oleanolic acid and the ursolic acid reference substance HPLC chromatogram in the Quality Control parameter of the mobile decoction pieces of Herba Verbenae of the present invention.
Fig. 2 is the Herba Verbenae need testing solution HPLC chromatogram in the Quality Control parameter of the mobile decoction pieces of Herba Verbenae of the present invention.
Fig. 3 is a Herba Verbenae tradition decoction pieces outward appearance photo.
Fig. 4 is mobile decoction pieces (ball blast) outward appearance of the Herba Verbenae photo that the present invention makes.
Fig. 5 is mobile decoction pieces (ball blast) the microstructure comparison diagram that Herba Verbenae tradition decoction pieces and the present invention make.
Fig. 6 is that mobile decoction pieces (ball blast) thin layer that Herba Verbenae tradition decoction pieces and the present invention make is differentiated figure, wherein, and the S-ursolic acid; 1-Herba Verbenae control medicinal material; 2-Herba Verbenae tradition decoction pieces; The mobile decoction pieces of 3-Herba Verbenae.
Fig. 7 be Herba Verbenae tradition decoction pieces (on) with mobile decoction pieces (descending) decocting liquid mirror image HPLC contrast color spectrogram.
Fig. 8 be traditional decoction pieces (on) with mobile decoction pieces (descending) alcohol extract mirror image HPLC comparison diagram.Wherein, traditional decoction pieces is last, mobile decoction pieces infra.
Fig. 9 be traditional decoction pieces (on) with mobile decoction pieces (descending) alcohol extract mirror image HPLC comparison diagram.
Figure 10 be traditional decoction pieces (on) with mobile decoction pieces (descending) alcohol extract mirror image HPLC comparison diagram.
Figure 11 be medicated powder (on) with high-temperature process 8h after (descending) alcohol extract mirror image HPLC comparison diagram.
Figure 12 be traditional decoction pieces (on) with mobile decoction pieces (descending) alcohol extract mirror image HPLC comparison diagram.
Figure 13 be traditional decoction pieces (on) with mobile decoction pieces (descending) alcohol extract mirror image HPLC comparison diagram (part).
The specific embodiment
Through specific embodiment, technical scheme of the present invention is further specified below.The mobile decoction pieces of the Herba Verbenae of the following stated (ball blast) all makes with the inventive method; The tradition decoction pieces is according to " Chinese pharmacopoeia was stipulated in the version to make in 2010.
Herba Verbenae tradition decoction pieces is pulverized, sieved, screened part is not crushed to all through 80 mesh sieves repeatedly.The medicated powder pre-treatment: high-temperature process is 4 hours in 95 ℃ of baking ovens, fully enzyme denaturing.Technical process: medicated powder after the pre-treatment and water are pressed the mixed of 1:2.2, get soft material, granulate (mesh size 1.0mm); Wet granular places centrifugal finisher,pill ball blast (rotating speed 500rpm; Time 20min), make wet ball blast and put into air dry oven, dry under≤80 ℃ temperature.Taking-up is placed to room temperature, sieves, and gets 10 ~ 24 purpose ball blasts, promptly gets the mobile decoction pieces (ball blast) of Herba Verbenae.
Herba Verbenae tradition decoction pieces is pulverized, sieved, screened part is not crushed to all through 85 mesh sieves repeatedly.The medicated powder pre-treatment: high-temperature process is 4 hours in 95 ℃ of baking ovens, fully enzyme denaturing.Technical process: medicated powder after the pre-treatment and water are pressed the mixed of 1:2.2, get soft material, granulate (mesh size 1.0mm); Wet granular places centrifugal finisher,pill ball blast (rotating speed 500rpm; Time 30min), make wet ball blast and put into air dry oven, dry under 80 ℃ of temperature.Taking-up is placed to room temperature, sieves, and gets 10 ~ 24 purpose ball blasts, promptly gets the mobile decoction pieces (ball blast) of Herba Verbenae.
Herba Verbenae tradition decoction pieces is pulverized, sieved, screened part is not crushed to all through 75 mesh sieves repeatedly.The medicated powder pre-treatment: high-temperature process is 5 hours in 95 ℃ of baking ovens, fully enzyme denaturing.Technical process: medicated powder after the pre-treatment and water are pressed the mixed of 1:2.2, get soft material, granulate (mesh size 1.0mm); Wet granular places centrifugal finisher,pill ball blast (rotating speed 500rpm; Time 20min), make wet ball blast and put into air dry oven, dry under the temperature about 70 ℃.Taking-up is placed to room temperature, sieves, and gets 10 ~ 24 purpose ball blasts, promptly gets the mobile decoction pieces (ball blast) of Herba Verbenae.
Mobile decoction pieces (ball blast) the optimal process parameter experiment of embodiment Herba Verbenae
1, crushing process
Herba Verbenae tradition decoction pieces pulverize separately is become the powder of different meshes, sieve, screened part is not pulverized repeatedly, to all through screen cloth, must 60 orders, 80 orders, 100 order powder, and carry out the trial-production of mobile decoction pieces.The result shows that 60 order powder fiber contents are too high, in pelletization, is difficult to extrude, and can not become ball; Though 100 purpose powder can become ball, more because of rhizome in the medical material, it is more to pulverize the back fiber, crosses 100 mesh sieves, the crushing screening process wastes time and energy repeatedly, influences process.Attempt directly carrying out the preparation of ball blast, but, become ball less because of the too much pelletization of fiber content is difficult to extrude with pulverizing the unsifted medicated powder in back.
Take all factors into consideration, final definite 80 order medicated powder of selecting carry out the preparation of ball blast.
2, the preferred optimised process of orthogonal test
With amount of water, to throw between bowlder and throw the circle rotating speed be the investigation factor, adopts three factors, three horizontal L
9(3
4) the orthogonal experiment design, specifically see table 1.Total content with roundness, target yield, oleanolic acid and ursolic acid is an index, carries out the optimization screening of process conditions.
Table 1 quadrature factor level table
Experimental result: can know that by range analysis directly perceived in scope of experiment, each horizontal size that influences of investigating factor is followed successively by amount of water>throw between bowlder throwing circle rotating speed.To factor A, III
A＞II
A＞I
AFactor B, I
B＞III
B＞II
BFactor C, II
C＞I
C＞III
CCan know that by variance analysis in scope of experiment, each horizontal size that influences of investigating factor also is an amount of water>throw between bowlder throwing circle rotating speed, wherein the amount of water factor has the significance influence, influence that there are no significant between throwing circle rotating speed and throwing bowlder.Analysis-by-synthesis, factor A are chosen level 3, and factor B chooses level 1, and factor C chooses level 2, and optimised process is A
3B
1C
2
The optimised process of the mobile decoction pieces of Herba Verbenae (ball blast) is: standard 80 order medicated powder, water addition ratio example 1:2.2 throws circle rotating speed 500rpm, throws 20min between bowlder, 80 ℃ of oven dry.Through demonstration test, stablize feasible.
The Quality Control parameter of the mobile decoction pieces of embodiment Herba Verbenae
1, micromeritis character
(1) the roundness ball blast that takes a morsel at random places on the bright and clean smooth glass plate; One side of plate is lifted, write down respectively that ball blast begins to roll, half rolls, the angle of glass plate and horizontal plane when all rolling, average; Angle is more little, and the roundness of ball blast is good more.Every duplicate samples is surveyed 6 times, obtains meansigma methods.The result: the roundness meansigma methods of ball blast is 16.3 °, 14.3 ° ~ 17.3 ° of fluctuation ranges.
(2) angle of repose the fixed funnel method; Be about to funnel and be fixed in graph paper (paper is positioned on the horizontal stand) top certain altitude; Adding material from funnel just contacts with funnel bottom up to the accumulation circular cone top that forms; Measure cone diameter, calculate angle of repose as tangent value with hopper base height and circular cone radius ratio.Every duplicate samples is surveyed 6 times, obtains meansigma methods.The result: meansigma methods angle of repose of ball blast is 31.4 °, 30.4 ° ~ 32.5 ° of fluctuation ranges.
(3) friability is got the mobile decoction pieces of about 3g Herba Verbenae, and precision is weighed, and puts in the friabilator, rotates 100 times.Take out, cross No. 2 and screen out powder, precision is weighed, and subtracts weight loss/former weight * 100%, calculates friability.Every duplicate samples is surveyed 6 times, obtains meansigma methods.The result: the friability meansigma methods is 0.42%, fluctuation range 0.26% ~ 0.56%.
(4) bulk density is got the mobile decoction pieces (ball blast) of Herba Verbenae, gets the 50ml volumetric flask, weighs, add sample in volumetric flask to graduation mark.Weigh, obtain bulk density by formula d=m/V.Every duplicate samples is surveyed 6 times, obtains meansigma methods.The result: the meansigma methods of bulk density is 0.335g/cm
3, fluctuation range 0.328 g/cm
3~ 0.342 g/cm
3Because of the more reason of the fiber of medical material own, the ball blast quality is lighter, and density is less, thinks that the bulk density of the mobile decoction pieces of Herba Verbenae (ball blast) must not be less than 0.30 g/cm
3
2, moisture, total ash, acid-insoluble ash
(1) moisture is got the mobile decoction pieces (ball blast) of Herba Verbenae, according to " an appendix IX of Chinese pharmacopoeia version in 2010 H first method is measured water content." Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and decoction pieces item regulation moisture down must not surpass 10.0%, and the watered pill must not surpass 9.00%, and measuring the result is 4.15% ~ 5.77%, up to specification.
(2) total ash is got the mobile decoction pieces (ball blast) of Herba Verbenae, according to " an appendix IX of Chinese pharmacopoeia version in 2010 K method is measured." Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and decoction pieces item regulation total ash down must not surpass 12.0%, and measuring the result is 9.18% ~ 9.57%, up to specification.
(3) acid-insoluble ash is got the mobile decoction pieces (ball blast) of Herba Verbenae, according to " an appendix IX of Chinese pharmacopoeia version in 2010 K method is measured." Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and decoction pieces item regulation acid-insoluble ash down must not surpass 4.0%, and measuring the result is 1.93% ~ 2.19%, up to specification.
3, HPLC assay
" total amount with oleanolic acid and ursolic acid under Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and the decoction pieces item is the assay index, and the regulation total amount must not be lower than 0.30%.Measure the total amount of oleanolic acid, ursolic acid in the mobile decoction pieces of Herba Verbenae (ball blast) according to its following method.
Measuring the result according to HPLC illustrated in figures 1 and 2 can know: the total amount meansigma methods of oleanolic acid, ursolic acid is 0.4423% in the mobile decoction pieces of Herba Verbenae (ball blast), meets " Chinese pharmacopoeia version regulation in 2010.
The contrast of the mobile decoction pieces of embodiment Herba Verbenae (ball blast) and traditional decoction pieces
1, outward appearance
As shown in Figure 3, Herba Verbenae tradition decoction pieces is irregular section.The stem square column type, there is longitudinal furrow at the four sides, and surperficial green and brown color is coarse.Tangent plane has marrow or hollow.How broken leaf is, green and brown color, and complete person flattens rear blade 3 drastic cracks, and there is sawtooth at the edge.Spike has Xiao Hua most.Feeble QI, bitter in the mouth.
As shown in Figure 4, the mobile decoction pieces of Herba Verbenae (ball blast) is the ball shape granule of coffee-like color, and size evenly has certain roundness, and the surface is more smooth, good fluidity, and hands is pinched non-friable.Feeble QI, bitter in the mouth.
2, microscopical identification
The microscopic features of Herba Verbenae tradition decoction pieces and mobile decoction pieces (ball blast) are relatively seen Fig. 5, and the microscopic features of Herba Verbenae tradition decoction pieces and mobile decoction pieces meet there was no significant difference basically.
3, thin layer is differentiated
According to " Chinese pharmacopoeia Herba Verbenae medical material of version in 2010 and decoction pieces item be regulation down, is that reference substance carries out thin layer and differentiates with the ursolic acid, require in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the speckle of apparent same color.As shown in Figure 6, the result: the chromatograph and the ursolic acid of Herba Verbenae tradition decoction pieces and mobile decoction pieces (ball blast) show the same color speckle at same position.Both TLC differentiate no marked difference.
4, the total solid of decocting liquid
Get Herba Verbenae tradition decoction pieces and each 10 g of the mobile decoction pieces of Herba Verbenae (ball blast), add 200 ml water, soak 30 min, decoct and maintenance boiling 30 min; Filter, medicinal residues add entry 200 ml once more, decoct and maintenance boiling 30 min, filter; Merging filtrate is put coldly, measures its volume.
Precision pipettes each 50ml of decocting liquid respectively, puts in the evaporating dish that is dried to constant weight, and water bath method is put in 105 ℃ of baking ovens and is dried to constant weight, and accurate the title decides, and calculates the yield of solid content.Parallel 3 parts, average.The result is as shown in table 2.
The solid content of table 2 Herba Verbenae tradition decoction pieces and mobile decoction pieces (ball blast) decocting liquid relatively
| Sample | The volume (ml) of total decocting liquid | The weight (g) of average solid content | Yield (%) |
| The tradition decoction pieces | 352.2 | 0.1555 | 10.95 |
| Mobile decoction pieces | 352.3 | 0.2156 | 15.19 |
Can know that by table 2 decocting rate of the mobile decoction pieces of Herba Verbenae is higher than traditional decoction pieces.The mobile decoction pieces of ball shape is beneficial to the fried of composition more.
5, the HPLC of decocting liquid analyzes
As shown in Figure 7, chemical constituent does not have significant change in the decocting liquid of the mobile decoction pieces of Herba Verbenae and traditional decoction pieces.
6, the HPLC of alcohol extract analyzes
When (1) medicated powder does not carry out pre-treatment
Herba Verbenae medicated powder when crossing the high temperature enzyme denaturing, prepare mobile decoction pieces (descend) and traditional decoction pieces (on) the alcohol extract finger printing contrast as shown in Figure 8.
Can be known that by last figure mobile decoction pieces prepares and lost a plurality of chemical constituents in the process, is mostly phenylpropyl alcohol glucosides class material, wherein maximum with the loss of verbascoside, iridoid glycosides material halberd leaf verbenalin also has loss.
(2) after the high temperature enzyme denaturing is handled
The pre-treatment process of medicated powder is handled 4h for continuing under 75 ℃ of high temperature.
After carrying out the medicated powder pre-treatment, prepare mobile decoction pieces, and carry out the contrast of finger printing with the alcohol extract of traditional decoction pieces, as shown in Figure 9.The result shows, processes ball blast through the medicated powder that the high temperature enzyme denaturing is handled, and can farthest keep the equity of chemical constituent, and promptly verbascoside content reduces approximately 9%, and all the other compositions do not have significant change.
The pre-treatment research (deactivation of glycosides enzyme) of embodiment medicated powder
Experimental result shows that after undressed 80 order Herba Verbenae medicated powder were prepared into ball blast, chemical constituent has tangible loss, is mostly phenylpropyl alcohol glucosides class material, and was wherein maximum with the loss of verbascoside.
For reducing the loss of chemical constituent, each step of technical process is investigated, find that the loss process of chemical constituent occurs in initial blend step.Because of the chemical constituent of loss is the glycoside material, doubt to due to the effect of glycosides enzyme, so, guarantee the equity of ball blast front and back chemical constituent, the used medicated powder of ball blast has been carried out pre-treatment, with deactivation glycosides enzyme for reducing the loss of chemical constituent.
1, ethanol soaks vexed enzyme denaturing
(1) concentration of alcohol is investigated and is got 95% ethanol; Be mixed with 70%, 80%, 95% ethanol respectively; Ratio according to every 100g medicated powder 30ml alcoholic solution adds (consider the cost problem, alcoholic acid addition can not be too high) mixing, and medicated powder is fully soaked; Seal, dry ethanol after soaking vexed certain hour.
Medicated powder with after handling prepares ball blast, and relatively its finger printing is shown in figure 10 with traditional decoction pieces, and the result shows that the loss with chemical constituent after 95% Ethanol Treatment reduces.But verbascoside content still reduces about 30%.
(2) soak vexed time investigation and get 95% ethanol, add according to the above ratio in the medicated powder, soak vexed 2h, 4h, 6h, 8h oven dry respectively, the preparation ball blast.Compare its finger printing, the result shows indifference.So soaking the vexed time does not have influence to the result.
2, high temperature enzyme denaturing
(1) the temperature investigation is got Herba Verbenae 80 order medicated powder and is placed 60 ℃, 75 ℃, 85 ℃, 95 ℃, 105 ℃ baking ovens respectively, the different time sampling, and the preparation ball blast compares finger printing with traditional decoction pieces.The result shows that 95 ℃, 105 ℃ enzyme denaturing effects are better, about the requirement of watered pill baking temperature, for keeping the stable of volatile ingredient, selects 95 ℃ of enzyme denaturing for use in the consideration pharmacopeia.
(2) the time investigation is got Herba Verbenae 80 order medicated powder and is placed 95 ℃ of baking oven high temperature enzyme denaturing, and the different time sampling is carried out the comparison of finger printing with medicated powder behind the high temperature enzyme denaturing and former medicated powder; See Figure 11; The result shows in lasting 95 ℃ of high temperature 8h, chemical constituent no change in the medicated powder, and medicated powder is stable.
The medicated powder that different time is taken out prepares ball blast, and with traditional decoction pieces finger printing relatively, the result shows pill behind the high temperature 2h, and chemical constituent also has loss; Pill behind the high temperature 4h loses less; Pill collection of illustrative plates indistinction behind high temperature 4h ~ 8h, the chemical constituent extent of damage is suitable.After being high-temperature process 4h, reach optimum efficiency, see Figure 12.It is about 9% that the content of verbascoside reduces, and all the other compositions do not have significant change.
3, high temperature adds the alcohol leaching enzyme denaturing
It is an amount of to get Herba Verbenae 80 order medicated powder, respectively according to method under above-mentioned alcohol leaching and the high temperature item, get after a medicated powder elder generation alcohol leaching again through the high temperature enzyme denaturing, behind the first high temperature of another part again through the alcohol leaching enzyme denaturing.With two parts of medicated powder pills, carry out the fingerprint contrast with traditional decoction pieces, investigate the variation that chemical constituent becomes.Show according to the result of Figure 13, two parts of ball blast indifferences, it is about 9% that the content of comparing verbascoside with traditional decoction pieces all reduces, identical with the effect of high temperature enzyme denaturing.
Comprehensive above result, and consider technology cost problem, the best pre-treatment process of medicated powder is handled 4h for continuing under 95 ℃ of high temperature, can farthest keep the equity of chemical constituent.
It is an amount of to get Herba Verbenae 80 order medicated powder, behind above-mentioned requirements high temperature enzyme denaturing, and the preparation ball blast; And repeat 3 batches, and carry out the fingerprint contrast with traditional decoction pieces, the situation of change of chemical constituent conforms to The above results as a result; It is about 9% to be that the content of verbascoside reduces, the content there was no significant difference of all the other compositions.
Above-described embodiment is a kind of preferable scheme of the present invention, is not that the present invention is done any pro forma restriction, under the prerequisite that does not exceed the technical scheme that claim puts down in writing, also has other variant and remodeling.
Claims (5)
1. the mobile decoction pieces of a Herba Verbenae is characterized in that it is prepared from following method:
A, pulverizing medicinal materials: the Herba Verbenae after Herba Verbenae tradition decoction pieces or arrangement selected is pulverized, and crosses 75～85 mesh sieves, obtains medicated powder;
B, medicated powder enzyme denaturing: medicated powder enzyme denaturing in 95～105 ℃ of baking ovens is handled more than 4 hours;
The preparation of c, ball blast: with the medicated powder after the pre-treatment with must soft material after an amount of water mixes, granulation, wet granular places the finisher,pill ball blast; The wet ball blast that makes is dry under≤80 ℃ of temperature, is placed to room temperature after the taking-up, sieves; Get 10 ~ 24 purpose ball blasts, promptly get the mobile decoction pieces of Herba Verbenae.
2. the method for preparing of the mobile decoction pieces of the described Herba Verbenae of a claim 1 is characterized in that may further comprise the steps:
A, pulverizing medicinal materials: the Herba Verbenae after Herba Verbenae tradition decoction pieces or arrangement selected is pulverized, and crosses 75～85 mesh sieves, obtains medicated powder;
B, medicated powder enzyme denaturing: medicated powder enzyme denaturing in 95～105 ℃ of baking ovens is handled more than 4 hours;
The preparation of c, ball blast: with the medicated powder after the pre-treatment with must soft material after an amount of water mixes, granulation, wet granular places the finisher,pill ball blast; The wet ball blast that makes is dry under≤80 ℃ temperature, is placed to room temperature after the taking-up, sieves; Get 10 ~ 24 purpose ball blasts, promptly get the mobile decoction pieces of Herba Verbenae.
3. method for preparing according to claim 2 is characterized in that: b is in the step, and medicated powder enzyme denaturing in 95～105 ℃ of baking ovens was handled 4～5 hours.
4. method for preparing according to claim 2 is characterized in that: c goes on foot medicated powder and water after the described pre-treatment by the mixed of 1:2～2.2.
5. method for preparing according to claim 2 is characterized in that: c goes on foot described ball blast process parameter for throwing circle rotating speed 500rpm, throws 20～25min between bowlder.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102986948A (en) * | 2012-12-02 | 2013-03-27 | 湖南金拓天油茶科技开发有限公司 | Preparation method of oil-tea camellia flower combined tea bags |
| CN103271986A (en) * | 2013-04-27 | 2013-09-04 | 浙江中医药大学 | Boiling pill of longtube ground ivy herb formula, and preparation technology thereof |
| CN103316065A (en) * | 2013-05-10 | 2013-09-25 | 浙江中医药大学中药饮片有限公司 | Dandelion fluid decoction pieces and preparation method thereof |
| CN103349679A (en) * | 2013-06-08 | 2013-10-16 | 浙江中医药大学中药饮片有限公司 | Mulberry leaf fluid decoction tablets and preparation method thereof |
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| CN101757043A (en) * | 2010-01-22 | 2010-06-30 | 浙江中医药大学中药饮片厂 | Liquid traditional Chinese medicine decoction piece and preparation method thereof |
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| CN101757043A (en) * | 2010-01-22 | 2010-06-30 | 浙江中医药大学中药饮片厂 | Liquid traditional Chinese medicine decoction piece and preparation method thereof |
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| 丛晓东，张云，杜伟锋，蔡保昌: "《中药流动性饮片的制备与传统饮片的比较》", 《中华中医药学会中药炮制分会2008年学术研讨会论文集》, 31 December 2008 (2008-12-31), pages 227 - 232 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102986948A (en) * | 2012-12-02 | 2013-03-27 | 湖南金拓天油茶科技开发有限公司 | Preparation method of oil-tea camellia flower combined tea bags |
| CN103271986A (en) * | 2013-04-27 | 2013-09-04 | 浙江中医药大学 | Boiling pill of longtube ground ivy herb formula, and preparation technology thereof |
| CN103316065A (en) * | 2013-05-10 | 2013-09-25 | 浙江中医药大学中药饮片有限公司 | Dandelion fluid decoction pieces and preparation method thereof |
| CN103349679A (en) * | 2013-06-08 | 2013-10-16 | 浙江中医药大学中药饮片有限公司 | Mulberry leaf fluid decoction tablets and preparation method thereof |
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