CN1813888A - Process for preparing fresh motherwort powder - Google Patents

Process for preparing fresh motherwort powder Download PDF

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CN1813888A
CN1813888A CN 200510004941 CN200510004941A CN1813888A CN 1813888 A CN1813888 A CN 1813888A CN 200510004941 CN200510004941 CN 200510004941 CN 200510004941 A CN200510004941 A CN 200510004941A CN 1813888 A CN1813888 A CN 1813888A
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fresh
powder
juice
herba leonuri
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CN100457138C (en
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王建国
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Zhejiang Dade Pharmaceutical Group Co Ltd
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Abstract

The present invention discloses a preparation process of Chinese medicine fresh leonurus powder. Said preparation process includes the following steps: cleaning fresh leonurus, cutting, pressing to make juice, collecting juice, sieving to obtain fresh leonurus juice, conveying the fresh leonurus juice into a container, making reduced pressure concentration at 45 plus or minus 5 deg.C to obtain the concentrate whose relative density is 1.04-10.6, spraying said concentrate or freeze-drying said concentrate so as to obtain the fresh leonurus powder.

Description

The preparation technology of fresh motherwort powder
Technical field
The present invention relates to a kind of preparation technology of Chinese medicine fresh motherwort powder.
Background technology
Herba Leonuri is that the herb of labiate Herba Leonuri Leconumus heterophyllus sweet is used as medicine with the full-bloom stage dry stem and leaf of gathering traditionally, now is stated from one one of version pharmacopeia in 2000.Have promoting blood flow to regulate menstruation, promoting tissue regeneration by removing blood stasis, the effect of inducing diuresis to remove edema is described as " gynecological's panacea ".Compendium of Material Medica is said: " removing blood stasis of invigorating blood circulation, regulating menstruation detoxifcation.Control the vaginal bleeding during pregnancy difficult labour, placenta retention ... " and for example " book on Chinese herbal medicine converge with sound " say: " promoting the circulation of blood is nourished blood, and fresh blood is not hindered in the tool promoting the circulation of blood, the blood stasis that do not stagnate that nourishes blood, really for the panacea of doctor family also." the motherwort formulation kind is more, to the treatment menorrhagia, menostaxis and postpartum lochiorrhea, metrorrhagia, artificial abortion, drug induced abortion, puerperal uterine atony, recover of uterus is bad to be used for many years, and records pharmacopeia.Present clinical common dosage forms has Herba Leonuri paste, ext leonuri sibirici liq, Herba Leonuri soup, Herba Leonuri compound preparation, Herba Leonuri granule, Herba Leonuri capsule etc.Its source of formula is in " Hui Zhitang is through proved recipe " volume four directions, now is stated from one one of Pharmacopoeia of the People's Republic of China version in 2000, and used crude drug is exsiccant Herba Leonuri, ubiquity technology is numerous and diverse, curative effect is not remarkable, and dose is big, takes problems such as inconvenience.It is that raw material is made preparation with bright product that bibliographical information is also arranged, for example document CN1456253A discloses a kind of preparation method of fresh Herba Leonuri sheet, key step comprises: get the fresh Herba Leonuri fragmentation, squeeze the juice, filter, being concentrated into relative density is 1.05~1.15 (60 ℃) spray drying, add right amount of auxiliary materials, mixing is granulated, tabletting, coating.Fresh Herba Leonuri juice concentrates the organic principles such as marennin that can destroy in the Herba Leonuri in this method under 60 ℃ temperature, the color burn that causes the Herba Leonuri concentrated solution, by green transition is brown, cause powder to darken, do not meet that the spissated relative density of Herba Leonuri grass juice factor is 1.05~1.15 in standard-required (standard code motherwort powder color for green) and this method, easy plug nozzle when the spray dry run.Document CN1055011C discloses a kind of preparation method of bright motherwort preparation, mainly may further comprise the steps: the fresh Herba Leonuri homogenate that will spend early stage, centrifugal filtration adds dextrin and stirs evenly, and is spray dried to medicated powder, makes medicament with the pharmaceutical methods of routine again.Before spray drying, add dextrin in this method and can cause powder to produce caking phenomenon, and the easy coking of dextrin, cause that breeze is arranged in the powder, and can cause powder content defective.
Summary of the invention
Technical problem to be solved by this invention is to avoid above-mentioned deficiency of the prior art, and proposes the preparation technology of the good fresh motherwort powder of a kind of steady quality.
Technical scheme provided by the present invention is: this technology includes following steps
Get fresh Herba Leonuri, clean, shred, squeeze the juice, collect juice, sieve, get fresh Herba Leonuri juice;
Fresh Herba Leonuri juice is delivered in the container, carries out concentrating under reduced pressure and get concentrated solution;
Concentrated solution directly sprayed or concentrated solution is carried out lyophilization promptly gets fresh motherwort powder, and described concentrating under reduced pressure process conditions are: temperature is 40 ℃~50 ℃.
Further, the relative density of described concentrated solution is 1.04~1.06.
Further, described conveying is carried for the pump line road.
Further, the inlet temperature of described spray process is 195 ℃~205 ℃, and outlet temperature is 95 ℃~105 ℃.
Further, described cryodesiccated pre-freeze temperature is-50 ℃~-30 ℃.
The present invention has following advantage: step is simple, and is easy to operate; Prepared product is satisfied the criteria, and good stability; Powder directly is evenly distributed, color even, and moisture-sensitive not, opaque amount are easy to control, and save operation, reduce adjuvant, have reduced product cost.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described.
Get fresh Herba Leonuri, clean, shred, squeeze the juice, collect juice, sieve, get fresh Herba Leonuri juice; Fresh Herba Leonuri juice is stored in the storage tank of chuck before concentrating, cooling medium is a water in the chuck, Herba Leonuri grass juice factor temperature remains on 3~10 ℃, can guarantee Herba Leonuri grass juice factor opaque amount like this, if fresh Herba Leonuri juice temperature is above 40 ℃, the powder color is bad, in time concentrate, thickening temperature can not surpass 50 ℃, concentrates back relative density 1.04~1.06 (45 ± 5 ℃ of temperature), can guarantee that like this powder color is up to specification, when spray drying, do not add adjuvants such as dextrin in the fresh Herba Leonuri juice, simplified operation, and guaranteed the quality of powder.In addition, the out temperature during spray drying is for the color and luster of powder, and temperature all has a significant impact, and the out temperature of strict control spray dryer can be controlled the color and luster of powder within the scope of the present invention well, improves the particle size distribution of powder, makes it reach standard.Be the textual criticism thickening temperature, concentrate relative density, out temperature etc. may influence the factor of opaque amount when whether adding dextrin and spray drying, we have done relevant contrast test (seeing Table 1), the result shows that temperature is obvious to the influence of fresh motherwort powder quality when concentrating, when temperature was higher than 50 ℃, color promptly can deepen, so the control temperature is being essential below 50 ℃.In theory, thickening temperature be lower than 40 ℃ also feasible, but consider energy consumption and production efficiency, so best thickening temperature is decided to be 40 ± 5 ℃.
Table 1 thickening temperature and concentrated solution color and powder color
Thickening temperature The concentrated solution color The powder color
35℃ Emerald green Green
40℃ Emerald green Green
45℃ Green Green
50℃ Green Green
55℃ Brown-green Brown-green
60℃ Brown-green Brown
65℃ Brown Brown
If adopt unconcentrated medicinal liquid to carry out spray drying, then the powder delivery yield only is 1.5~2.0kg/h, adopt concentrated solution carry out spray drying then the powder delivery yield rise to 6~7kg/h, concentrating capacity is about 1000L/h.(remarks: above data are relevant with bright herbaceous stem amount and concentrated solution relative density) concentrates and spray drying can be carried out simultaneously, shortened the production cycle greatly, reduced energy consumption.Test shows that concentrating relative density also is clearly (seeing Table 2) for the influence of the state of powder, and relative density is low excessively, then is prone to caking, too high then can plug nozzle, therefore, it also is essential concentrating and controlling relative density, and best relative density is 1.04~1.06.
Table 2 concentrated solution relative density and powdery attitude situation
Relative density The powdery condition Relative density The powdery condition
Unconcentrated Herba Leonuri grass juice factor Caking is arranged 1.05 Do not have caking, mealiness is good
1.01 Caking is arranged 1.06 Do not have caking, mealiness is good
1.02 Caking is arranged 1.07 Nozzle easily stops up
1.03 Caking is arranged 1.08 Nozzle easily stops up
1.04 Do not have caking, mealiness is good 1.09 Nozzle easily stops up
Find to add dextrin and can cause the powder caking phenomenon when the influencing of the amount that investigate to add adjuvant, and the easy moisture absorption, the easy coking of dextrin during spray drying produces breeze, and is also influential to product colour, and can cause powder content defective (standard for 〉=23mg/g).Do not add dextrin, then powder directly is evenly distributed, and color even does not have caking and breeze phenomenon (seeing Table 3) during not moisture-sensitive, and spray drying.The opaque amount is easy to control, and saves operation, reduces adjuvant, has reduced product cost.
Table 3 adds dextrin and opaque magnitude relation
Add the dextrin amount The powder appearance character Stachydrine hydrochloride content mg/g
On average
50% Powder has caking, and breeze is arranged, and the powder moisture-sensitive darkens 17.4 16.8 16.5 16.9
40% Powder has caking, and breeze is arranged, and the powder moisture-sensitive darkens 19.3 20.2 19.9 19.8
30% Powder has caking, and breeze is arranged, and the powder moisture-sensitive darkens 22.8 23.7 21.9 22.8
20% Powder has caking, and breeze is arranged, and the powder moisture-sensitive darkens 25.4 26.9 27.1 26.5
10% Powder has caking, and a little breeze is arranged, and the powder moisture-sensitive darkens 28.9 30.6 29.4 29.6
5% Powder has caking, and a little breeze is arranged, and the powder moisture-sensitive darkens 30.2 31.9 32.5 31.5
1% A little breeze is arranged, and the powder moisture-sensitive darkens 32.8 33.4 32.0 32.7
0% Do not have caking, color even is difficult for the moisture absorption 34.1 33.6 33.9 33.9
In addition, the utilization freeze drying process can be protected thermally labile sexual element in the Herba Leonuri to greatest extent, and can overcome difficulties such as the coking that can run into when conventional drying, powder diameter skewness, and is easy to the sterile working.Lyophilization efficient height, with short production cycle, be beneficial to the stable of maintenance product quality.
In addition preparation fresh Herba Leonuri capsule for treating postpartum subinvolution of uterus (syndrome of blood stasis) patient 60 examples made from the motherwort powder of gained of the present invention have been carried out clinical verification, wherein 30 examples are organized in treatment, the cure-remarkable-effectiveness rate of Clinical results Herba Leonuri capsule for treating postpartum subinvolution of uterus (syndrome of blood stasis) is 90.00%, total effective rate is 96.67%, matched group ext leonuri sibirici liq cure-remarkable-effectiveness rate is 63.33%, total effective rate is 86.67%, and the treatment group obviously is better than matched group (P<0.01).Do not see obvious adverse reaction in the clinical verification, obvious toxic-side effects is not seen in safety inspection.
Fresh Herba Leonuri capsule for treating menorrhagia (blood stasis type), Western medicine diagnose is ovulation type dysfunctional uterine bleeding 30 examples, with ext leonuri sibirici liq 30 examples, matched group is observed the untoward reaction of the capsular clinical efficacy of fresh Herba Leonuri, be 2 menstrual cycle observing time, the produce effects of wherein fully recovering patient followed up a case by regular visits to three months, show by clinical observation result, fresh Herba Leonuri capsule for treating menorrhagia cure-remarkable-effectiveness rate is 40%, total effective rate is 76.67%, is higher than contrast medicine ext leonuri sibirici liq (cure-remarkable-effectiveness rate is 23.33%, and total effective rate is 56.67%), but there was no significant difference is analysed in credit by statistics, does not all find side effect and untoward reaction for two groups.
Embodiment 1 spray drying prepares fresh motherwort powder
1.1, squeeze the juice: get fresh Herba Leonuri 1000kg and remove the foreign material weeds, drench cleaning machine, clean up through swing cleaning machine bubble, chaffcutter cutting after the vibration water-strainer dewaters, crusher in crushing is squeezed the juice, discard residue, collect juice, fresh Herba Leonuri juice filters through 60 eye mesh screens.
1.2, the Herba Leonuri grass juice factor concentrates: suck in the haplo-effect concentrator and concentrate, thickening temperature is controlled at 45 ± 5 ℃ and is concentrated into relative density 1.04~1.06 (45 ± 5 ℃)
1.3, spray drying: get concentrated solution and filter, carry out spray drying.The control parameter is that inlet temperature is 200 ± 5 ℃, and outlet temperature is 100 ± 5 ℃, collects dry powder, weighing and bagging, and the powder check contains moisture≤8.0%, and assay should be not less than 23mg/g in stachydrine hydrochloride.
Embodiment 2 lyophilizations prepare fresh motherwort powder
2.1, squeeze the juice: get fresh Herba Leonuri 1000kg and remove the foreign material weeds, drench cleaning machine, clean up through swing cleaning machine bubble, chaffcutter cutting after the vibration water-strainer dewaters, crusher in crushing is squeezed the juice, discard residue, collect juice, fresh Herba Leonuri juice filters through 60 eye mesh screens.
2.2, the Herba Leonuri grass juice factor concentrates: suck in the haplo-effect concentrator and concentrate, thickening temperature is controlled at 45 ± 5 ℃ and is concentrated into relative density 1.04~1.06 (45 ± 5 ℃)
2.3, lyophilization: get concentrated solution and filter, carry out lyophilization, the control parameter is that liquid layer thickness is 8mm, and phase I pre-freeze temperature be-40 ± 5 ℃, and second stage drying baffle temperature is ± 10 ℃, and pressure is 4Pa.Collect dry powder, weighing and bagging, the powder check contains moisture≤8.0%, and assay should be not less than 23mg/g in stachydrine hydrochloride.
Experimental example one: accelerated stability test
According to " two " stability test guideline " items of Chinese pharmacopoeia version in 2000 are pharmaceutical preparation accelerated test detailed rules and regulations down, carry out accelerated stability test.
Experimental condition: simulation street drug packing (aluminum-plastic composite membrane), 40 ℃ ± 2 ℃ of temperature, relative humidity 75% ± 5%.
Test method: by the three batch samples (lot number: 020301,020302,020303) of producing prescription, explained hereafter, under the commercially available back condition,, placed 6 months under relative humidity 75% ± 5% condition in 40 ± 2 ℃ of temperature, respectively at 1st month, the 2nd month, the 3rd month and the 6th the end of month, sampling and measuring detects (character, discriminating by stable high spot reviews project, assay, moisture, microbial limit) every index and the comparison of 0 month detection data, investigate its sample stability.
Investigation project: character, discriminating, assay, moisture, microbial limit.
Result of the test sees Table 4,5,6.
Experimental example two: long-time stability experiment
According to " two " stability test guideline " items of Chinese pharmacopoeia version in 2000 are pharmaceutical preparation accelerated test detailed rules and regulations down, carry out long-term stable experiment.
Experimental condition: simulation street drug packing (aluminum-plastic composite membrane), 25 ℃ ± 2 ℃ of temperature, relative humidity 60% ± 10%.
Test method: by the three batch samples (lot number: 020301,020302,020303) under the commercially available back condition, of producing prescription, explained hereafter in 25 ℃ ± 2 ℃ of temperature, relative humidity 60% ± 10%.
Placed 12 months under the condition, respectively at 1st month, the 2nd month, 3rd month, the 6th month, the 9th month and 12 the end of month, sampling and measuring detects (character by stable high spot reviews project, differentiate, assay, moisture, microbial limit) after 12 months, still need continue to investigate, respectively at 18th month, the 24th month sampling and measuring, every index and 0 month detection data are relatively investigated its sample stability.
Investigation project: character, discriminating, assay, moisture, microbial limit.
Result of the test sees Table 7,8,9.
Table 4, fresh motherwort powder accelerated stability test result ()
Sample title: fresh motherwort powder lot number: 020301
Figure A20051000494100091
Table 5, fresh motherwort powder accelerated stability test result (two)
Sample title: fresh motherwort powder lot number: 020302
Figure A20051000494100101
Table 6, fresh motherwort powder accelerated stability test result (three)
Sample title: fresh motherwort powder lot number: 020303
Table 7, fresh motherwort powder long-term stable experiment result ()
Sample title: fresh motherwort powder lot number: 020301
Table 8, fresh motherwort powder long-term stable experiment result (two)
Sample title: fresh motherwort powder lot number: 020302
Table 9, fresh motherwort powder long-term stable experiment result (three)
Sample title: fresh motherwort powder lot number: 020303

Claims (5)

1, a kind of preparation technology of fresh motherwort powder, this technology includes
Get fresh Herba Leonuri, clean, shred, squeeze the juice, collect juice, sieve, get fresh Herba Leonuri juice;
Fresh Herba Leonuri juice is delivered in the container, carries out concentrating under reduced pressure and get concentrated solution;
Concentrated solution directly sprayed or concentrated solution is carried out lyophilization promptly gets fresh motherwort powder,
It is characterized in that: described concentrating under reduced pressure process conditions are: temperature is 40 ℃~50 ℃.
2, the preparation technology of fresh motherwort powder according to claim 1 is characterized in that: the relative density of described concentrated solution is 1.04~1.06.
3, the preparation technology of fresh motherwort powder according to claim 1 is characterized in that: described conveying is carried for the pump line road.
4, the preparation technology of fresh motherwort powder according to claim 1 is characterized in that: the inlet temperature of described spray process is 195 ℃~205 ℃, and outlet temperature is 95 ℃~105 ℃.
5, the preparation technology of fresh motherwort powder according to claim 1 is characterized in that: described cryodesiccated pre-freeze temperature is-50 ℃~-30 ℃.
CNB2005100049413A 2005-01-31 2005-01-31 Process for preparing fresh motherwort powder Active CN100457138C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102058661B (en) * 2010-01-20 2013-05-08 浙江大德药业集团有限公司 Method for preparing fresh motherwort preparation
CN106377573A (en) * 2016-08-31 2017-02-08 宁夏多维药业有限公司 Preparation method of motherwort herb extract
CN109419712A (en) * 2017-09-03 2019-03-05 大德仟年生物技术有限公司 A kind of preparation method containing fresh leonurus and haematococcus pluvialis facial mask
CN109419713A (en) * 2017-09-03 2019-03-05 大德仟年生物技术有限公司 A kind of fresh leonurus ginseng beauty mask and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1569096A (en) * 2003-07-16 2005-01-26 浙江大德制药有限公司 Method for preparing fresh leonurus heterophyllus powder

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102058661B (en) * 2010-01-20 2013-05-08 浙江大德药业集团有限公司 Method for preparing fresh motherwort preparation
CN106377573A (en) * 2016-08-31 2017-02-08 宁夏多维药业有限公司 Preparation method of motherwort herb extract
CN109419712A (en) * 2017-09-03 2019-03-05 大德仟年生物技术有限公司 A kind of preparation method containing fresh leonurus and haematococcus pluvialis facial mask
CN109419713A (en) * 2017-09-03 2019-03-05 大德仟年生物技术有限公司 A kind of fresh leonurus ginseng beauty mask and preparation method thereof

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Denomination of invention: Preparation process of fresh motherwort powder

Effective date of registration: 20231222

Granted publication date: 20090204

Pledgee: CITIC Bank Co.,Ltd. Yiwu Branch

Pledgor: ZHEJIANG DADE PHARMACEUTICAL GROUP Co.,Ltd.

Registration number: Y2023330003084