CN102266437A - Vacuum freeze-drying process of callicarpa leaf and preparation process of callicarpa leaf powder - Google Patents
Vacuum freeze-drying process of callicarpa leaf and preparation process of callicarpa leaf powder Download PDFInfo
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Abstract
The invention discloses a vacuum freeze-drying process of callicarpa leaf and a preparation process of callicarpa leaf powder. The vacuum freeze-drying process of the callicarpa leaf comprises the following steps: (1) selecting raw materials; (2) cleaning: quickly leaching the callicarpa leaf; (3) pre-drying: pre-drying the callicarpa leaf till water content is 60-70%; (4) loading onto a plate and pre-freezing: loading the pre-dried callicarpa leaf onto the plate, and gradually cooling for 2-3 hours, and then pre-freezing at the temperature of (-20)-(-40) DEG C, wherein the loading weigh is 2.7-4 kg/m<2> and the loading thickness is 2-3 cm; (5) sublimation drying: vacuumizing until the absolute pressure of the system is 100 Pa, entering a heating process, raising the shed temperature to 40-70 DEG C while controlling the vacuum degree at 55-65 Pa, and carrying out sublimation drying for 10-15 hours; and (6) desorption drying: maintaining the material temperature at 20-50 DEG C and discharging when the water content is below 3%. In the vacuum freeze-drying process of the callicarpa leaf disclosed by the invention, the vacuum freezing time, temperature, pressure and other parameters are reasonably set, so that the pharmaceutically active ingredients are maximally maintained.
Description
Technical field
The invention belongs to Chinese medicine fabricating technology field, be specifically related to a kind of Chinese medicine Folium Callicarpae Formosanae vacuum lyophilization and keep the technology of drug activity composition and the preparation technology of Folium Callicarpae Formosanae powder.
Background technology
Folium Callicarpae Formosanae is the dried leaves of Verenaceae plant callicarpa pedunculata Callicarpa formosana Rolfe, plucks drying when summer, autumn, two seasons, branch and leaf were luxuriant.Fresh leaf sheet oblong, ellipse or ovum shape ellipse, long 4～19cm, wide 2.5～9cm, tip be point or blunt circle gradually, wide wedge shape of base portion or blunt circle, edge tool serration.Dried leaves is the broken strand shape that curls, and is different in size; Upper surface celadon or brown-green are by stellate hair or short and thick hair; Lower surface light green or light brown green, close by yellowish-brown stellate hair and golden yellow gland point, master pulse and lateral vein are outstanding, and scun stretches into increment.
Folium Callicarpae Formosanae nature and flavor hardship, puckery, cool is returned liver, lung, stomach warp, and it has the removing heat from blood astringing to arrest bleeding, the effect of dissipating blood stasis removing toxic substances and promoting subsidence of swelling; Be used for epistaxis, spitting of blood, spit blood, have blood in stool, metrorrhagia, traumatic hemorrhage, pathopyretic ulcer, burn due to hot liquid or fire.For oral administration: as to fry in shallow oil soup, 3～15g (bright product 30～60g); Or grind into powder and swallow, each 1.5～3g.External: smash and apply or grind into powder and spread.Folium Callicarpae Formosanae is a kind of Callicarpa plant of being rich in bioactive substance, and main component is flavonoid, terpenoid, condensed tannin, still contains trace element such as resinene, saccharide, hydroxy compounds and magnesium, calcium, ferrum.
The pharmacologically active of Folium Callicarpae Formosanae has been reported hemostasis, anti peroxidation of lipid, analgesia, antibacterial and antitumor etc.1. anastalsis: pharmacological research finds that Folium Callicarpae Formosanae has strong contraction intestinal smooth muscle, shortens the effect of bleeding stopping period.By discovering that callicarpa pedunculata has obvious anastalsis, hemostatic mechanism is an increased platelets counts, and this also is the hemorrhage pharmacological basis of treatment thrombocytopenic.2. lipoid peroxidization resistant; 3. antibacterial action: the bacteriostasis of callicarpa cathayana Chang and callicarpa pedunculata has been carried out experiment relatively, find the two has height to staphylococcus aureus and Salmonella bacteriostasis, Candida albicans, Bacillus typhi and dysentery bacterium are had stronger bacteriostasis, and both do not have significant difference.4. antitumor action.5. analgesic activity: adopt the acetic acid twisting method that the analgesic activity of Folium Callicarpae Formosanae is studied, the result shows that the Folium Callicarpae Formosanae ethanol extract has significant analgesia role to mice, 6 monomer components that separation is obtained have also carried out activity rating, experiment shows that triterpenoid of this plant and flavone compound have shown good analgesic activity, but its mechanism of action is still indeterminate.
Beginning of Folium Callicarpae Formosanae sees supplement to the Herbal, meaning: " just ripe to autumn, purple circle is given birth between woods pool, the east of a river as globule." author of " Chinese medicine voluminous dictionary " book thinks that contained its former plant of Folium Callicarpae Formosanae of supplement to the Herbal is callicarpa pedunculata.Also collected in the version in 2010 at the Pharmacopoeia of the People's Republic of China.Clinical prescription is selected for use: it is hemorrhage 1. to treat the intestines and stomach: dried Folium Callicarpae Formosanae end 3～5 minutes.Transfer cold boiled water, clothes were 1 time in per 4 hours; Continue with dried Folium Callicarpae Formosanae end two money, decocting is often drunk (" Fujian traditional herbal medicine ") for tea.2. treatment spitting of blood: dried Folium Callicarpae Formosanae end 5～7 minutes.Transfer Ovum Gallus domesticus album, clothes were 1 time in per 4 hours; Continue with dried Folium Callicarpae Formosanae end two money, decocting is often drunk (" Fujian traditional herbal medicine ") for tea.3. treat wound hemorrhage: bright Folium Callicarpae Formosanae, clean with cold boiled water, smash even back and apply wound; Or grind into powder to apply with dried Folium Callicarpae Formosanae and mix, the external sterilizing gauze is wrapped up it (" Fujian traditional herbal medicine ").4. treat epistaxis: dried Folium Callicarpae Formosanae two money.Accent Ovum Gallus domesticus album clothes; The external sterilizing Cotton Gossypii is dipped in Ye Mosai nose (" Fujian traditional herbal medicine ").
The Folium Callicarpae Formosanae traditional diamond-making technique is removed impurity after plucking usually, cleans, and cuts off drying.Drying means is substantially for drying or drying.But in traditional drying or concocting process, effective ingredient very easily runs off or is destroyed, thereby has obviously reduced drug effect and active component; More very important is that its water content of the exsiccant Folium Callicarpae Formosanae of employing traditional method almost reaches 15%, very easily goes mouldy, and is difficult for storing and utilizing.
Summary of the invention
The invention provides the vacuum lyophilization of a kind of Chinese medicine Folium Callicarpae Formosanae and can keep the technology of drug activity composition and the preparation technology of Folium Callicarpae Formosanae powder.Chinese medicine Folium Callicarpae Formosanae vacuum freeze-drying technique of the present invention takes time, temperature, the pressure and other parameters to vacuum freezing to carry out reasonable configuration, thereby makes the drug effect active component obtain maximum reservation.
The present invention takes following technical scheme: the vacuum lyophilization of Chinese medicine Folium Callicarpae Formosanae keeps the technology of drug activity composition, comprise choose Folium Callicarpae Formosanae raw material, cleaning, predrying, sabot is freezing, sublimation drying, parsing-desiccation, concrete steps are as follows:
1) raw material is chosen: choose fresh Folium Callicarpae Formosanae raw material, take out inferior, impurity;
2) clean: quick drip washing Folium Callicarpae Formosanae;
3) predrying: that Folium Callicarpae Formosanae is predrying to water content 60～70%;
4) sabot pre-freeze: pre-dried Folium Callicarpae Formosanae is carried out sabot, and sabot weight is 2.7～4kg/m
2, thickness 2～3cm after lowering the temperature gradually 2～3 hours, carries out pre-freeze at-20 ℃～-40 ℃ temperature conditions;
5) sublimation drying: the system absolute pressure of being evacuated to is 100Pa, enters heating process, and vacuum keeps 55～65Pa, and the canopy temperature is warming up to 40 ℃～70 ℃, sublimation drying 10～15 hours;
This step is an important operation in the Folium Callicarpae Formosanae vacuum lyophilization process, and in the drying sublimation stage, material need absorb heat (every gram ice is sublimed into the heat that steam absorbs 2.8 Kilojoule approximately fully).If medicine is not heated or shortage of heat, then moisture can absorb the heat of medicine itself and the temperature of medicine is reduced when distillation, causes the vapour pressure of medicine to reduce, so cause the reduction of rate of sublimation, the whole exsiccant time will prolong, and productivity ratio descends; If to medicine heating too much, the rate of sublimation of medicine no doubt can improve, but after having offset the heat that the medicine distillation absorbed, unnecessary heat can make the temperature of freezing medicine itself rise, make whole dry the failure.
Because the particularity of Chinese medicine Folium Callicarpae Formosanae, if temperature is too high, effective ingredient or activity are with destroyed, therefore, take following steps with head it off: the system absolute pressure of being evacuated to is 100Pa, enters heating schedule, vacuum keeps 55～65Pa, heating canopy temperature is warming up to 40 ℃～70 ℃, sublimation drying 10～15 hours, and this is a sublimation drying step in the Folium Callicarpae Formosanae vacuum freezing process.
6) parsing-desiccation: keep temperature of charge at 20 ℃～50 ℃, make water content reach back discharging below 3%.
Preferably, the 5th) in the step, sublimation drying: vacuum keeps 60Pa.
No matter on profile or volume, all very nearly the same with fresh medical material the vacuum lyophilization of Folium Callicarpae Formosanae crude drug is handled the back finished product and described: the Folium Callicarpae Formosanae medical material after the lyophilization can not produce any contraction.One is frozen exsiccant Folium Callicarpae Formosanae and can presents cellular appearance at microscopically, very easily grinding.
Through the Folium Callicarpae Formosanae of vacuum freeze-drying technique, can preserve the active ingredient of former medicine and the performance of going back crude drug in whole to greatest extent, taking dose is little, and active component is lost few, and curative effect is more definite.After testing, with a collection of fresh Folium Callicarpae Formosanae, use the Folium Callicarpae Formosanae main component verbascoside (C of vacuum freeze-drying technique
29H
36O
15) content be 1～5 times of traditional drying technology.
After adopting the Folium Callicarpae Formosanae vacuum freeze-drying technique to handle, its water content can reach below 3%, is difficult for going mouldy, damaging by worms, and helps storing and utilizing.
The invention also discloses a kind of preparation technology of Folium Callicarpae Formosanae powder, will carry out levigation, physical wall breaking, discharging dehumidifying packing, sterilization, make the Folium Callicarpae Formosanae powder, can make oral formulations through the Folium Callicarpae Formosanae that aforementioned vacuum freeze-drying technique is handled.
Preferably: 1) levigation: the Folium Callicarpae Formosanae material is ground, cross 100 mesh sieves.2) physical wall breaking adopts two strands of ultrasonic air-flows that the Folium Callicarpae Formosanae powder is clashed under the hermetically drying state, and sporoderm-broken rate reaches 98%.3) discharging dehumidifying packing will be carried out in the constant temperature dehumidification workshop, in order to avoid the material suction is made moist.4) sterilization stores.
The present invention has realized the oral safe edible grade standard of Folium Callicarpae Formosanae decoction pieces by quick drip washing, cryogenic vacuum lyophilization, physics cell ultra micro wall breaking technology, dehumidifying packing back sterilization treatment.
It is that full medicine is taken that Folium Callicarpae Formosanae is processed into peroral dosage form, can save the dose more than 70%, and process levigation breaking cellular wall makes the more abundant absorption of performance of drug effect, and the dehumidifying packing is that the Folium Callicarpae Formosanae mildew-resistant behind the guarantee vacuum lyophilization levigation breaking cellular wall is guaranteed the quality.Therefore, the Folium Callicarpae Formosanae oral formulations room temperature of prepared of the present invention is given birth to the edible way that clothes are the tool medical values of Folium Callicarpae Formosanae.
Chinese medicine processing pharmaceutically occupies very consequence in motherland, we can say the quality of Chinese medicine processing, directly the effect of influence treatment disease.Vacuum Freezing ﹠ Drying Technology (abbreviation freeze drying technology) is under vacuum low-temperature environment, and research is by the science of diabatic process, characteristics and rule inside and outside the freeze-dried material, and it is a complex technology interdisciplinary.In the last few years, the application of freeze drying technology in high-technology field extremely people paid close attention to, but the Chinese medicine lyophilizing does not also come into one's own at home, only be confined at present the lyophilizing of a small amount of Chinese crude drug such as Radix Ginseng, Cornu Cervi Pantotrichum, Rhizoma Dioscoreae, Cordyceps, a large amount of Chinese crude drugs has been lost most effective ingredient or active component in common or traditional dry run.In today of modernization of Chinese medicine develop rapidly, the active component of Chinese crude drug or effective ingredient also do not have the clear and definite stage, and Chinese crude drug adopts the more active component that 1. at utmost kept medical material of benefit of freeze drying technology; 2. realize easily quantitatively accurately; 3. realize the asepticize operation easily; 4. the medicine loss and waste is few; 5. the rehydration performance is good; 6. taking convenience; 7. medicine never degenerates, and is suitable for long-term storage.Chinese medicine Folium Callicarpae Formosanae vacuum freeze-drying technique of the present invention to keeping drug effect and active component thereof, is saved natural resources of Chinese medicinal materials, promotes the modernization of Chinese medicine, for new road has been opened up in the development of traditional Chinese medicine.
Description of drawings
Fig. 1 is the process chart of Folium Callicarpae Formosanae vacuum lyophilization of the present invention.
Fig. 2 is the process chart of prepared Folium Callicarpae Formosanae oral formulations of the present invention.
Fig. 3 is the operating curve figure of a kind of preferred embodiment of Folium Callicarpae Formosanae vacuum freeze-drying technique of the present invention.
The specific embodiment
Embodiment 1
Adopt vacuum freeze drier to carry out Folium Callicarpae Formosanae vacuum lyophilization.
As shown in Figure 1, choose fresh Folium Callicarpae Formosanae raw material, impurity, poor quality and dead leaves such as the debranching tip; Drip washing fast; Folium Callicarpae Formosanae is predrying to water content 70%; Pre-dried Folium Callicarpae Formosanae is carried out sabot, and sabot weight is 2.7kg/m
2, thickness 2cm ,-20 ℃～-40 ℃ are carried out pre-freeze after lowering the temperature gradually 2～3 hours; Being evacuated to system's absolute pressure then is 100Pa, enters heating schedule, and vacuum keeps 55～65Pa, and the canopy temperature is warming up to 65 ℃, sublimation drying 15 hours; Keep temperature of charge at 35 ℃ again, make water content reach back discharging below 2%.
As shown in Figure 2, the Folium Callicarpae Formosanae after previous process steps carries out physical wall breaking behind 100 mesh sieves excessively by levigation, under the hermetically drying state, adopts two strands of ultrasonic air-flows that the Folium Callicarpae Formosanae powder is clashed into, and sporoderm-broken rate reaches 98%.
Advance after the physical wall breaking Folium Callicarpae Formosanae packing back sterilization that dehumidifies in the constant temperature dehumidification workshop, made peroral dosage form, but long preservation.
Embodiment 2
Adopt vacuum freeze drier to carry out Folium Callicarpae Formosanae vacuum lyophilization.
Choose fresh Folium Callicarpae Formosanae raw material, impurity and dead leaves such as the debranching tip; Drip washing fast; Folium Callicarpae Formosanae is predrying to water content 60%; Pre-dried Folium Callicarpae Formosanae is carried out sabot, and sabot weight is 3kg/m
2, thickness 2.5cm ,-20 ℃～-40 ℃ are carried out pre-freeze after lowering the temperature gradually 2～3 hours; Being evacuated to system's absolute pressure then is 100Pa, enters heating schedule, and vacuum keeps 55～65Pa, and the canopy temperature is warming up to 40 ℃, sublimation drying 15 hours; Keep temperature of charge at 40 ℃ again, make water content reach back discharging below 3%.
Folium Callicarpae Formosanae after abovementioned steps passes through levigation, carry out physical wall breaking after crossing 100 mesh sieves, under the hermetically drying state, adopt two strands of ultrasonic air-flows that the Folium Callicarpae Formosanae powder is clashed into, sporoderm-broken rate reaches 98%, advanced after the physical wall breaking Folium Callicarpae Formosanae packing back sterilization that dehumidifies in the constant temperature dehumidification workshop, made peroral dosage form, also can make composite prescription with other prepared slices of Chinese crude drugs.
Embodiment 3
Adopt vacuum freeze drier to carry out Folium Callicarpae Formosanae vacuum lyophilization.
Choose fresh Folium Callicarpae Formosanae raw material, impurity and dead leaves such as the debranching tip; Drip washing fast; Folium Callicarpae Formosanae is predrying to water content 65%; Pre-dried Folium Callicarpae Formosanae is carried out sabot, and sabot weight is 3.5kg/m
2, thickness 3cm ,-20 ℃～-40 ℃ are carried out pre-freeze after lowering the temperature gradually 2～3 hours; Being evacuated to system's absolute pressure then is 100Pa, enters heating schedule, and vacuum reaches 65Pa, and the canopy temperature is warming up to 60 ℃, sublimation drying 12 hours; Keep temperature of charge at 50 ℃ again, make water content reach back discharging below 3%.
Folium Callicarpae Formosanae after abovementioned steps passes through levigation, carry out physical wall breaking after crossing 100 mesh sieves, under the hermetically drying state, adopt two strands of ultrasonic air-flows that the Folium Callicarpae Formosanae powder is clashed into, sporoderm-broken rate reaches 98%, advanced after the physical wall breaking Folium Callicarpae Formosanae packing back sterilization that dehumidifies in the constant temperature dehumidification workshop, made peroral dosage form, also can make composite prescription with other prepared slices of Chinese crude drugs.
Embodiment 4
Adopting Shenyang JDF-0.2 type vacuum freeze drier to carry out Folium Callicarpae Formosanae vacuum lyophilization handles.
As shown in Figure 1, choose fresh Folium Callicarpae Formosanae raw material, impurity and dead leaves such as the debranching tip; Drip washing fast; Folium Callicarpae Formosanae is predrying to water content 60%; Pre-dried Folium Callicarpae Formosanae is carried out sabot, and sabot weight is 4kg/m
2, thickness 3cm ,-20 ℃～-40 ℃ are carried out pre-freeze after lowering the temperature gradually 2～3 hours; Being evacuated to system's absolute pressure then is 100Pa, enters heating schedule, and vacuum reaches 60Pa, and the canopy temperature is warming up to 70 ℃, sublimation drying 14 hours; Keep temperature of charge at 40 ℃ again, make water content reach back discharging below 2%.
The parameter operating curve of the concrete technology of present embodiment as shown in Figure 3.
Bai Kang pharmaceutcal corporation, Ltd institute of materia medica, Zhejiang is detected effective ingredient by high performance liquid chromatography according to 2010 editions one one of the Pharmacopoeia of the People's Republic of China.From testing result as can be known, the Folium Callicarpae Formosanae of vacuum freeze-drying technique preparation of the present invention, main component verbascoside (C
29H
36O
15) content be 1～5 times of traditional drying technology.
Those of ordinary skill in the art will be appreciated that the present invention is not limited to the foregoing description, any conversion of the present invention, modification is all fallen into protection scope of the present invention.
Claims (6)
1. Folium Callicarpae Formosanae vacuum freeze-drying technique is characterized in that as follows:
(1) raw material is chosen: choose fresh Folium Callicarpae Formosanae raw material, take out inferior, impurity;
(2) clean: quick drip washing Folium Callicarpae Formosanae;
(3) predrying: that Folium Callicarpae Formosanae is predrying to water content 60～70%;
(4) sabot pre-freeze: with pre-dried Folium Callicarpae Formosanae sabot, sabot weight is 2.7～4kg/m
2, thickness 2～3cm after lowering the temperature gradually 2～3 hours, carries out pre-freeze under-20 ℃～-40 ℃ temperature;
(5) sublimation drying: the system absolute pressure of being evacuated to is 100Pa, enters heating process, and vacuum keeps 55～65Pa, and the canopy temperature is warming up to 40 ℃～70 ℃, sublimation drying 10～15 hours;
(6) parsing-desiccation: keep temperature of charge at 20 ℃～50 ℃, water content reaches back discharging below 3%.
2. Folium Callicarpae Formosanae vacuum freeze-drying technique as claimed in claim 1 is characterized in that: in (5) step, sublimation drying: vacuum keeps 60Pa.
3. the preparation technology of Folium Callicarpae Formosanae powder is characterized in that: will carry out levigation, physical wall breaking, discharging dehumidifying packing, sterilization through the Folium Callicarpae Formosanae of claim 1 or 2 vacuum freeze-drying techniques, and make the Folium Callicarpae Formosanae powder.
4. the preparation technology of Folium Callicarpae Formosanae powder as claimed in claim 3 is characterized in that: Folium Callicarpae Formosanae is ground, cross 100 mesh sieves.
5. the preparation technology of Folium Callicarpae Formosanae powder as claimed in claim 3 is characterized in that: physical wall breaking adopts two strands of ultrasonic air-flows that the Folium Callicarpae Formosanae powder is clashed under the hermetically drying state.
6. the preparation technology of Folium Callicarpae Formosanae powder as claimed in claim 3 is characterized in that: the discharging dehumidifying is packaged in the constant temperature dehumidification workshop and carries out.
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| CN105687207A (en) * | 2016-02-26 | 2016-06-22 | 江西省皮肤病专科医院 | Ointment for treating dermatitis and eczema and preparation method thereof |
| CN107865893A (en) * | 2016-09-27 | 2018-04-03 | 柳州昕霖科技有限公司 | A kind of lyophilized preparation technology of fresh goods strophanthus divaricatus |
| CN108576561A (en) * | 2018-03-14 | 2018-09-28 | 安徽金太阳食品有限公司 | A kind of Gluten drying and processing method |
| US20190381121A1 (en) * | 2018-06-18 | 2019-12-19 | Eric Young | Method of Drying Botanicals |
| CN111248426A (en) * | 2020-02-13 | 2020-06-09 | 中国热带农业科学院香料饮料研究所 | Leaf product of herba Epilobii and its preparation method |
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| CN103230434B (en) * | 2013-04-18 | 2015-04-15 | 杭州求本植物科技有限公司 | Manufacturing process of leonurus |
| CN105104644A (en) * | 2015-09-07 | 2015-12-02 | 文成县益禾农业科技有限公司 | Production technology of okra scented tea |
| CN105687207A (en) * | 2016-02-26 | 2016-06-22 | 江西省皮肤病专科医院 | Ointment for treating dermatitis and eczema and preparation method thereof |
| CN105687207B (en) * | 2016-02-26 | 2018-04-10 | 江西省皮肤病专科医院 | A kind of paste for being used for dermatitis, eczema and preparation method thereof |
| CN107865893A (en) * | 2016-09-27 | 2018-04-03 | 柳州昕霖科技有限公司 | A kind of lyophilized preparation technology of fresh goods strophanthus divaricatus |
| CN108576561A (en) * | 2018-03-14 | 2018-09-28 | 安徽金太阳食品有限公司 | A kind of Gluten drying and processing method |
| US20190381121A1 (en) * | 2018-06-18 | 2019-12-19 | Eric Young | Method of Drying Botanicals |
| US10639340B2 (en) * | 2018-06-18 | 2020-05-05 | Eric Young | Method of drying botanicals |
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