CN104173445A - Method for lyophilizing magnolia officinalis - Google Patents
Method for lyophilizing magnolia officinalis Download PDFInfo
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- CN104173445A CN104173445A CN201410418727.1A CN201410418727A CN104173445A CN 104173445 A CN104173445 A CN 104173445A CN 201410418727 A CN201410418727 A CN 201410418727A CN 104173445 A CN104173445 A CN 104173445A
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- magnoliae officinalis
- lyophilizing
- cortex magnoliae
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Abstract
The invention relates to a method for lyophilizing magnolia officinalis. The method comprises the following steps: slightly boiling or steaming fresh magnolia officinalis in boiling water; piling in a dark place, and sweating until the inner surface turns purple brown or dark brown; and lyophilizing. The prepared magnolia officinalis is high in content of multiple active components, and has a relatively good curative effect when being used for treating enteroplegia.
Description
Invention field
The present invention relates to medicine method for making, particularly a kind of freeze drying process of Cortex Magnoliae Officinalis, belongs to medical technical field.
Background technology
Cortex Magnoliae Officinalis is the dry root bark of Magnoliacea plant Cortex Magnoliae Officinalis (Magnolia officinalisREHD et), branch skin and dried bark, for conventional Chinese medicine, there is dampness expectorant, the therapeutic method to keep the adverse QI flowing downwards except full effect, for humidity hysteresis damaging the spleen and stomach, the vomiting and diarrhoea of gastral cavity painful abdominal mass, stagnation of QI due to dyspepsia, abdominal distention constipation, the phlegm retention disease such as breath with cough.The good medicine for the treatment of gastroenteropathy, it is again the primary raw material of multiple Chinese patent medicine, Cortex Magnoliae Officinalis is mainly containing lignan component (Magnolol and Honokiol), volatile oil (being mainly eucalyptus oil), alkaloid (being mainly magnocurarine) etc., in order to guarantee the quality of Cortex Magnoliae Officinalis, Cortex Magnoliae Officinalis dried bark after going through edition < < Chinese Pharmacopoeia > > and all stipulating to gather should be put in boiling water after micro-boiling, the dark and damp place of banking up, diaphoresis is during to inner surface purpling brown or sepia, steams softly, takes out, be rolled into tubular, dry.
Vacuum lyophilization claims again lyophilizing, can preserve to greatest extent the activity of effective medicinal components, keeps preferably exterior quality, color, the abnormal smells from the patient of medical material, and thoroughly, keeping quality is good in dehydration.The object of vacuum lyophilization is to preserve to greatest extent fresh the effective elements of the medicine, makes it active suitable with fresh medicine.We find to get fresh Cortex Magnoliae Officinalis, and its various active component content of lyophilizing is not high.
At present in the processing in production place of Cortex Magnoliae Officinalis, except pressing the diaphoresis method processing of < < Chinese Pharmacopoeia > > regulation, many places of production adopt the method without " diaphoresis " convection drying, and adopt " diaphoresis " to process, its " diaphoresis " method is also different, also have and steam rear " diaphoresis ", multiple " diaphoresis " such as sealings " diaphoresis " put in thick type packaging bag in shredding, and also exists at present Cortex Magnoliae Officinalis whether to need the difference of " diaphoresis ".For above problem, the inventor compares research to main effective ingredient magnolol honokiol and volatile oil and alkaloid in the Cortex Magnoliae Officinalis of different processing methods, has proposed a kind of new freeze drying process.
Summary of the invention
The object of this invention is to provide the freeze drying process that a kind of Cortex Magnoliae Officinalis is new, the Cortex Magnoliae Officinalis of the method lyophilizing, main effective ingredient magnolol honokiol, volatile oil and alkaloid are high, are used for the treatment of enteroparalysis effective.
The object of the present invention is achieved like this:
A freeze drying process for Cortex Magnoliae Officinalis, gets fresh Cortex Magnoliae Officinalis, put in boiling water micro-boil or micro-steaming after, the dark and damp place of banking up, diaphoresis is to inner surface purpling brown or sepia, lyophilizing.
The freeze drying process of a kind of Cortex Magnoliae Officinalis of the present invention, lyophilizing is to be refrigerated to below-20 ℃, is evacuated to below drying chamber pressure 30Pa, subliming by heating, the temperature of distillation is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
The application of Cortex Magnoliae Officinalis prepared by the freeze drying process of a kind of Cortex Magnoliae Officinalis of the present invention, is characterized in that: be used for the treatment of enteroparalysis.
So far completed the present invention, the freeze drying process of a kind of Cortex Magnoliae Officinalis of the present invention, is different from the lyophilizing of prior art, and the lyophilizing of prior art is to get the direct lyophilizing of fresh medicine.The present invention gets fresh Cortex Magnoliae Officinalis, put in boiling water micro-boil or micro-steaming after, the dark and damp place of banking up, diaphoresis is during to inner surface purpling brown or sepia, lyophilizing, the Cortex Magnoliae Officinalis various active component content of preparation is high, is used for the treatment of enteroparalysis effective.
Below by test example, further illustrate usefulness of the present invention, test example is intended to further illustrate usefulness of the present invention, but not limitation of the present invention.
To, with a collection of fresh Cortex Magnoliae Officinalis, process by the following method.
1) bank up after boiling and dry: the fresh trunk bark of Cortex Magnoliae Officinalis is put in boiling water after micro-boiling, and the dark and damp place of banking up, when " diaphoresis " becomes sepia to inner surface, spreads out and dry.
2) after steaming, bank up and dry: by after the micro-steaming of the fresh trunk bark of Cortex Magnoliae Officinalis, the dark and damp place of banking up, when " diaphoresis " becomes sepia to inner surface, spreads out and dry.
3) lyophilizing of banking up after boiling: the fresh trunk bark of Cortex Magnoliae Officinalis is put in boiling water after micro-boiling, the dark and damp place of banking up, when " diaphoresis " becomes sepia to inner surface, be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 30Pa, subliming by heating, sublimation temperature is controlled at below 40 ℃, resolution temperature is controlled at below 45 ℃, to dry.
4) lyophilizing of banking up after steaming: the fresh trunk bark of Cortex Magnoliae Officinalis is put in boiling water after micro-boiling, the dark and damp place of banking up, when " diaphoresis " becomes sepia to inner surface, be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 30Pa, subliming by heating, sublimation temperature is controlled at below 40 ℃, resolution temperature is controlled at below 45 ℃, to dry.
5) lyophilizing: be refrigerated to-20 ℃, reach after cryogenic temperature, be evacuated to below drying chamber pressure 30Pa, subliming by heating, sublimation temperature is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
One, Magnolol and Honokiol content comparison in the dry Cortex Magnoliae Officinalis of distinct methods
Method according to defined under Cortex Magnoliae Officinalis item of < < Chinese Pharmacopoeia > > version in 2010 is carried out HPLC mensuration to the magnolia medicament of different dry drying method, the results are shown in Table 1.
Table 1 distinct methods is dried Cortex Magnoliae Officinalis Magnolol and Honokiol content (%)
| Drying means | Magnolol | Honokiol | Total phenol content |
| After boiling, bank up and dry | 4.43 | 3.34 | 7.77 |
| After steaming, bank up and dry | 4.51 | 3.42 | 7.93 |
| The lyophilizing of banking up after boiling | 5.73 | 3.65 | 9.38 |
| The lyophilizing of banking up after steaming | 5.62 | 3.56 | 9.18 |
| Lyophilizing | 3.24 | 2.27 | 5.51 |
By table 1, found out, Cortex Magnoliae Officinalis " lyophilizing of banking up after boiling " or " lyophilizing of banking up after steaming ", Magnolol and Honokiol and total phenol content are apparently higher than " bank up and dry after boiling ", " bank up and dry after steaming " and " lyophilizing ".Magnolol and Honokiol is the main effective ingredient of Cortex Magnoliae Officinalis, Cortex Magnoliae Officinalis good effect prepared by known the inventive method.
Two, the dry Cortex Magnoliae Officinalis alkaloid comparison of distinct methods
According to appendix of < < Chinese Pharmacopoeia > > version in 2010, titration in nonaqueous solvent is measured.
1, the preparation of 0.02mol/L perchloric acid titration liquid and demarcation: according to preparing under appendix of Chinese Pharmacopoeia version in 2010 " 0.1mol/L perchloric acid titration liquid " item and demarcating, must test perchloric acid concentration used is 0.019mol/L.
2, the preparation of sample: get the about 1.0g of testing sample powder (by No. four sieves), accurately weighed, to put in tool plug conical flask, precision adds methanol 40mL, weighed quality, shakes up, and room temperature is placed and spent the night, more weighed quality, supply the quantity of solvent of loss, after jolting, place, with filter paper, filter.Precision measures subsequent filtrate 10 mL, puts evaporate to dryness in water-bath.
3, alkaloidal mensuration: residue adds anhydrous glacial acetic acid 15mL to be made to dissolve, and adds 1 of crystal violet indicator solution, is titrated to blueness with perchloric acid titration liquid (0.02mol/L), calculates and get final product.The results are shown in Table 2.
Table 2 distinct methods is dried Cortex Magnoliae Officinalis alkaloid (%)
| Drying means | Alkaloid |
| After boiling, bank up and dry | 0.25 |
| After steaming, bank up and dry | 0.25 |
| The lyophilizing of banking up after boiling | 0.35 |
| The lyophilizing of banking up after steaming | 0.34 |
| Lyophilizing | 0.12 |
By table 2, found out, Cortex Magnoliae Officinalis " lyophilizing of banking up after boiling " and " lyophilizing of banking up after steaming ", Cortex Magnoliae Officinalis alkaloid is apparently higher than " bank up and dry after boiling ", " bank up and dry after steaming " and " lyophilizing ".It is relevant to contained magnocurarine (magnocurarine) etc. that Cortex Magnoliae Officinalis cures mainly distension and fullness of the chest and abdomen, Cortex Magnoliae Officinalis good effect prepared by known the inventive method.
Three, the dry Cortex Magnoliae Officinalis volatile oil content comparison of distinct methods
According to appendix of < < Chinese Pharmacopoeia > > version in 2010, under determination of volatile oil item, measure.
Every duplicate samples is got respectively 200g, accurately weighed, puts in 2000mL flask, adds water 1200Ml, after shaking up, connects volatile oil determination apparatus and condensing tube.Autocondensation pipe upper end Jia Shui makes to be full of the scale part of volatile oil determination apparatus, and overflow while entering flask till, put in electric jacket and be slowly heated to boil, and keep micro-about 5h that boils, no longer increase to oil mass in determinator, stop heating, place a moment, open the piston of determinator lower end, water is slowly emitted, above oil reservoir upper end arrives scale 0 line till 5mm place, more than placing 2h, then opening piston, to make oil reservoir drop to its upper end just concordant with scale 0 line, reads volatilization oil mass, and calculate the amount of volatile oil in test sample, the results are shown in Table 3.
Table 3 distinct methods is dried Cortex Magnoliae Officinalis volatile oil content (mL/g)
| Drying means | Volatile oil content |
| After boiling, bank up and dry | 0.15 |
| After steaming, bank up and dry | 0.19 |
| The lyophilizing of banking up after boiling | 0.28 |
| The lyophilizing of banking up after steaming | 0.26 |
| Lyophilizing | 0.17 |
By table 3, found out, Cortex Magnoliae Officinalis " lyophilizing of banking up after boiling " and " lyophilizing of banking up after steaming ", the Cortex Magnoliae Officinalis that volatile oil content is prepared apparently higher than " bank up and dry after boiling ", " bank up and dry after steaming " and " lyophilizing ", especially higher than lyophilizing Cortex Magnoliae Officinalis, known the inventive method has advance.
Four, the dry Cortex Magnoliae Officinalis treatment Postoperative enteroparalysis curative effect comparison of distinct methods.
1, data and method
1.1 cases: 50 surgical postoperative enteroparalysis patients, are divided into 5 groups, every group 10 examples of preparation at random.Being respectively banks up after Cortex Magnoliae Officinalis is boiled dries group, bank up after steaming dry group, the lyophilizing group of banking up after boiling, bank up after steaming lyophilizing group, lyophilizing group.There is by analysis comparability.
1.2 Therapeutic Method: each organizes case, are all decocted in water for oral dose, 1 12g, and 3 times on the one 3 days was 1 course for the treatment of.
2, criterion of therapeutical effect and result
2.1 criterions of therapeutical effect: gastrointestinal functions resumed (mainly comparing passage of gas by anus time of occurrence).
2.2 therapeutic effect: each organizes Stomach in Patients intestinal function recovery (passage of gas by anus time of occurrence) relatively in Table 4.
Table 4 distinct methods is dried Cortex Magnoliae Officinalis clinical efficacy (mL/g)
| Group | Average micturition time (h) |
| After boiling, bank up and dry group | 43.75 |
| After steaming, bank up and dry group | 43.56 |
| The lyophilizing group of banking up after boiling | 20.32 |
| The lyophilizing group of banking up after steaming | 20.34 |
| Lyophilizing group | 45.32 |
By table 4, found out, Cortex Magnoliae Officinalis " the lyophilizing group of banking up after boiling " and " the lyophilizing group of banking up after steaming ", clinical efficacy is significantly better than " bank up after boiling and dry group ", " bank up after steaming and dry group " and " lyophilizing group ".
The specific embodiment
embodiment 1
Get fresh Cortex Magnoliae Officinalis, put in boiling water after micro-boiling, the dark and damp place of banking up, diaphoresis is during to inner surface purpling brown, put in freeze dryer, be refrigerated to-20 ℃, be evacuated to drying chamber pressure 30Pa, subliming by heating, sublimation temperature is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 2
Get fresh Cortex Magnoliae Officinalis, put in boiling water after micro-boiling, the dark and damp place of banking up, when diaphoresis becomes sepia to inner surface, put in freeze dryer, be refrigerated to-28 ℃, be evacuated to drying chamber pressure 50Pa, subliming by heating, sublimation temperature is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 3
Get fresh Cortex Magnoliae Officinalis, put in boiling water after micro-boiling, the dark and damp place of banking up, when diaphoresis becomes sepia to inner surface, put in freeze dryer, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 50Pa, subliming by heating, sublimation temperature is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 4
Get fresh Cortex Magnoliae Officinalis, put in boiling water after micro-boiling the dark and damp place of banking up, diaphoresis is during to inner surface purpling brown, put in freeze dryer, be refrigerated to-25 ℃, be evacuated to drying chamber pressure 60Pa, start heater switch, promote distillation, the temperature of distillation is controlled at 40 ℃, to distillation end, resolution temperature is controlled at below 45 ℃, to dry.
embodiment 5
Get fresh Cortex Magnoliae Officinalis, after micro-steaming, the dark and damp place of banking up, diaphoresis is during to inner surface purpling brown, put in freeze dryer, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 60Pa, subliming by heating, sublimation temperature is controlled at 40 ℃, and to distillation end, resolution temperature is controlled at below 45 ℃, to dry.
embodiment 6
Get fresh Cortex Magnoliae Officinalis, after micro-steaming, the dark and damp place of banking up, when diaphoresis becomes sepia to inner surface, puts in freeze dryer, is refrigerated to-32 ℃, is evacuated to drying chamber pressure 50Pa, subliming by heating, and sublimation temperature is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 7
Get fresh Cortex Magnoliae Officinalis, after micro-steaming, the dark and damp place of banking up, diaphoresis during to inner surface purpling brown, is put in freeze dryer, is refrigerated to-28 ℃, is evacuated to drying chamber pressure 50Pa, subliming by heating, the temperature of distillation is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
Claims (3)
1. a freeze drying process for Cortex Magnoliae Officinalis, is characterized in that: get fresh Cortex Magnoliae Officinalis, put in boiling water micro-boil or micro-steaming after, the dark and damp place of banking up, diaphoresis is to inner surface purpling brown or sepia, lyophilizing.
2. according to the freeze drying process of a kind of Cortex Magnoliae Officinalis of claim 1, it is characterized in that: lyophilizing is to be refrigerated to below-20 ℃, is evacuated to below drying chamber pressure 30Pa, subliming by heating, the temperature of distillation is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
3. the application of the Cortex Magnoliae Officinalis of preparing according to the freeze drying process of a kind of Cortex Magnoliae Officinalis of claim 1, is characterized in that: be used for the treatment of enteroparalysis.
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| CN201410418727.1A CN104173445A (en) | 2014-08-25 | 2014-08-25 | Method for lyophilizing magnolia officinalis |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101332235A (en) * | 2008-01-07 | 2008-12-31 | 四川新荷花中药饮片有限公司 | Magnolia bark and processing technique |
| CN103285086A (en) * | 2013-07-04 | 2013-09-11 | 江西中医学院 | Novel processing method of gingered Mangnolia officinalis |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101332235A (en) * | 2008-01-07 | 2008-12-31 | 四川新荷花中药饮片有限公司 | Magnolia bark and processing technique |
| CN103285086A (en) * | 2013-07-04 | 2013-09-11 | 江西中医学院 | Novel processing method of gingered Mangnolia officinalis |
Non-Patent Citations (3)
| Title |
|---|
| 刘元慧等: "厚朴饮片不同加工工艺的比较研究", 《时珍国医国药》 * |
| 沈丕安: "《中药不良反应与临床》", 31 October 2007, 第二军医大学出版社 * |
| 胡丽萍等: "高效液相色谱法测定不同厚朴饮片中厚朴酚含量及厚朴姜制原理的研究", 《中国中药杂志》 * |
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Application publication date: 20141203 |