CN104147123A

CN104147123A - Freeze-drying method of cortex magnoliae officinalis

Info

Publication number: CN104147123A
Application number: CN201410418489.4A
Authority: CN
Inventors: 赵颖; 王丽; 刘金磊; 石红艳
Original assignee: Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
Current assignee: Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
Priority date: 2014-08-25
Filing date: 2014-08-25
Publication date: 2014-11-19

Abstract

The invention relates to a freeze-drying method of cortex magnoliae officinalis. The freeze-drying method comprises the steps: taking fresh cortex magnoliae officinalis, micro-steaming, then stacking in a dark and moist place, sweating until the inner surface becomes purple brown or tan, and freeze-drying. The prepared cortex magnoliae officinalis comprises main effective components of magnolol, honokiol, alkaloid and an extract having high contents, and thus the clinical effect is known to be better.

Description

A kind of freeze drying process of Cortex Magnoliae Officinalis

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.

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, the Cortex Magnoliae Officinalis of the method lyophilizing, main effective ingredient magnolol honokiol, alkaloid and extract content are high, and then known clinical effectiveness is better.

The object of the present invention is achieved like this:

A freeze drying process for Cortex Magnoliae Officinalis, gets fresh Cortex Magnoliae Officinalis, after micro-steaming, and 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.

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) 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;

2) 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, " diaphoresis " is during to inner surface sepia, 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.

3) 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 steaming, bank up and dry	4.51	3.42	7.93
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 steaming ", Magnolol and Honokiol and total phenol content are apparently higher than " 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 steaming, bank up and dry	0.25
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 steaming ", Cortex Magnoliae Officinalis alkaloid is apparently higher than " 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 extractum rate comparison of distinct methods

Chemical composition of Chinese materia medica is complicated, mainly with decoction, takes, and clinical efficacy is the result of multicomponent comprehensive function, and the content Chang Zuowei of water solublity and ethanol-soluble extractives evaluates the comprehensive judge index of drug quality height.

Adopt one of < < Chinese Pharmacopoeia > > version in 2010, appendix XA method is carried out the assay of water solublity and ethanol-soluble extractives.Wherein alcohol extract solvent adopts 70% ethanol.The Cortex Magnoliae Officinalis extractum rate result that distinct methods is dry, in Table 3.

The Cortex Magnoliae Officinalis extractum rate measurement result (%) that table 3 distinct methods is dry

Sample	After steaming, bank up and dry	The lyophilizing of banking up after steaming	Lyophilizing
				Water extraction	18.63	27.52	17.87
Alcohol extract	12.58	18.65	11.97

Table 3 finds out, the Cortex Magnoliae Officinalis lyophilizing of banking up after boiling, and the content of water solublity and ethanol-soluble extractives all dries and lyophilizing higher than banking up after boiling, and illustrates that the lyophilizing effective ingredient leaching rate of banking up after Cortex Magnoliae Officinalis is boiled is high.

The specific embodiment

embodiment 1

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-20 ℃, 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 60 ℃, to dry.

embodiment 2

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 3

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-10 ℃, 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 50 ℃, to dry.

Claims

1. a freeze drying process for Cortex Magnoliae Officinalis, gets fresh Cortex Magnoliae Officinalis, after micro-steaming, and 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, lyophilizing is to be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 30Pa, and subliming by heating, the temperature of distillation is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.