CN104147124A - Drying method of cortex magnoliae officinalis - Google Patents

Abstract

The invention relates to a drying method of cortex magnoliae officinalis. Fresh cortex magnoliae officinalis is slightly steamed and is placed in stacks at a shade and damp place. The cortex magnoliae officinalis is subjected to a "sweating" process until color of an internal surface turns into purple-brown or brown. A freeze-drying process is carried out until sublimation is finished. The cortex magnoliae officinalis is packaged in a sealing manner. Prepared cortex magnoliae officinalis is high in contents of various active ingredients. The method is low in energy consumption and is stable in product quality.

Description

A kind of drying means of Cortex Magnoliae Officinalis

Invention field

The present invention relates to medicine method for making, particularly a kind of drying means of Cortex Magnoliae Officinalis, belongs to medical technical field.

Background technology

Traditional Chinese medicine drying has very long history in China, the Chinese herbal medicine of drying can keep certain medicinal ingredient and be difficult for putrid and deteriorated, the dry important measures as guaranteeing Chinese herbal medicine quality, it is a requisite technical process in Chinese herbal medicine processing, it is in close relations that dry and Chinese medicine are produced, and dry method will directly affect the quality of product.

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 drying means that the object of this invention is to provide a kind of Cortex Magnoliae Officinalis, Cortex Magnoliae Officinalis prepared by the method, main effective ingredient magnolol honokiol, volatile oil and alkaloid are high, and energy consumption is low.

The object of the present invention is achieved like this:

A drying means for Cortex Magnoliae Officinalis, is characterized in that: get fresh Cortex Magnoliae Officinalis, and after micro-steaming, the dark and damp place of banking up, diaphoresis is during to inner surface purpling brown or sepia, and lyophilizing to distillation finishes.

The drying means of a kind of Cortex Magnoliae Officinalis of the present invention, is characterized in that: it is to be refrigerated to below-20 ℃ that lyophilizing to distillation finishes, be evacuated to below drying chamber pressure 30Pa, and subliming by heating, the temperature of distillation is controlled at below 40 ℃, to distilling, finishes.

The drying means of a kind of Cortex Magnoliae Officinalis of the present invention, is characterized in that: a kind of judgement of distillation in finishing by the following method 1. serviceability temperature Sensor monitoring temperature of charge judge whether the ice in material all distils; 2. condenser temperature drops to the state before distillation; 3. the pressure drop of freeze drying box is to the pressure that approaches cryoprobe.

So far completed the present invention.Cortex Magnoliae Officinalis prepared by the method, main effective ingredient magnolol, honokiol and alkaloid are high, and energy consumption is low.

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 to the distillation of banking up after steaming finishes: 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 ℃, to distillation end.

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, the dry Cortex Magnoliae Officinalis Magnolol and Honokiol content comparison 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
Lyophilizing to the distillation of banking up after steaming finishes	5.64	3.57	9.21
				Lyophilizing	3.24	2.27	5.51

By table 1, found out, the Cortex Magnoliae Officinalis lyophilizing of banking up after steaming finishes to distillation, and Magnolol and Honokiol and total phenol content dry and lyophilizing apparently higher than banking up after steaming.Magnolol and Honokiol is the main effective ingredient of Cortex Magnoliae Officinalis, and Cortex Magnoliae Officinalis clinical efficacy prepared by known the inventive method is good.

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
Lyophilizing to the distillation of banking up after steaming finishes	0.37
		Lyophilizing	0.12

By table 2, found out, the Cortex Magnoliae Officinalis lyophilizing of banking up after steaming finishes to distillation, and Cortex Magnoliae Officinalis alkaloid dries and lyophilizing apparently higher than banking up after steaming.It is relevant that Cortex Magnoliae Officinalis cures mainly distension and fullness of the chest and abdomen and contained magnocurarine (magnocurarine) etc., Cortex Magnoliae Officinalis treatment distension and fullness of the chest and abdomen good effect prepared by known the inventive method.

Three, the dry Cortex Magnoliae Officinalis friability comparison of distinct methods

1, instrument friability somascope, analytical balance, hair-dryer.

2, inspection method

The rotating speed that regulates instrument before 2.1 adjusting instrument speed tests is per minute 25 to turn ± 1 turn, and setting test period is 4 minutes, and the total degree of rotary drum is 100 times.

10 of test sample decoction pieces are got in the each test of the amount of taking of 2.2 test samples, with hair-dryer, blow away surperficial powder, precise weighing.

2.3 check

Test sample after above-mentioned weighed weight is put in cylinder, started motor and rotate 100 times.After rotation finishes, check test sample shatter number, then blow away after powder with hair-dryer, accurate claim kind, be the weight of less loss with the difference of the amount of taking, calculate percentage ratio.

3, result, is shown in 3.

Table 3 different dry drying method Cortex Magnoliae Officinalis friability

?	Shatter (%)	Less loss amount (%)
			After steaming, bank up and dry	Nothing	1.42
Lyophilizing to the distillation of banking up after steaming finishes	Nothing	1.41
			Lyophilizing	2	2.76

Table 3 result is known, and the lyophilizing of banking up finishes Cortex Magnoliae Officinalis to distillation, and antivibration wear resistant ability is better than the lyophilizing Cortex Eucommiae, and product is non-friable, and storage, transportation easily keep decoction pieces shape, constant product quality.

The specific embodiment

embodiment 1

Get fresh Cortex Magnoliae Officinalis, after micro-steaming, the dark and damp place of banking up, when diaphoresis becomes sepia to inner surface, put in freeze dryer, be refrigerated to-15 ℃, be evacuated to drying chamber pressure 60Pa, subliming by heating, sublimation temperature is controlled at 40 ℃, and when the ice in serviceability temperature Sensor monitoring temperature of charge judgement material all distils, distillation finishes, take out, pack.

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, put in freeze dryer, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 50Pa, subliming by heating, sublimation temperature is controlled at 50 ℃, to distillation end, during state before condenser temperature drops to distillation, distillation finishes, and takes out, and packs.

embodiment 3

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-28 ℃, be evacuated to drying chamber pressure 45Pa, subliming by heating, the temperature of distillation is controlled at 50 ℃, when the pressure drop of freeze drying box is when approaching the pressure of cryoprobe, and distillation end, take out, pack.

Claims (3)

1. a drying means for Cortex Magnoliae Officinalis, is characterized in that: get fresh Cortex Magnoliae Officinalis, and after micro-steaming, the dark and damp place of banking up, diaphoresis is during to inner surface purpling brown or sepia, and lyophilizing to distillation finishes, and packs.

2. according to the drying means of a kind of Cortex Magnoliae Officinalis of claim 1, it is characterized in that: it is to be refrigerated to below-20 ℃ that lyophilizing to distillation finishes, be evacuated to below drying chamber pressure 30Pa, subliming by heating, the temperature of distillation is controlled at below 40 ℃, to distilling, finishes.

3. according to the drying means of a kind of Cortex Magnoliae Officinalis of claim 1, it is characterized in that: a kind of judgement of distillation in finishing by the following method 1. serviceability temperature Sensor monitoring temperature of charge judge whether the ice in material all distils; 2. condenser temperature drops to the state before distillation; 3. the pressure drop of freeze drying box is to the pressure that approaches cryoprobe.