CN104180614A

CN104180614A - Freeze-drying method for roots of red-rooted salvia

Info

Publication number: CN104180614A
Application number: CN201410418543.5A
Authority: CN
Inventors: 周宝艳; 李强; 赵建东; 杨龙飞
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: 2014-12-03

Abstract

The invention relates to a freeze-drying method for roots of red-rooted salvia. The freeze-drying method includes that the fresh roots of red-rooted salvia are selected to be freeze-dried till completion of sublimation and taken out for spreading cooling prior to sealed packaging. The prepared roots of red-rooted salvia are high in main active ingredients of danshinolic acid B and tanshinone II A, energy consumption is low, products are not easy to break, decoction pieces are easy to sustain in shape, and quality is stable.

Description

A kind of freeze drying process of the red sage root

Invention field

The present invention relates to medicine, particularly a kind of freeze drying process of the red sage root, belongs to medical technical field.

Background technology

The red sage root is the dry root and rhizome of the labiate red sage root, has stasis-dispelling and pain-killing, activating blood to promote menstruation, and the effects such as relieving restlessness that clear away heart-fire, are usually used in chest impediment and cardialgia, dysphoria and insomnia, irregular menstruation, the sore disease such as swell and ache.The active component of the red sage root mainly comprises taking tanshin polyphenolic acid B as main liposoluble ingredient, as protocatechuic acid, protocatechualdehyde, danshensu, caffeic acid, alkannic acid, Rosmarinic acid, salviandic acid A, tanshin polyphenolic acid B and salvianolic acid C etc., with the tanshinone component taking tanshinone IIA as master, as Cryptotanshinone, dihydrotanshinone Ⅰ, salvia miltiorrhiza bge I, Tanshinone II etc.

Freeze-drying is widely applied for fresh medicine new fresh keeping technique and processing method China.Freeze drying technology can be preserved the activity of effective medicinal components to greatest extent, keeps preferably exterior quality, color, the smell of medicinal material, makes fresh and alive plant or animal drug keep the effect of fresh medicine.But freeze-drying medicinal material quality loose gently crisp, product is frangible, is difficult for keeping medicine materical crude slice shape.

The freeze-drying of prior art is vacuum freeze drying by name entirely, claims again freeze drying, refers to medicinal material is freezed at low temperatures, then under vacuum condition, distils, and removes ice crystal, after distillation finishes, carries out adsorption stripping and dry again, and remove portion is in conjunction with the drying means of water.The steps such as freezing dry process mainly can be divided into primary drying (distillation), redrying (desorb).The difference of the present invention and existing freeze drying technology is no longer to carry out redrying after distillation finishes.The effect that this difference produces is: energy consumption is low, and product antivibration wear resistant ability is strong, and extract content is high.

Further illustrate beneficial effect of the present invention below by test example, test example is intended to further illustrate effect of the present invention, but not restriction of the present invention.

One, processed sample

Native fresh salvia miltiorrhiza root is played in same plot simultaneously, processes respectively by the following method:

1) the fresh red sage root: fresh salvia miltiorrhiza root soil buries, plastic bag sealing moisturizing;

2) red sage root that dries in the shade: get the fresh red sage root, thinly slice, put shady and cool ventilation place and dry;

3) dry the red sage root: get the fresh red sage root, thinly slice, dry;

4) dry the red sage root: get the fresh red sage root, thinly slice, lower than drying at 60 DEG C of temperature;

5) the freeze-drying red sage root: get the fresh red sage root, thinly slice, in value freeze dryer, solidification point is controlled at-30 DEG C, reaches and controls after temperature, is evacuated to below drying chamber pressure 50Pa, and then heating promotes distillation; The temperature of distillation is controlled at below 40 DEG C; Resolution temperature is controlled at below 45 DEG C;

6) freeze-drying to distillation finishes the red sage root: get the fresh red sage root, thinly slice, in value freeze dryer, solidification point is controlled at-30 DEG C, reaches and controls after temperature, is evacuated to below drying chamber pressure 50Pa, and then heating promotes distillation; The temperature of distillation should be controlled at below 40 DEG C; To distillation end.

Two, the dry red sage root water content comparison of distinct methods

According to Chinese pharmacopoeia 2010 editions (one 's) moisture analysis content.Specific as follows: testing sample is placed in the culture dish that is dried to constant weight and precise weighing, after precision weighing initial weight, be placed in drier, 105 DEG C are dried to constant weight, the moisture of calculation sample.The results are shown in Table 1.

Table 1 distinct methods is dried red sage root water content (%)

Medicinal material	Fresh	Dry in the shade	Dry	Dry	Freeze-drying	Freeze-drying to distillation finishes
							Water content	75.21	11.42	8.75	6.62	7.82	9.52

As shown in Table 1, the red sage root that distinct methods is dry, its moisture can reach below 13.0% of " Chinese pharmacopoeia " regulation.

Three, the dry red sage root extract content comparison of distinct methods

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

Adopt one of " Chinese pharmacopoeia " version in 2010, under red sage root item, Extract mensuration is measured, and the results are shown in Table 2.

Table 2 distinct methods drying leaching thing assay result.

Sample	Dry in the shade	Dry	Dry	Freeze-drying	Freeze-drying to distillation finishes
						Water extraction content (%)	38.4	37.5	37.2	42.9	50.6
Ethanol soluble extractives (%)	16.3	16.3	15.4	17.2	20.7

Table 2 finds out, red sage root freeze-drying to distillation finishes and freeze-drying, and the content of water-soluble and ethanol soluble extractives is all higher than drying in the shade, dry and drying, but red sage root energy consumption of freeze drying is high, and the process-cycle is long.

Four, the dry red sage root friability comparison of distinct methods

1, instrument friability somascope, assay 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 medicine materical crude slice are got in the each test of the amount of taking of 2.2 test samples, blow away surperficial powder, precise weighing with hair-dryer.

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.

3, result, is shown in 3.

Table 3 different dry drying method glutinous rehmannia friability

?	Shatter (%)	Less loss amount (%)
			Dry in the shade	Nothing	1.63
Dry	Nothing	1.59
			Dry	Nothing	1.72
Freeze-drying	2	5.84
			Freeze-drying to distillation finishes	Nothing	1.64

Table 3 result is known, and freeze-drying red sage root friability of the present invention, antivibration wear resistant ability are better than the freeze-drying red sage root, and product is non-friable, and storage, transport easily keep medicine materical crude slice shape, constant product quality.

Summary of the invention

The object of this invention is to provide a kind of freeze drying process of the red sage root, the effective component in red sage content of preparation is high, and product is non-friable, product quality.

The object of the present invention is achieved like this:

A freeze drying process for the red sage root, gets the fresh red sage root, and in value freeze dryer, solidification point is controlled at-30 DEG C, reaches and controls after temperature, is evacuated to below drying chamber pressure 50Pa, and then heating promotes distillation; The temperature of distillation is controlled at below 40 DEG C; After distillation finishes, finish.

The freeze drying process of a kind of red sage root of the present invention, is characterized in that: distillation finish a kind of judgement in 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 freezer unit.

So far completed the present invention.

Detailed description of the invention

embodiment 1

Get the fresh red sage root and clean impurity elimination, be cut into the segment of length 5cm; By segment sabot, loading amount is 4Kg/ ㎡ left and right; Solidification point is controlled at-28 DEG C; Reach and control after temperature, be evacuated to below drying chamber pressure 50Pa, then heating promotes distillation; The temperature of distillation is controlled at below 40 DEG C; , in the time that all distilling, finishes in the ice in material with temperature sensor monitors temperature of charge.

embodiment 2

Get the fresh red sage root, clean impurity elimination, be cut into the red sage root section of length 3cm; By the sabot of red sage root section, loading amount is 8Kg/ ㎡; Solidification point is controlled between-32 DEG C; Reach and control after temperature, be evacuated to below drying chamber pressure 50Pa, then heating promotes distillation; The temperature of distillation is controlled at below 40 DEG C; When state before condenser temperature drops to distillation, finish.

embodiment 3

Get the fresh red sage root and clean impurity elimination, be cut into the red sage root section of length 2cm, sabot, sabot weight is 7kg/ ㎡ left and right, puts in ZG-100 ㎡ type vacuum freeze drier, after lowering the temperature gradually 2 hours, freezes to-28 DEG C; Be evacuated to system absolute pressure 40Pa, be heated to 35 DEG C of distillations, when the pressure drop of freeze drying box is when approaching the pressure of freezer unit, finish.

embodiment 4

Get the fresh pellet newly digging out, clean impurity elimination, sabot, thickness is 15～20 mm, in freezing process, with 0.3 DEG C/min cooling, solidification point is controlled at-30 DEG C; The vacuum degree control of distillation is at 60pa, and temperature is controlled at below 40 DEG C; Distillation finishes rear end.

Claims

1. a freeze drying process for the red sage root, gets the fresh red sage root, and in value freeze dryer, solidification point is controlled at-30 DEG C, reaches and controls after temperature, is evacuated to below drying chamber pressure 50Pa, and then heating promotes distillation; The temperature of distillation is controlled at below 40 DEG C; After distillation finishes, finish.

2. according to the freeze drying process of a kind of red sage root of claim 1, it is characterized in that: distillation finish a kind of judgement in 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 freezer unit.