CN103948649A

CN103948649A - Method for drying lonicera japonica thumb

Info

Publication number: CN103948649A
Application number: CN201410204821.7A
Authority: CN
Inventors: 卢宁; 赵颖; 张为胜; 丁桂丽; 孙志芳
Original assignee: Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
Current assignee: Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
Priority date: 2014-05-15
Filing date: 2014-05-15
Publication date: 2014-07-30

Abstract

The invention relates to a method for drying lonicera japonica thunb. The method is characterized by comprising the following steps: selecting fresh lonicera japonica thunb; removing impurities; thoroughly steaming; lyophilizing and drying. According to the lonicera japonica thunb dried by the method, the main effective components are high in content of sterols and polysaccharides.

Description

The drying means of a kind of golden sesame

Invention field

The present invention relates to medicine method for making, particularly the drying means of a kind of golden sesame, 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 quality will directly affect the quality of product.

Jin Zhi is the dry sporophore of the Hymenochaetaceae of caprifoliaceae plant Radix Ophiopogonis Lonicera japonica Thunb basal part of stem parasitism lobate layer Pseudomonas fungus currant leaf pore fungi [Phylloporia ribis (Schumach.:Fr.) Ryvarden].There is heat-clearing and toxic substances removing, detumescence sore-throat relieving, antiinflammatory, antiviral, suppresses the effect of tumor.Jin Zhi is with a long history Medicinal, is usually used in treating pharyngitis, laryngitis, and tonsillitis, oral inflammation, cancer, diabetes, antibacterial and viral infection and ulcer etc., clinical efficacy is definite.According to the effective ingredient of bibliographical information gold sesame, be sterols and polysaccharide etc.

Jin Zhi records the Chinese crude drug standard > > in < < Shandong Province, and the drying means of gathering is that summer, Qiu Erji gather, and removes impurity, dries in the shade or 60-70 ℃ of oven dry.We study and find to dry in the shade or 60-70 ℃ of oven dry after golden sesame is gathered, and effective ingredient sterols and polysaccharide content are low.

Summary of the invention

The object of this invention is to provide the dry new method of a kind of golden sesame, the golden sesame that the method is dry, main effective ingredient sterols and polysaccharide content are high.

The present invention is achieved in that

A drying means for golden sesame, is characterized in that: get the golden sesame of newly gathering, remove impurity, steam thoroughly lyophilizing.

The drying means of a kind of golden sesame of the present invention, is characterized in that: steaming is to steam more than 10 minutes thoroughly.

The drying means of a kind of golden sesame of the present invention, is characterized in that: 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 the temperature of resolution phase should be controlled at below 45 ℃, to dry.

So far completed the present invention, the golden sesame of preparing by drying means of the present invention, main effective ingredient sterols and polysaccharide content are high.

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.

By with a collection of golden sesame of newly gathering, remove impurity, process by the following method.

1) dry: shady and cool ventilation place, spread out and dry;

2) dry: 60 ℃ of following oven dry;

3) steam rear lyophilizing: steam 10 minutes, through watching, steam the heart, be refrigerated to-20 ℃, be evacuated to drying chamber pressure 30Pa, subliming by heating, the temperature of distillation is controlled at 40 ℃, and the temperature of resolution phase should be controlled at 45 ℃, to dry.

One, the dry golden sesame sterols content comparison of distinct methods

1, instrument and material

Instrument: Agilentl 100 high performance liquid chromatographs, G1315A/B (DAD UV-detector); Medicine: ergosterol reference substance, methanol, ultra-pure water, other reagent are analytical pure.

2, method

Chromatographic condition chromatographic column: Zorbax eclips XDB C8 (150mm * 4.6mm); Mobile phase: methanol; Flow velocity: 1.0 mL/ min; Detect wavelength: 282nm; Column temperature: 30 ℃; Sample size: 20 μ L.Under these conditions, inject sample solution, theoretical cam curve is greater than 10000 in ergosterol.

The preparation of reference substance solution: it is appropriate that precision takes ergosterol reference substance, is mixed with the solution of 0.3mg/mL with methanol, 4 ℃ of cold preservations are standby.

The preparation of need testing solution: get the about 0.5g of each sample powder (crossing sieve No. three), accurately weighed, be placed in tool plug triangular flask, add methanol 40mL, weighed weight, ultrasonic (400W, 40kHz) 1h, place room temperature, weigh, add methanol to former weight, get supernatant and cross 0.45 μ m filter membrane, obtain need testing solution, 4 ℃ of cold preservations are standby.

Sample determination: the accurate need testing solution 20 μ m that draw, injection liquid chromatography, records peak area value, calculates content by dry product.

3, result

The results are shown in Table 1.

Table 1 distinct methods is dried golden sesame sterols content (%)

Drying means	Dry	Dry	Lyophilizing after steaming
				Content (%)	0.11	0.12	0.41

By table 1, found out, Jin Zhi " heap postpone is dry ", sterols content is apparently higher than " drying " and " oven dry ", and known the inventive method has advance.

Two, the dry golden sesame polyoses content comparison of distinct methods

1, instrument and material

Instrument: ultraviolet-uisible spectrophotometer, electronics typing balance, electric-heated thermostatic water bath.

Material: phenol, sulphuric acid, glucose, ethanol.

2. method and result

The preparation of glucose standard solution: precision takes anhydrous glucose 100 mg that are dried to constant weight, puts in 100mL volumetric flask, is diluted with water to scale, shakes up, and obtains.

The preparation of need testing solution: each sample powder (crossing sieve No. three) approximately 0.2 g, accurately weighed, 80% ethanol 100mL refluxes and carries 1h respectively, filters, 80% washing with alcohol for powder (10mL * 3), to remove the interference compositions such as monosaccharide disaccharidase, oligosaccharide.Powder is placed in flask together with filter paper, with 100mL water heating extraction 1 h, filters, and hot wash for mycopowder (10 ml * 3), washing liquid is incorporated to filtrate, and filtrate is moved in 250 volumetric flasks, is diluted to scale, standby.

The selection of maximum absorption wavelength: first use blank solution baseline balance, the accurate 0.6mL glucose standard solution of drawing is placed in 10mL tool plug test tube again, add respectively water and mend to 2.0mL, then each precision adds 5% phenol solution 1mL, shake up, drip rapidly concentrated sulphuric acid 5.0mL, shake up, in 70 ℃ of water-baths, heat 25 min, adopt psychrolusia cooling, from 200-700nm wavelength, carry out full wavelength scanner, trying to achieve maximum absorption wavelength is 490nm.

The mensuration of polysaccharide: the accurate need testing solution 1mL that draws each sample is placed in l0 mL tool plug test tube, adding distil water 1mL, add 5% phenol 1mL, mix, drip rapidly concentrated sulphuric acid 5mL, at once shake up, in 70 ℃ of water-baths, heat 25min, after employing psychrolusia is cooling, in 490nm place colorimetric, survey light absorption value.Press dry product and calculate content.

3, result the results are shown in Table 2.

Table 2 distinct methods is dried golden sesame polyoses content (%)

Drying means	Dry	Dry	Lyophilizing after steaming
				Content (%)	4.35	4.34	6.82

By table 2, found out, Jin Zhi " heap postpone is dry ", polyoses content is apparently higher than " drying " and " oven dry ", and known the inventive method has advance.

The specific embodiment

The drying means of a kind of golden sesame, it is characterized in that: get the golden sesame of newly gathering, remove impurity, steam more than 10 minutes, vexed, be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 30Pa, subliming by heating, the temperature of distillation is controlled at below 40 ℃, the temperature of resolution phase should be controlled at below 45 ℃, to dry.

embodiment 1

Get the golden sesame of newly gathering, remove impurity, steam 10 minutes, vexed, be refrigerated to-25 ℃, be evacuated to drying chamber pressure 35Pa, subliming by heating, the temperature of distillation is controlled at below 35 ℃, and the temperature of resolution phase should be controlled at 40 ℃, to dry.

embodiment 2

Get the golden sesame of newly gathering, remove impurity, steam 15 minutes, through watching, steam, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 40Pa, subliming by heating, the temperature of distillation is controlled at below 30 ℃, and the temperature of resolution phase should be controlled at 40 ℃, to dry.

embodiment 3

Get the golden sesame of newly gathering, remove impurity, steam 20 minutes, through watching, steam the heart, be refrigerated to-28 ℃, be evacuated to drying chamber pressure 50Pa, subliming by heating, the temperature of distillation is controlled at below 40 ℃, and the temperature of resolution phase should be controlled at 45 ℃, to dry.

embodiment 4

Get the golden sesame of newly gathering, remove impurity, steam 20 minutes, vexed, to put in freeze dryer, solidification point is controlled at-30 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation, the temperature of distillation should be controlled at below 40 ℃; The temperature of resolution phase should be controlled at below 45 ℃, to dry.

Claims

1. a drying means for golden sesame, is characterized in that: get the golden sesame of newly gathering, remove impurity, steam thoroughly lyophilizing.

2. according to the drying means of a kind of golden sesame of claim 1, it is characterized in that: steaming is to steam more than 10 minutes thoroughly.

3. according to the drying means of a kind of golden sesame 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 the temperature of resolution phase should be controlled at below 45 ℃, to dry.