CN1068121A

CN1068121A - Extraction process of sapogenin

Info

Publication number: CN1068121A
Application number: CN 92100484
Authority: CN
Inventors: 陈延镛; 马资华; 颜邦宁; 胡兴隆; 曾丽修; 黄翠莲; 承葆生; 徐礼燊; 刘爱茹
Original assignee: NANNING PHARMACEUTIC ENTERPRIS; Institute of Materia Medica of CAMS and PUMC
Current assignee: NANNING PHARMACEUTIC ENTERPRIS; Institute of Materia Medica of CAMS and PUMC
Priority date: 1992-01-20
Filing date: 1992-01-20
Publication date: 1993-01-20

Abstract

本发明提出了一种替告皂甙元即剑麻皂素的提取工艺方法。该工艺的特点是从去纤维的东一号剑麻废渣中取汁，经发酵、水解、皂化、提取、去蜡脱色、浓缩、结晶、烘干而得。该工艺方法成本低，收率高，质量好，且原料来源广，变废为宝，综合利用，为开发利用甾体激素药物提供了一种新的原料资源。The present invention proposes a method for extracting sisal saponin from sapogenin Take the process method. The craft features a sword from the de-fibered East One Extract juice from hemp waste residue, undergo fermentation, hydrolysis, saponification, extraction, dewaxing and decolorization, Concentration, crystallization, drying derived. The process method is low in cost and high in yield, Good quality, and wide source of raw materials, turning waste into treasure, comprehensive utilization, for development The use of steroid hormone drugs provides a new source of raw materials.

Description

The process for extracting of Tigogenin

The present invention relates to a kind of process for extracting of process for extracting, especially Tigogenin of natural resource of steroid hormone class medicine.

Tigogenin (Tigogenin, trade(brand)name tigogenin) formal name used at school: 5a, 25D-spirostane-3 β hydroxyl, it and diosgenin (Diosgenin), hecogenin (Hecogenin) are all important steroid hormone raw material.The raw material potato of diosgenin is a wild plant, resource-constrained; The american aloe of hecogenin is the kind that eliminate gradually on the farm because of producing the fiber rate low also; And the sisal hemp in east produces fiber rate height, and fiber is long, is the cash crop of a large amount of plantations of China's southern farm, the resource abundance.Tigogenin extracts from the dried slag of sisal hemp in east that removes fiber, replace other saponin that resource peters out and become trend, and higher with tigogenin synthesizing efficient cortin yield, cost is lower, demonstrates bigger superiority.

The objective of the invention is for development and use steroid hormone medicine provides a kind of new raw material resources, and be that a kind of cost is low, yield is high, the measured process for extracting that is suitable for the Tigogenin of industrialness production of matter.

Operational path of the present invention is seen accompanying drawing.

Production process of the present invention is:

1, the preparation of the dried slag of sisal hemp in east:

The dried slag of sisal hemp is the starting raw material that enters the factory-prepared tigogenin, and the preparation of the dried slag of sisal hemp is to finish in the raw material site on farm.Get the bright numb meat waste residue that the raw material site has been removed fiber, get numb juice through squeezing, put in the pond open-air spontaneous fermentation sedimentation after 10～15 days, supernatant liquid bleeds off, sediment put the sunning ground after drying the dried slag of sisal hemp.

4 tons of the sisal hemp leaf average yield per mus in east of the annual harvesting in farm, sisal hemp leaf per ton goes the bright numb meat waste residue compressible behind the fiber to get numb water 0.5M ³, every 1M ³Fiber crops water sediment after fermenting dries and can get 10～15 kilograms of the dried slags of sisal hemp.

2, the preparation of tigogenin:

A, hydrolysis

Material ratio: the dried slag of sisal hemp: water: the vitriol oil: lime=1: 45: 0.5: 0.1

Water is dropped into hydrolytic decomposition pot according to quantity, add sulfuric acid then lentamente and make and become 2 equivalents, drop into sealed cans mouth behind the dried slag of sisal hemp again.Stir and steam heating, temperature is 130 ℃～142 ℃ in the control, interior pressure 2.5～3kg/cm ²Discharging is finished in reaction, puts whizzer and gets rid of and wash hydrolyzate to neutral.Add lime mixing furnishing pasty state in the hydrolyzate, tray send dry back to be the saponification hydrolyzate.The hydrolyzate yield is that 60～70%(connects lime heavily).

B, extraction

Material ratio: hydrolyzate: alcohol: concentrated hydrochloric acid: gac=1: 15: an amount of: 0.2

Saponification posthydrolysis thing alcoholic extraction secondary.Make with the heating of 10 times of amount 95% alcohol for the first time and refluxed 1 hour; Reflux filtered while hot half an hour with 5 times of amounts for the second time.Twice extract merges, and transferring PH with concentrated hydrochloric acid is 5, adds gac, reflux 1 hour, heat filter.Filtrate send concentration tank dense surplus 1: 4 volume.Concentrated solution is cooled to about 25 ℃ to be placed crystallization and spends the night.Leach crystal, it is neutral colourless only to be washed till washing lotion with alcohol.Promptly get tigogenin after the crystal drying, be Tigogenin.Yield is that 3～6.6%(is to the dried slag meter of sisal hemp), content is more than 85%, fusing point: 196～206 ℃.

Extraction process cost of the present invention is low, yield is high, and quality is good, and raw material sources are wide, turn waste into wealth, and comprehensive utilization is for development and use steroid hormone medicine provides a kind of new raw material resources.

Embodiment:

Get the bright dregs of linseeds or sesame seeds that the raw material site has been removed fiber, get its juice through squeezing machine squeezing, it is surplus to put in the pond open-air spontaneous fermentation sedimentation first quarter moon, and supernatant liquid discards, and sediment is put the sunning ground and dried and get final product.

In hydrolytic decomposition pot, add 900L water and 200 kilograms of sulfuric acid.Stir evenly (measure the sulfuric acid equivalent and should be 2N, should drink when not enough add to foot) slightly, seal after dropping into 200 kilograms of dried slags of sisal hemp, start and stir and jacket steam, heating makes 135 ℃, interior pressure 2.5kg/cm ²The time hydrolysis 2 hours, hydrolyzate is pressed in the container for storing liquid, change the whizzer inner filtration in batches, be washed to neutrality, take out hydrolyzate, in mixing machine, add calcium hydroxide and be mixed into pasty state for 20 kilograms, go into the drying room drying and dehydrating in the immigration dish.Weigh after doing 120～140 kilograms of hydrolyzates (comprising calcium hydroxide).

Hydrolyzate is dropped into extractor add alcohol 1000L, being heated to and boiling backflow after 1 hour, blowing makes extracting solution change in the bleacher by the insulation pressure-filtering tank.Add for the second time 500L alcohol reflux equally the back by pressure-filtering tank make filtered till.Twice extract adds 25 kilograms of hydrochloric acid 4L and gacs in bleacher, reflux 1 hour takes advantage of hot discharging to enter concentration tank by the insulation pressure-filtering tank, steams alcohol 600L, makes and extracts till the dense extremely about 800L of destainer.Take advantage of heat that concentrated solution is sent into crystallizer.

Concentrated solution is put into behind the crystallizer interlayer feed the cold water cooling and be cooled to room temperature, leave standstill and move into whizzer after 24 hours and filter, it is colourless only to be washed till washing lotion with an amount of alcohol.Send the drying room drying in the finished product immigration dish.Get tigogenin more than 9 kilograms, content 85%, fusing point: 196～206 ℃.

Claims

1. A process for extracting sapogenin, characterized in that: taking the waste residue of No. 1 sisal hemp as raw material, extracting juice through pressing, fermentation and sedimentation, drying, acid hydrolysis, saponification, extraction, dewaxing and decolorization, Concentration, crystallization, drying and other processes in the system.

2. The method according to claim 1, characterized in that the raw material is hemp meat residue after defibrosis, which is squeezed to extract juice and naturally fermented to produce sediment, which is obtained by drying.

3. The method according to claim 1, characterized in that the hydrolysis of sisal dry residue uses 5 times the volume of 2 equivalents of sulfuric acid for 2 hours at an internal temperature of 130-142°C and an internal pressure of 2.5-3kg/cm ² .

4. The method as claimed in claim 1, characterized in that 20% of lime is added to the hydrolyzate for saponification, and then dried after being adjusted into a paste.

5. The method according to claim 1, characterized in that the hydrolyzate after saponification is extracted twice with alcohol heating under reflux, filtered, combined extracts, adjusted to pH 5 with hydrochloric acid, added activated carbon to reflux for 1 hour, and hot filtered. The filtrate was concentrated, cooled and crystallized. Wash with alcohol until neutral and dry to obtain the product.