CN104479566A - After-extraction method of medicinal pigskin gelatin - Google Patents

After-extraction method of medicinal pigskin gelatin Download PDF

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Publication number
CN104479566A
CN104479566A CN201410580760.4A CN201410580760A CN104479566A CN 104479566 A CN104479566 A CN 104479566A CN 201410580760 A CN201410580760 A CN 201410580760A CN 104479566 A CN104479566 A CN 104479566A
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pigskin gelatin
medicinal
concentration
nanofiltration
gelatin
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CN201410580760.4A
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CN104479566B (en
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吴家麟
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Suzhou yifanghua Intellectual Property Operation Co., Ltd
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ZHEJIANG JEDDAH BIOLOGICAL TECHNOLOGY Co Ltd
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Abstract

The invention relates to a gelatin production method and especially relates to an after-extraction method of medicinal pigskin gelatin. The after-extraction method comprises the following steps of 1, diluting pigskin gelatin liquid boiled by an alkali method to obtain a pigskin gelatin diluent with a concentration of 1-3wt% and carrying out filtration, 2, treating the filtrate by an ion exchange device with an anion exchange resin column and a cation exchange resin column connected to the anion exchange resin column in series to obtain a permeate liquid, 3, carrying out concentration on the permeate liquid by a ultrafiltration membrane to obtain a ultrafiltration concentrate with a concentration of 20-25wt%, and concentrating the ultrafiltration concentrate by a nanofiltration membrane to obtain a nanofiltration concentrate with a concentration of 30-50wt%, 4, carrying out disinfection on the nanofiltration concentrate obtained by the step 3, carrying out quick-freezing to obtain ice, and shaving the ice to obtain roll films with thickness of 0.2-1.5mm, 5, drying the roll films obtained by the step 4 at a temperature of 40-55 DEG C for 15-20min, and 6, carrying out crushing and mixing. The after-extraction method saves energy. The product obtained by the method has the advantages of uniform particles, high gel strength and high viscosity.

Description

A kind of method for post extraction of medicinal pigskin gelatin
Technical field
The present invention relates to the production method of gelatin, particularly a kind of method for post extraction of medicinal pigskin gelatin.
Background technology
The application of gelatin is very extensive, and can be divided into the large kind of edible Gelatinum oxhide, pharmagel, photosensitive gelatin and technical gelatine four by purposes, the main purposes of pharmagel is for being used in hard capsule, soft capsule, plasma substitute and dressing etc.
The preparation method of traditional gelatin, be gelatin thin liquid first filtered, concentrate, freezing, section final drying, as: " friend got rich " the 3rd phase 22-22 page in 1997, the document describe first congeal, dry after flaking, due to the drying of sheet gelatin, contact area is limited, and easily will separate up and down due to sheet, also easily stick together in drying process, block the relative flowing of upper and lower hot gas, and each position of loft drier has certain relative temperature difference, causes uneven drying, cause the granularity of gelatin after pulverizing also uneven.
CN201110167217.8, publication date is: on December 21st, 2011, this invention relates to the rear extraction step of producing gelatin by using acid method technique, and the gelatin solution obtained by acid system filtration, ion-exchange, membrane ultrafiltration are concentrated, triple effect evaporation.Not only need to consume a large amount of energy in triple effect evaporation process, and the long-time higher meeting of temperature make gelatin freeze power and viscosity can decline to some extent, and freeze the most important index that power and viscosity are pharmagels.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of epigranular, height freezes power and the method for post extraction of full-bodied and energy-conservation medicinal pigskin gelatin.
The present invention is by the following technical solutions:
1) be the pigskin gelatin thin liquid of 1 ~ 3 wt % by the pigskin gelatin liquid boiled by alkaline process dilution, then filter;
2) filtrate is passed through with the ion-exchange unit of series connection anion-exchange resin column, cation exchange resin column, obtain permeate;
3) by step 2) gained permeate ultra-filtration membrane is concentrated into the ultrafiltration and concentration liquid of 20 ~ 25wt%, then is concentrated into the nanofiltration concentrated solution of 30 ~ 50 wt % by nanofiltration membrane;
4) by after the sterilizing of step 3) gained nanofiltration concentrated solution, quick-frozen becomes ice-like, digs into the roll film that thickness is 0.2 ~ 1.5mm;
5) under 40 ~ 55 DEG C of conditions, drying 15 ~ 20min is carried out to step 5) gained roll film;
6) pulverize, mix.
Preferably, adopt diatomite, cottonseed cake or gac as filtration medium in described filtration.
Preferably, described sterilising temp is 136 ~ 145 DEG C.
Preferably, the pressure of described ultrafiltration and concentration is 0.5 ~ 0.8MPa.
Preferably, the temperature of described ultrafiltration and concentration is 35 ~ 45 DEG C.
Preferably, the pressure that described nanofiltration is concentrated is 0.5 ~ 0.8MPa.
Preferably, the temperature that described nanofiltration is concentrated is 40 ~ 50 DEG C.
Preferably, described drying is vacuum-drying.
Advantageous Effects of the present invention:
Pigskin gelatin thin liquid is first through filtering, filtering macromolecular particle, medium grain impurity such as filtering salinity, metal ion, acid ion, chromogen is crossed again through ion exchange resin, concentrate through secondary membrane again, ultrafiltration and concentration mainly removes organism and the part salt of part intermediate molecular weight, and cycles of concentration is lower; Nanofiltration is concentrated removes small-molecular-weight organism and low price salt, ratio of desalinization is high, cycles of concentration is high, through secondary concentration, eliminate all kinds of organic impurities and various salt, the pigskin gelatin thin liquid of 1 ~ 3 wt % can be concentrated into 30 ~ 50wt% pigskin gelatin concentrated solution, due to membrane concentration without evaporation concentration, save the energy greatly.
Concentrated solution sterilizing after nanofiltration concentrates, quick freezing, ice-like gelatin after freezing is dug into thin roll film, then vacuum-drying is carried out, in drying process, because thin roll film is large with the surface-area of hot air impingement, and the inside and outside of thin roll film all contacts hot gas, each position of thin roll film is all in hot gas environments, and, in the indoor arbitrarily stacking of vacuum-drying, have space between roll film, make hot gas follow roll film fully to contact, thus make the evaporation of the moisture on roll film surface fast, rate of drying uniform particles soon and after crushed.On the other hand, due to gelatin viscosity and freeze power and all can decline to some extent, the method that the application of the invention adopts in high temperature environments, time of drying is short, and temperature is no more than 55 DEG C, thus products obtained therefrom viscosity of the present invention and power of freezing all higher.
Applicant is found by a large amount of experiments, ultrafiltration membrane pressure be 0.5 ~ 0.8MPa, under temperature be 35 ~ 45 DEG C and nanofiltration membrane pressure is 0.5 ~ 0.8MPa, temperature is 40 ~ 45 DEG C of conditions, cycles of concentration improves further, the gelatin washing lotion of 1 ~ 3wt% can be concentrated into 40 ~ 50wt%, so can greatly save time in follow-up drying process, can also ensure that high viscosity and the height of gelatin freeze power, thus meet the requirement of pharmagel.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, therefore do not limit the present invention among described scope of embodiments.
001 × 7 (732) the type vinylbenzene storng-acid cation exchange resin that following examples institute spent ion exchange resin provides for Lai Te Rider Genie et Environnement and (201*7) 717 columns in series of type styrene type strong anion-exchange resin; Ultra-filtration membrane thickening equipment model: HC-D-73, is provided by Chengdu and sincere Filter Co., Ltd; Nanofiltration membrane thickening equipment model: RNF-0460, by Xiamen, Shi Damo company limited provides.Vacuumdrier model: YZG, the rich vertical drying and granulating equipment company limited of Changzhou provides.
Embodiment 1
1) the pigskin gelatin liquid boiled by alkaline process is diluted the pigskin gelatin thin liquid for 1wt%, filter;
2) filtrate is passed through with the ion-exchange unit of series connection anion-exchange resin column, cation exchange resin column, obtain permeate;
3) by step 2) gained permeate ultra-filtration membrane concentrates, pressure be 0.5MPa, temperature is concentrated into the ultrafiltration and concentration liquid of 25wt% under being 45 DEG C of conditions; Again ultrafiltration and concentration liquid nanofiltration membrane is concentrated, pressure be 0.8MPa, temperature is concentrated into the nanofiltration concentrated solution of 30 wt % under being 50 DEG C of conditions;
4) by step 3) gained nanofiltration concentrated solution after 140 DEG C of sterilizings, quick-frozen becomes ice-like, digs into the roll film that thickness is 0.2mm;
5) under 40 DEG C of conditions, vacuum-drying 15min is carried out to step 5) gained roll film;
6) pulverize, mix.
Embodiment 2
1) the pigskin gelatin liquid boiled by alkaline process is diluted the pigskin gelatin thin liquid for 3wt%, filter;
2) filtrate is passed through with the ion-exchange unit of series connection anion-exchange resin column, cation exchange resin column, obtain permeate;
3) by step 2) gained permeate ultra-filtration membrane concentrates, pressure be 0.8MPa, temperature is concentrated into the ultrafiltration and concentration liquid of 20 wt % under being 35 DEG C of conditions; Again ultrafiltration and concentration liquid nanofiltration membrane is concentrated, pressure be 0.6MPa, temperature is concentrated into the nanofiltration concentrated solution of 50 wt % under being 45 DEG C of conditions;
4) by step 3) gained nanofiltration concentrated solution after 136 DEG C of sterilizings, quick-frozen becomes ice-like, digs into the roll film that thickness is 1.5mm;
5) under 55 DEG C of conditions, vacuum-drying 20min is carried out to step 5) gained roll film;
6) pulverize, mix.
Embodiment 3
1) be the pigskin gelatin thin liquid of 2 wt % by the pigskin gelatin liquid boiled by alkaline process dilution, filter;
2) filtrate is passed through with the ion-exchange unit of series connection anion-exchange resin column, cation exchange resin column, obtain permeate;
3) by step 2) gained permeate with ultra-filtration membrane concentrate, pressure be 0.6MPa, temperature is concentrated into the ultrafiltration and concentration liquid of 25 wt % under being 40 DEG C of conditions, again ultrafiltration and concentration liquid nanofiltration membrane is concentrated, pressure be 0.5MPa, temperature is concentrated into the nanofiltration concentrated solution of 40 wt % under being 40 DEG C of conditions;
4) by step 3) gained nanofiltration concentrated solution after 145 DEG C of sterilizings, quick-frozen ice-like, digs into the roll film that thickness is 1mm;
5) under 50 DEG C of conditions, vacuum-drying 20min is carried out to step 5) gained roll film;
6) pulverize, mix.
Comparative examples 1-3
All be with the difference of embodiment 1-3, freezing rear gelatin is cut into plane lamina.
The detection of gelatin
One, size-grade distribution situation is surveyed with dry sieve method:
1, equipment and instrument prepares
Need during test to prepare: standard sieve a set of (6,8,10,12 order), vibrating scalper one, table balance one frame, enamel tray two, baking oven.
2, concrete operation step
1) sample preparation: use conical quartering curtailed sampling, accurately take 100 grams.
2) bushing screen is sequentially folded from large to small by aperture, and loads onto the sieve end, is arranged on vibrating scalper, the sample weighed up is poured into the superiors' sieve 6 order, add screen cover.
3) start vibratory screening apparatus, vibrate 20 minutes, then every layer of sieve is taken off, with hand screening, if 1 minute gained undersize material is less than 1% of on-the-sieve material, then thinks and reach screening terminal, otherwise hand will be continued be sieved to terminal.
4) carefully take out sample, to weigh respectively on each sieve and sample mass in chassis.
Two, the detection method of gelatin viscosity
Get 60g gelatin, add 230ml water, after dissolving, be warmed to 40 DEG C, be placed in Xuan Shi viscometer, maintenance 40 DEG C of heating.Pull out bottom outlet stopper, glue slag is naturally dirty, flows to and bears in bottle, with manual time-keeping, when bear in bottle flow into glue 200ml time, block stopwatch, record the time, by the time used divided by 51 seconds, gained quotient is exactly viscosity number.
Three, the detection method of Gel Strength of Gelatin
Get gelatin 7.5g+105ml water and be made into 6.67% concentration with freezing power instrument mensuration.
Table 1: the granularity Detection result of embodiment and comparative examples products obtained therefrom:
Table 2: viscosity and the detected result of freezing power of embodiment and comparative examples products obtained therefrom
As can be known from Table 1, embodiment 1 ~ 3 products obtained therefrom mainly concentrates on 10 mesh sieves, and that is the granularity of product is 8 ~ 10 orders, accounts for more than 98%, even particle size distribution.
As can be known from Table 2, the viscosity of embodiment 1 ~ 3 products obtained therefrom freezes the related request that power meets medicinal skin gelatin completely, all exceeds much than comparative examples in power and viscosity.

Claims (8)

1. a method for post extraction for medicinal pigskin gelatin, is characterized in that comprising the following steps:
1) be the pigskin gelatin thin liquid of 1 ~ 3 wt % by the pigskin gelatin liquid boiled by alkaline process dilution, then filter;
2) filtrate is passed through with the ion-exchange unit of series connection anion-exchange resin column, cation exchange resin column, obtain permeate;
3) by step 2) gained permeate ultra-filtration membrane is concentrated into the ultrafiltration and concentration liquid of 20 ~ 25wt%, then is concentrated into the nanofiltration concentrated solution of 30 ~ 50 wt % by nanofiltration membrane;
4) by after the sterilizing of step 3) gained nanofiltration concentrated solution, quick-frozen becomes ice-like, digs into the roll film that thickness is 0.2 ~ 1.5mm;
5) under 40 ~ 55 DEG C of conditions, drying 15 ~ 20min is carried out to step 5) gained roll film;
6) pulverize, mix.
2. the method for post extraction of medicinal pigskin gelatin according to claim 1, is characterized in that: adopt diatomite, cottonseed cake or gac as filtration medium in described filtration.
3. the method for post extraction of medicinal pigskin gelatin according to claim 1, is characterized in that: described sterilising temp is 136 ~ 145 DEG C.
4. the method for post extraction of medicinal pigskin gelatin according to claim 1, is characterized in that: the pressure of described ultrafiltration and concentration is 0.5 ~ 0.8MPa.
5. the method for post extraction of medicinal pigskin gelatin according to claim 1, is characterized in that: the temperature of described ultrafiltration and concentration is 35 ~ 45 DEG C.
6. the method for post extraction of medicinal pigskin gelatin according to claim 1, is characterized in that: the pressure that described nanofiltration concentrates is 0.5 ~ 0.8MPa.
7. the method for post extraction of medicinal pigskin gelatin according to claim 1, is characterized in that: the temperature that described nanofiltration concentrates is 40 ~ 50 DEG C.
8. the method for post extraction of medicinal pigskin gelatin according to claim 1, is characterized in that: described drying is vacuum-drying.
CN201410580760.4A 2014-10-27 2014-10-27 A kind of method for post extraction of medicinal pigskin gelatin Active CN104479566B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108187497A (en) * 2017-12-27 2018-06-22 成都经典明胶有限公司 A kind of film method for concentration of edible gelatin
CN108203566A (en) * 2016-12-20 2018-06-26 湖南尔康明胶有限公司 The technique that a kind of alkaline process prepares pharmagel

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JP2004043580A (en) * 2002-07-10 2004-02-12 Hiroshige Itakura Method for producing collagen
WO2009064437A1 (en) * 2007-11-13 2009-05-22 The Board Of Trustees Of The Leland Stanford Junior University Oriented protein films as a substrate for cell growth
CN102181234A (en) * 2011-03-16 2011-09-14 罗赛洛(温州)明胶有限公司 Process for producing high-viscosity cowhide alkaline gelatin by batch and alkaline (BATALK) method
CN102286252A (en) * 2011-06-21 2011-12-21 郭小棋 Process for producing gelatin by using acid method
CN103084066A (en) * 2013-01-23 2013-05-08 余苟 Membrane filtration gelatin dehydration preconcentration system

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JP2004043580A (en) * 2002-07-10 2004-02-12 Hiroshige Itakura Method for producing collagen
WO2009064437A1 (en) * 2007-11-13 2009-05-22 The Board Of Trustees Of The Leland Stanford Junior University Oriented protein films as a substrate for cell growth
CN102181234A (en) * 2011-03-16 2011-09-14 罗赛洛(温州)明胶有限公司 Process for producing high-viscosity cowhide alkaline gelatin by batch and alkaline (BATALK) method
CN102286252A (en) * 2011-06-21 2011-12-21 郭小棋 Process for producing gelatin by using acid method
CN103084066A (en) * 2013-01-23 2013-05-08 余苟 Membrane filtration gelatin dehydration preconcentration system

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108203566A (en) * 2016-12-20 2018-06-26 湖南尔康明胶有限公司 The technique that a kind of alkaline process prepares pharmagel
CN108187497A (en) * 2017-12-27 2018-06-22 成都经典明胶有限公司 A kind of film method for concentration of edible gelatin

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Address before: 313000 Zhejiang Jida Biotechnology Co., Ltd., Lingang Industrial Zone, Meixi Town, Anji County, Huzhou City, Zhejiang Province

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