CN108753451A - In a kind of injection stage/purification process and products thereof of backbone triglycerides - Google Patents
In a kind of injection stage/purification process and products thereof of backbone triglycerides Download PDFInfo
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- CN108753451A CN108753451A CN201810516704.2A CN201810516704A CN108753451A CN 108753451 A CN108753451 A CN 108753451A CN 201810516704 A CN201810516704 A CN 201810516704A CN 108753451 A CN108753451 A CN 108753451A
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- triglycerides
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
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- Oil, Petroleum & Natural Gas (AREA)
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- Fats And Perfumes (AREA)
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Abstract
The invention discloses in a kind of injection stage/purification process and products thereof of backbone triglycerides, it is characterised in that：Including silica gel absorption purifying：In/backbone triglycerides crude product in silochrom is added, premix；Gross porosity chromatography silica gel is added again and petroleum ether is added, in absorption and purification/backbone triglycerides obtain in/backbone triglycerides purifying intermediate；Molecular distillation is refined：The purifying intermediate preheating, adjustment feed rate, temperature, knifing rotating speed carry out molecular distillation and refine, in obtaining after purification/backbone triglycerides.The present invention establishes in a kind of injection stage/purification process of long-chain STG, present invention determine that in purifying/concrete technology and parameter of long-chain STG, moderate cost of the present invention, in can be achieved/the domestic industrialized production of long-chain STG, product indices can meet State Food and Drug Administration's import drugs (structured triglyceride) registered standard.
Description
Technical field
The invention belongs to grease intensive processing, technical field of modification, and in particular in a kind of injection stage/backbone glycerine
The purification process and products thereof of three esters.
Background technology
In/backbone triglycerides (in/long-chain STG) it is a kind of novel knot synthesized by esterification or transesterification mode
Structure triglycerides, its main feature is that containing medium chain fatty acid (MCFA, the aliphatic acid of 8~12 carbon) and long-chain on glycerol backbone simultaneously
Aliphatic acid (LCFA, the aliphatic acid of 14~22 carbon).In/more traditional long-chain STG long chain triglycerides (LCT), medium chain triglyceride
In three esters (MCT) and physical mixed/long chain triglycerides (MCT/LCT) in terms of Nutrition and Metabolism have many advantages, food,
Pharmaceuticals industry application demand increasingly all increases, the application especially in fat emulsion.
In/long-chain STG compared with the LCT and MCT/LCT of physical mixed have faster oxidation, hydrolysis release and plasma clearance
Rate, better N-saving effect, while having many advantages, such as not influence body reticuloendothelial system function.In currently ,/long-chain STG types
In Fat Emulsion primary raw material/long-chain STG is from external import, market price is 3-5 times of domestic common fats breast.Cause
This, in research/synthesis of long-chain STG and purification process have great importance.
This research team in/long-chain STG synthesis in terms of done a large amount of research, and apply obtaining concerned countries invention special
Profit two (in a kind of/synthetic method of backbone triglycerides, ZL 201110052579.2 and a kind of enzyme law catalysis ester are handed over
/ the method for backbone triglycerides, ZL 201010529356.6 are changed in synthesis).But found during early-stage study,
Either enzyme process or chemical method, in obtaining/reaction of long-chain STG in, no matter which kind of method used, can all generate and not expect out
Existing side reaction product, such as free fatty, fatty acid methyl ester, monoglyceride, diglyceride, so needing to obtained by the reaction
In/long-chain STG purified, it can meet State Food and Drug Administration's import drugs (structured triglyceride) note to obtain
Volume standard (standard No.：JX20070100 in)/long-chain STG products.
As a kind of special new separation technology, the application in fields such as food, medicine, chemical industry is more and more wider for molecular distillation
It is general, the purification & isolation especially to higher boiling, heat sensitive material.Using molecular clock high-purity fat in oil prodution industry
The reports such as acid, monoglyceride, diglyceride, vitamin E are also commonplace.Molecular distillation is as a kind of distillation side under a high vacuum
Method, be using each component evaporation rate in feed liquid (with the ratio between component vapour pressure and molecular weight in relation to) difference to realize to liquid
The separation of body mixture isolates and purifies principle and determines that molecular distillation purifying does not have selectivity.Our early-stage studies are a large amount of
The experimental results showed that：Merely using in molecular distillation purifying/long-chain STG is extremely difficult to its quality criteria requirements, especially product
Requirement cannot be fully achieved in the percentage of medium chain triglyceride, combination chain (middle long-chain) triglycerides and long chain triglycerides.
The main difference of comprehensive analysis raw material and target product quality of the present invention, using free fatty, fatty acid methyl ester,
The polarity difference of the impurity such as monoglyceride, diglyceride and triglycerides, designed and developed silica gel absorption/silicagel column absorption-film/
Molecular distillation is combined the process route for isolating and purifying middle long-chain STG, obtains and meets State Food and Drug Administration's import
Drug (structured triglyceride) registered standard (standard No.：JX20070100) long-chain STG products in the high-quality of indices, can
/ the industrialized production of backbone triglycerides is realized in injection stage.
Invention content
The purpose of this part is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferably to implement
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
In view of above-mentioned technological deficiency, it is proposed that the present invention.
Therefore, as one aspect of the present invention, the present invention overcomes the deficiencies in the prior art, provides a kind of note
/ the purification process of backbone triglycerides is penetrated in grade.
In order to solve the above technical problems, the present invention provides following technical solutions：In a kind of injection stage/backbone glycerine
The purification process of three esters comprising,
Silica gel absorption purifies：In/backbone triglycerides crude product in silochrom is added, premix；It is added again thick
Hole chromatography silica gel and petroleum ether is added, in absorption and purification/backbone triglycerides obtain in/backbone triglycerides
Purify intermediate；
Molecular distillation is refined：The purifying intermediate preheating, adjustment feed rate, temperature, knifing rotating speed carry out molecule steaming
Evaporate it is refined, in obtaining after purification/backbone triglycerides.
As in injection stage of the present invention/a kind of preferred embodiment of the purification process of backbone triglycerides：Institute
State silica gel absorption purifying, wherein it is described in/backbone triglycerides crude product in be added silochrom, including in/long-chain
10%~30% silochrom, the silochrom are added in structured triglyceride crude product, water content is no more than 10%.
As in injection stage of the present invention/a kind of preferred embodiment of the purification process of backbone triglycerides：Institute
State silica gel absorption purifying, wherein the premix, vacuum premixes 40min under conditions of being included in 80 DEG C, is cooled to 60 DEG C or less and breaks
Vacuum.
As in injection stage of the present invention/a kind of preferred embodiment of the purification process of backbone triglycerides：Institute
It states and gross porosity chromatography silica gel is added again and petroleum ether is added, including press in the gross porosity Se spectrum Gui Jiao ︰/backbone glycerine three
Ester crude product quality for the ratio of 1 ︰ 1~2 than adding gross porosity chromatography silica gel, in pressing/backbone triglycerides crude product quality：Oil
The petroleum ether that boiling range is 60~90 DEG C is added in the ratio that ether volume is 1 ︰ 6~12, is adsorbed.
As in injection stage of the present invention/a kind of preferred embodiment of the purification process of backbone triglycerides：Institute
It states and gross porosity chromatography silica gel is added again and petroleum ether is added, it is described to be adsorbed, it is included under conditions of room temperature or temperature control and stirs
Absorption is mixed, time 30min stands, collects supernatant.
As in injection stage of the present invention/a kind of preferred embodiment of the purification process of backbone triglycerides：?
Petroleum ether is added in the precipitation of the silica gel after standing again, repeats stirring and adsorbing, time 10mim is stood, in collection
Clearly, and with a preceding supernatant it mixes.
As in injection stage of the present invention/a kind of preferred embodiment of the purification process of backbone triglycerides：It will
Obtained supernatant evaporation volatilizes, and the evaporation volatilizes, and is included in temperature and is 60 DEG C, rotates and steam under the conditions of rotating speed 50rpm
It plays dry.
As in injection stage of the present invention/a kind of preferred embodiment of the purification process of backbone triglycerides：Also
Including, evaporation is dried in vacuo after volatilizing, and temperature is 80 DEG C, time 40min, obtain it is described in/backbone glycerine three
Ester purifies intermediate.
As in injection stage of the present invention/a kind of preferred embodiment of the purification process of backbone triglycerides：Institute
It is refined to state molecular distillation, including, will described in/backbone triglycerides purifying intermediate after 40~60 DEG C of heat-insulation preheatings,
In 2~10mL/min of feed rate, the condition of 90-150 DEG C of evaporating surface temperature, knifing rotating speed 100-150rpm, vacuum degree < 5Pa
Lower processing, in obtaining after purification/backbone triglycerides.
As another aspect of the present invention, the present invention overcomes the deficiencies in the prior art, provides a kind of injection stage
In/the obtained injection of the purification process of backbone triglycerides in/backbone triglycerides.
In order to solve the above technical problems, the present invention provides following technical solutions：In injection stage/backbone triglycerides
The obtained injection of purification process in/backbone triglycerides, wherein：In the injection/backbone triglycerides
The rate of recovery reaches 75% or more.
Beneficial effects of the present invention：The present invention establishes in a kind of injection stage/purification process of long-chain STG, belong to and starts
Journal of Sex Research.
The present invention provides in/selection gists of long-chain STG purifying process parameters, it is determined that in purifying/tool of long-chain STG
Body technology and parameter.The present invention uses in this process purification/long-chain STG, moderate cost, it can be achieved that in/the domestic work of long-chain STG
Industry metaplasia is produced, and product indices can meet State Food and Drug Administration's import drugs (structured triglyceride) registration
Standard (standard No.：JX20070100) require, be conducive to break in the country backbone fat of triglyceride breast rely on for a long time into
The situation of mouth, overseas-funded enterprise's simple monopoly builds positive, orderly market competition structure.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without having to pay creative labor, it can also be obtained according to these attached drawings other
Attached drawing.Wherein：
Fig. 1 be before purification in/backbone triglycerides HPLC-ELSD spectrograms.
Fig. 2 be after purification in/backbone triglycerides HPLC-ELSD spectrograms.
The cities Tu3Wei mid-sales/backbone triglycerides HPLC-ELSD spectrograms.
Fig. 4 be the embodiment of the present invention 3 after purification in/backbone triglycerides HPLC-ELSD spectrograms.
Specific implementation mode
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to specific embodiment pair
The specific implementation mode of the present invention is described in detail.
Many details are elaborated in the following description to facilitate a thorough understanding of the present invention, still the present invention can be with
Implemented different from other manner described here using other, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by following public specific embodiment.
Secondly, " one embodiment " or " embodiment " referred to herein refers to that may be included at least one realization side of the present invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiment.
The present invention is with medium chain triglyceride (MCT), long chain triglycerides (LCT) molar ratio 1:In obtained by 1 ester exchange reaction
Long-chain STG products are raw material, using gross porosity chromatography silica gel (silica gel particle 70-200um, aperture), it is molten with petroleum ether
Agent, under conditions of room temperature or temperature control, by stirring or column chromatography absorption and purification/long-chain STG, solvent communicated concentration
Recycling design must purify intermediate, and long-chain STG is produced during middle long-chain STG intermediates must purify after molecular distillation is further processed
Product pass through silica gel water content, silica gel additive amount, sample concentration, mixing time using the rate of recovery for purifying final product as leading indicator
Etc. factors optimization, in determining/optimised process of long-chain STG purifying.Preparation process of the present invention is as follows：
One, in/preparation of long-chain STG raw materials：
With medium chain triglyceride (MCT), long chain triglycerides (LCT) molar ratio 1:1 feeds intake, in 40 DEG C -80 of reaction temperature
DEG C, react 10-50min under conditions of sodium methoxide additive amount 0.1%-0.4%；The termination that a certain amount of citric acid solution is added is anti-
It answers, neutral centrifugation is washed till with hot water；It is thick that long-chain STG during 20-90min postcoolings obtain is dried in vacuo under conditions of 70 DEG C -90 DEG C
Product.
Two, silica gel absorption purifies：
A certain amount of gross porosity chromatography silica gel is added into middle long-chain STG crude products, vacuum premixes in advance under conditions of 70 DEG C -90 DEG C
20-60min is cooled to 60 DEG C or less vacuum breakers；A certain amount of petroleum ether and gross porosity chromatography silica gel is added, in room temperature or temperature control
Under the conditions of, by stirring or column chromatography absorption and purification/long-chain STG, solvent communicated during concentration and recovery solvent must purify
Mesosome；
1, silica gel water content
Silica gel water content largely influences the activity of silica gel, and the polarity of water is big, it is easier to in the activity of silica gel
Hearty cord closes to reduce activity, therefore water content is higher, and Silica gel activated lower, unobvious are got in the absorption for treating separate substance.Silicon
Glue activity too it is high can centering/long-chain STG contents have an impact, and adsorbate is more difficult to be desorbed, Silica gel activated too low to influence point
From effect, it is therefore desirable to it is Silica gel activated to adjust by changing silica gel water content, and determine most suitable silica gel water content.
2, silica gel additive amount
Silica gel additive amount is bigger, contacts that more abundant purification effect is better with sample, but the silica gel underused is simultaneously
To in part/long-chain STG generates suction-operated, cause the rate of recovery of sample after purification to reduce.Therefore silica gel additive amount is certain
It should be controlled in range.
3, sample concentration
The experimental results showed that the variation of sample concentration purification effect is influenced it is little, but on sample recovery rate influence compared with
Greatly.As sample concentration increases, silica gel is not merely to free fatty, fatty-acid ethyl ester, monoglyceride, diglyceride isopolarity group
Point have a suction-operated, at the same also in sample/long-chain STG generates delay effect and made to which sample recovery rate is substantially reduced
At unnecessary loss.
4, adsorption time
Adsorption time is longer, and silica gel absorption is more abundant, but the phenomenon that exist simultaneously adsorbate desorption, influences purifying instead
Effect, therefore adsorption time is not that the longer the better.Meanwhile after first time adsorption equilibrium separation solid-liquid two-phase, solid phase silica gel
Can be remained in surface it is more in/long-chain STG, need to using it is fresh or recycling petroleum ether be solvent progress reextraction, to improve
Sample recovery rate.
Three, molecular distillation is refined：
Middle long-chain STG intermediates prepared by silica gel absorption purifying there is also certain dissolvent residual and some bad flavors,
It is necessary to be further processed, dissolvent residual and bad flavor are removed, is reached tasteless or almost tasteless.
Middle long-chain STG intermediates are after 40-60 DEG C of heat-insulation preheating, in feed rate 2-10mL/min, evaporating surface temperature 135
It is handled under conditions of DEG C (90-150 DEG C), knifing rotating speed 126 (100-150rpm), vacuum degree < 5Pa, gained heavy phase is to purify
In afterwards/long-chain STG.
Four, determination of quality index：
Overall quality index request is registered according to State Food and Drug Administration's import drugs (structured triglyceride)
Standard (standard No.：JX20070100 it) requires to carry out, wherein reference Chinese Pharmacopoeia (version in 2005) method is then corresponding using China
Pharmacopeia (version in 2010) method, table specific as follows：
Embodiment 1：
10% silochrom is added in long-chain STG crude products in 200g, and vacuum premixes cold after 40min under conditions of 80 DEG C
But to 60 DEG C or less vacuum breakers；40% silochrom and 2000mL petroleum ethers (60~90 DEG C) is added, at room temperature magnetic agitation
30min is stood, and shifts supernatant after supernatant clarification, 500ml petroleum ethers (60~90 DEG C), room are continuously added into precipitation
The lower magnetic agitation 10min of temperature, stands, and supernatant is shifted after supernatant clarification, merge twice supernatant in temperature 60 C, rotating speed
Rotary evaporation volatilizes solvent under conditions of 50rpm；Vacuum is opened, temperature is risen to 80 DEG C, continues revolving 40min and obtains middle long-chain
STG purifies intermediate；Divide under conditions of 135 DEG C of 3mL/min, evaporator temperature, scraper plate rotating speed 125rpm, vacuum degree < 5Pa
Son distillation；Heavy phase is taken to weigh, in calculating/the long-chain STG rate of recovery and measure correlated quality index.
The long-chain STG rate of recovery is 81.87% in calculating；Correlated quality index is shown in Table 1.
Embodiment 2：
20% silochrom is added in long-chain STG crude products in 10000g, cold after vacuum premix 40min under conditions of 80 DEG C
But to 60 DEG C or less vacuum breakers；80% silochrom and 100000mL petroleum ethers (60~90 DEG C) is added, is stirred under the conditions of 40 DEG C
Mix 30min, stand, filtering supernatant continuously adds 25000ml petroleum ethers (60~90 DEG C) into precipitation, under the conditions of 40 DEG C after
Continuous stirring 10min, stands, filtering supernatant, merges supernatant twice, in 60-90 DEG C of liter film temperature, vacuum degree -0.08Mpa
Concentration and recovery solvent obtains middle long-chain STG purifying intermediate under conditions of~-0.1Mpa；In 135 DEG C of 8mL/min, evaporator temperature,
Molecular distillation under conditions of scraper plate rotating speed 125rpm, vacuum degree < 5Pa；Take heavy phase to weigh, in calculating/the long-chain STG rate of recovery simultaneously
Measure correlated quality index.
The long-chain STG rate of recovery is 75.13% in calculating；Correlated quality index is shown in Table 1.
Spectrogram is shown in Fig. 1-Fig. 2 before and after middle long-chain STG purifying crudes；Structure glycerine three in city's mid-sales/long-chain STG fat emulsions
Ester spectrogram is shown in Fig. 3.
Table 1：In/backbone triglycerides quality index
Embodiment 3：
Different in moisture content silica gel purification effect compares, be respectively placed in after a certain amount of silica gel is dispensed with plate containing
NaOH, LiCl, KAc, MgCl2 saturated solution (corresponding system moisture is respectively 7%, 11%, 22.4% and 0.33%)
In drier for 24 hours in 25 DEG C of balances, remaining is the same as embodiment 1.The result shows that 22.4% and the above water content silica gel purification effect
It is decreased obviously, intuitively showing as purifying spectrogram front end has miscellaneous peak (Fig. 4) occur.Therefore, silica gel moisture is to purification effect
Have a direct impact, silica gel moisture should be controlled 22.4% hereinafter, it is preferred that 10% or less.
Embodiment 4：
Different sample concentration purification effects compare, by embodiment 1, after the silochrom for being added 40%, by quality and body
Product (m/v) ratio is separately added into 400,800,1200,1600,2000 and 2400mL petroleum ethers, remaining is the same as embodiment 1.Purified product
The rate of recovery is differed from 40.72%~82.01%, and early period increases the mass volume ratio of sample and solvent, and the rate of recovery obviously increases, when
Mass volume ratio reaches 1:After 10, the purifying rate of recovery increases slow, kept in balance, at the same consider to industrialize solvent recovery at
This, preferably sample solvent mass ratio is 1:10.
Embodiment 5：
Different adsorption time purification effects compare, by embodiment 1, it is front and back adsorb twice respectively stirring 10,20,30,40,
60min takes after standing supernatant to carry out HPLC-ELSD spectrum analysis, miscellaneous peak whether occurs as standard using spectrogram leading portion, selection is most
Good adsorption time.The experimental results showed that there is a small amount of miscellaneous peak on spectrogram when first time stirring and adsorbing 20min, 30,40,60min
When spectrogram without miscellaneous peak occur, show to have reached adsorption equilibrium when 30min；After second is added fresh solvent, in 10min
Spectrogram still without miscellaneous peak, and there is miscellaneous peak again in 20min and later spectrogram, and extend as the time surveys, and the rate of recovery is also omited
There is increase.Show the extension adsorbed with secondary agitation, under the more system of dilute concentration sample, silica gel is to that need to remove object
There are certain parsing phenomenons for selective absorption.Therefore, the preferred 30min of first time adsorption time, second of adsorption time are preferred
10min。
The present invention is dense by silica gel water content, silica gel additive amount, sample to purify the rate of recovery of final product as leading indicator
The silica gel absorptions of the factors such as degree, mixing time purifies, joint molecular distillation purification techniques, in determining/long-chain STG purifying is refined
Optimised process./ during the synthetic method (ZL201110052579.2) of backbone triglycerides obtains/link is grown in a kind of
Structure triglycerides is raw material to be purified, the silochrom (moisture is less than 10%) of 10%-30% is first added, in 80 DEG C of item
Vacuum premixes 40min postcoolings to 60 DEG C or less vacuum breakers under part；Gui Jiao ︰ sample qualities to be purified are pressed again than for the total of 1 ︰ 1-2
Ratio adds a certain amount of silica gel, by sample quality：Solvent volume (m/v) is 1:A certain amount of petroleum ether of 6-12 additions (60~
90 DEG C), stirring and adsorbing 30min under conditions of room temperature or temperature control stands to mixed liquor layering and supernatant clarification, is transferred out of
After clear liquid, the 1/8-1/2 fresh solvents of first time solvent are added again in silica gel precipitation, continues to stir 10min, stand extremely
Mixed liquor be layered and supernatant clarify, be transferred out of supernatant and mixed with a preceding supernatant, by obtained mixed liquor 60 DEG C,
Rotary evaporation volatilizes solvent under the conditions of rotating speed 50rpm, and being dried in vacuo (80 DEG C, 40min) to sample obtains middle long-chain STG purifying
Intermediate.
Middle long-chain STG purifies intermediate after 40-60 DEG C of heat-insulation preheating, in feed rate 2-10mL/min, evaporating surface temperature
It is handled under conditions of degree 135 DEG C (90-150 DEG C), knifing rotating speed 126 (100-150rpm), vacuum degree < 5Pa, gained heavy phase is
For in after purification/long-chain STG.
The present invention establishes in a kind of injection stage/purification process of long-chain STG, belong to pionerring research.
The present invention provides in/selection gists of long-chain STG purifying process parameters, it is determined that in purifying/tool of long-chain STG
Body technology and parameter.
The present invention uses in this process purification/long-chain STG, moderate cost, it can be achieved that in/the domestic industrialization of long-chain STG
Production, product indices can meet State Food and Drug Administration's import drugs (structured triglyceride) registered standard
(standard No.：JX20070100 it) requires, is conducive to break in the country that backbone fat of triglyceride breast is long-term to rely on import, outer
The situation of enterprise's simple monopoly is provided, positive, orderly market competition structure is built.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although with reference to preferable
Embodiment describes the invention in detail, it will be understood by those of ordinary skill in the art that, it can be to the technology of the present invention
Scheme is modified or replaced equivalently, and without departing from the spirit of the technical scheme of the invention and range, should all be covered in this hair
In bright right.
Claims (10)
1. in a kind of injection stage/purification process of backbone triglycerides, it is characterised in that：Including,
Silica gel absorption purifies：In/backbone triglycerides crude product in silochrom is added, premix；Gross porosity color is added again
Compose silica gel and petroleum ether be added, in absorption and purification/backbone triglycerides obtain in/purifying of backbone triglycerides
Intermediate；
Molecular distillation is refined：The purifying intermediate preheating, adjustment feed rate, temperature, knifing rotating speed carry out molecular distillation essence
System, in obtaining after purification/backbone triglycerides.
2. in injection stage as described in claim 1/purification process of backbone triglycerides, it is characterised in that：The silicon
Glue adsorption and purification, wherein it is described in/backbone triglycerides crude product in be added silochrom, including in/backbone
10%~30% silochrom, the silochrom are added in triglycerides crude product, water content is no more than 10%.
3. in injection stage as claimed in claim 1 or 2/purification process of backbone triglycerides, it is characterised in that：It is described
Silica gel absorption purifies, wherein the premix, vacuum premixes 40min under conditions of being included in 80 DEG C, is cooled to 60 DEG C or less and breaks very
It is empty.
4. in injection stage as claimed in claim 1 or 2/purification process of backbone triglycerides, it is characterised in that：It is described
Gross porosity chromatography silica gel is added again and petroleum ether is added, including presses in the gross porosity Se spectrum Gui Jiao ︰/backbone triglycerides
Crude product quality for the ratio of 1 ︰ 1~2 than adding gross porosity chromatography silica gel, in pressing/backbone triglycerides crude product quality：Petroleum ether
The petroleum ether that boiling range is 60~90 DEG C is added in the ratio that volume is 1 ︰ 6~12, is adsorbed.
5. in injection stage as claimed in claim 4/purification process of backbone triglycerides, it is characterised in that：It is described again
Secondary addition gross porosity chromatography silica gel and addition petroleum ether, it is described to be adsorbed, it is included in stirring suction under conditions of room temperature or temperature control
Attached, time 30min stands, collects supernatant.
6. in injection stage as claimed in claim 5/purification process of backbone triglycerides, it is characterised in that：It is standing
Petroleum ether is added in the precipitation of the silica gel afterwards again, repeats stirring and adsorbing, time 10mim is stood, and collects supernatant, and
It is mixed with a preceding supernatant.
7. as in injection stage described in claim 5 or 6/purification process of backbone triglycerides, it is characterised in that：Will
To supernatant evaporation volatilize, the evaporation volatilizes, and is included in temperature for 60 DEG C, rotary evaporation under the conditions of rotating speed 50rpm
It volatilizes.
8. in injection stage as claimed in claim 7/purification process of backbone triglycerides, it is characterised in that：Further include,
Evaporation is dried in vacuo after volatilizing, and temperature is 80 DEG C, time 40min, obtain it is described in/purifying of backbone triglycerides
Intermediate.
9. in the injection stage as described in claim 1,2,5,6 or 8 are any/purification process of backbone triglycerides, it is special
Sign is：The molecular distillation is refined, including, will described in/backbone triglycerides purifying intermediate is through 40~60 DEG C of guarantors
After temperature preheating, in 2~10mL/min of feed rate, 90-150 DEG C of evaporating surface temperature, knifing rotating speed 100-150rpm, vacuum degree <
It is handled under conditions of 5Pa, in obtaining after purification/backbone triglycerides.
10. in any injection stage of claim 1~9/the obtained injection of the purification process of backbone triglycerides
In/backbone triglycerides, it is characterised in that：In the injection/the backbone triglycerides rate of recovery reach 75% with
On.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810516704.2A CN108753451B (en) | 2018-05-25 | 2018-05-25 | Purification method of injection-grade triglyceride with medium/long chain structure and product thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810516704.2A CN108753451B (en) | 2018-05-25 | 2018-05-25 | Purification method of injection-grade triglyceride with medium/long chain structure and product thereof |
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| CN112661641A (en) * | 2020-12-09 | 2021-04-16 | 江南大学 | Method for separating and purifying medium-long chain structure ester |
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