CN104152501A - Gradual cooling auxiliary enzymatic method for glycerolysis preparation of lard diglyceride - Google Patents
Gradual cooling auxiliary enzymatic method for glycerolysis preparation of lard diglyceride Download PDFInfo
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- CN104152501A CN104152501A CN201410399993.4A CN201410399993A CN104152501A CN 104152501 A CN104152501 A CN 104152501A CN 201410399993 A CN201410399993 A CN 201410399993A CN 104152501 A CN104152501 A CN 104152501A
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Abstract
A gradual cooling auxiliary enzymatic method for glycerolysis preparation of lard diglyceride belongs to the field of deep processing of lard. The method comprises the steps as follows: 1, removing water from raw materials of lard and glycerin in a molar ratio of 1-3:1 under vacuum and heating conditions; 2, adding a catalyst 1,3 specific lipase LipozymeRM IM in the weight 6-16% of the lard, and gradually cooling with magnetic stirring, reacting at 60-70 DEG C for 2-4 h, reacting at 50-60 DEG C for 2-4 h, reacting at 35-50 DEG C for 4-20 h; and 3, after the reaction, taking out the sample, and filtering to remove the lipase, so as to obtain the lard diglyceride. The invention uses lard as the raw material and employs the gradual cooling auxiliary enzymatic method for glycerolysis preparation of lard diglyceride, so as to make full utilization of the cheap lard resource; at the same time, the invention has the advantages of no organic solvent residual and easy separation of product and enzyme, and lays foundation for constructing processing technology of healthful diacylglycerol oil.
Description
Technical field
The invention belongs to lard deep processing field, relate to a kind of auxiliary technique of preparing triglyceride of progressively cooling that adopts in lipase glycerine solution lard in solvent-free system.
Background technology
Triglyceride (diacylglycerol, DAG) is two hydroxyls of glycerine and the product after fatty acid esterification, with trace ingredients, is present in natural animal-plant grease.Triglyceride has 1,3-DAG and 1,2 (or 2,3)-two kinds of DAG isomer, in most natural fats and oils and artificial triglyceride, mainly with 1,3-DAG form, exists.Be rich in that the oil of triglyceride and the oil of triglyceride level (triglyceride, TAG) have similar taste, smell, color and luster, culinary art characteristic and to heat with oxygen is all had to certain stability.But the two metabolic mechanism is in vivo different.In triglyceride molecular structure, have two longer chain fatty acids, lipophilicity is stronger, meanwhile, also contains a hydrophilic radical-OH, therefore shows stronger surfactivity, adds the matter structure that can improve product in food to.Recent researches shows, after 1,3-DAG is edible, does not accumulate in vivo, can play reducing blood-fat to humans and animals, reduces body fat, suppress the functions such as body weight increase.
China's lard aboundresources, but its fusing point is higher, is difficult to digest and assimilate in human body, the main fatty acid simultaneously forming is longer chain fatty acid, and the heat providing is higher, so its processing and utilization degree is lower.How making full use of this reproducible low-cost resource of lard, increase utility value, is current problem demanding prompt solution.The fusing point of triglyceride, lower than triglyceride level, in glycerolysis reaction, adopts progressively cooling can significantly improve the productive rate of triglyceride.
Summary of the invention
The object of the present invention is to provide the auxiliary enzyme process glycerine solution of a kind of progressively cooling to prepare the method for lard triglyceride, take lard as raw material, utilize the auxiliary enzyme process of progressively cooling to carry out glycerine solution and prepare lard triglyceride, the resource of this cheapness of lard is fully used, organic solvent-free is residual simultaneously, it is separated that product and enzyme are easy to, and for building healthy triglyceride oil complete processing, lays a good foundation.
The object of the invention is to be achieved through the following technical solutions:
The auxiliary enzyme process glycerine solution of a kind of progressively cooling is prepared the method for lard triglyceride, take lard as raw material, in solvent-free system, enzyme process glycerine solution is prepared triglyceride, initial for some time reaction is carried out under the optimum temperuture of enzyme, make enzyme keep maximum vigor, reduce sweet oil viscosity simultaneously, reduce gradually subsequently temperature, the product generating is constantly separated out, being beneficial to reaction carries out to the direction that generates target compound, when temperature reduces again, the reactant of bottle mural margin is solid-state, further carrying out of impact reaction, in the triglyceride that adopts this method to generate, have higher by 1, the content of 3-triglyceride.Concrete preparation process is as follows:
One, take mol ratio as 1～3: 1 lard and glycerine are raw material, under the condition of decompression (vacuum tightness is-100kpa～-30kpa), heating (28～90 ℃), first remove moisture;
Two, the catalyzer 1 that then adds lard weight 6～16%, 3-specific lipase Lipozyme RM IM, magnetic agitation speed is 300～900r/min, 60～70 ℃ of reaction 2～4h, 50～60 ℃ of reaction 2～4h, 35～50 ℃ of reaction 4～20h;
Three, reaction finishes rear taking-up sample, removes by filter lipase, obtains lard triglyceride.
Four, utilize high effective liquid chromatography for measuring 1,3-DAG content, it is qualitative that different components utilizes standard substance to carry out, and each component concentration is pressed area normalization method and is calculated.Utilize gas chromatograph-mass spectrometer to analyze the lipid acid of product simultaneously, adopt infrared spectrometer to carry out qualitative analysis to the structure of product.
Than prior art, the present invention has following beneficial effect:
1, adopt narrow spectrum immobilized lipase, under solvent-free system, animal oil is carried out to glycerolysis reaction and prepare triglyceride, in reaction product, do not have undesirable substance to produce, do not exist organic solvent residual and enzyme and product to be easy to separated.
2, take lard as raw material, the resource of this cheapness is fully used, in preparation process, adopt diglyceride content that progressively falling temperature method obtains to be significantly higher than simultaneously and under same temperature, react the diglyceride content obtaining, can produce the triglyceride of generally regarded as safe high yield.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of lard glycerine hydrolysis products and lard.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described; but do not limit to so; every technical solution of the present invention is modified or is equal to replacement, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment 1:
The mol ratio lard of 1: 1 and glycerine are mixed in round-bottomed flask, in vacuum tightness-50.0kpa, Heating temperature, be to dewater after 30min under the condition of 82 ℃, mixture after dehydration is transferred in Erlenmeyer flask, add oil to weigh 10% Lipozyme RM IM, under the magnetic agitation speed of 400r/min, react.Initial reaction temperature is 65 ℃, after reaction 2h, temperature is adjusted to 55 ℃, reaction 2h, then temperature is adjusted to 40 ℃ of reaction 6h, and after reaction finishes, remove by filter lipase, obtain lard glycerine hydrolysis products.In this product of efficient liquid phase chromatographic analysis, the content of DAG is that 41.81%, 1,3-DAG content is 26.52%.
Embodiment 2:
The mol ratio lard of 1: 1 and glycerine are mixed in round-bottomed flask, in vacuum tightness-50kpa, Heating temperature, be to dewater after 30min under the condition of 82 ℃, mixture after dehydration is transferred in Erlenmeyer flask, add oil to weigh 14% Lipozyme RM IM, under the magnetic agitation speed of 400r/min, react.Initial reaction temperature is 65 ℃, after reaction 2h, temperature is adjusted to 55 ℃, reaction 2h, then temperature is adjusted to 40 ℃ of reaction 6h, and after reaction finishes, remove by filter lipase, obtain lard glycerine hydrolysis products.In this product of efficient liquid phase chromatographic analysis, the content of DAG is that 54.04%, 1,3-DAG content is 39.68%.
Embodiment 3:
The mol ratio lard of 2: 1 and glycerine are mixed in round-bottomed flask, in vacuum tightness-50kpa, Heating temperature, be to dewater after 30min under the condition of 82 ℃, mixture after dehydration is transferred in Erlenmeyer flask, add oil to weigh 14% Lipozyme RM IM, under the magnetic agitation speed of 400r/min, react.Initial reaction temperature is 65 ℃, after reaction 2h, temperature is adjusted to 55 ℃, reaction 2h, then temperature is adjusted to 40 ℃ of reaction 6h, and after reaction finishes, remove by filter lipase, obtain lard glycerine hydrolysis products.In this product of efficient liquid phase chromatographic analysis, the content of DAG is that 51.27%, 1,3-DAG content is 38.28%.
Embodiment 4:
The mol ratio lard of 1: 1 and glycerine are mixed in round-bottomed flask, in vacuum tightness-50kpa, Heating temperature, be to dewater after 30min under the condition of 82 ℃, mixture after dehydration is transferred in Erlenmeyer flask, add oil to weigh 14% Lipozyme RM IM, under the magnetic agitation speed of 500r/min, react.Initial reaction temperature is 65 ℃, after reaction 2h, temperature is adjusted to 55 ℃, reaction 2h, then temperature is adjusted to 40 ℃ of reaction 8h, and after reaction finishes, remove by filter lipase, obtain lard glycerine hydrolysis products.In this product of efficient liquid phase chromatographic analysis, the content of DAG is that 58.53%, 1,3-DAG content is 37.91%.
Embodiment 5:
The mol ratio lard of 1: 1 and glycerine are mixed in round-bottomed flask, in vacuum tightness-50kpa, Heating temperature, be to dewater after 30min under the condition of 82 ℃, mixture after dehydration is transferred in Erlenmeyer flask, add oil to weigh 14% Lipozyme RM IM, under the magnetic agitation speed of 500r/min, react.Initial reaction temperature is 65 ℃, after reaction 2h, temperature is adjusted to 55 ℃, reaction 2h, then temperature is adjusted to 45 ℃ of reaction 6h, and after reaction finishes, remove by filter lipase, obtain lard glycerine hydrolysis products.In this product of efficient liquid phase chromatographic analysis, the content of DAG is that 57.73%, 1,3-DAG content is 37.73%.
The lard glycerine hydrolysis products that the present embodiment is obtained carries out fatty acid compositional analysis and Structural Identification, the results are shown in Table 1 and Fig. 1.
Table 1 lard and lard glycerine hydrolysis products chief component lipid acid and content
Claims (8)
1. progressively cooling assists enzyme process glycerine solution to prepare a method for lard triglyceride, it is characterized in that described method steps is as follows:
One, take mol ratio as 1～3: 1 lard and glycerine are raw material, under the condition of decompression, heating, first remove moisture;
Two, the catalyzer 1 that then adds lard weight 6～16%, 3-specific lipase Lipozyme RM IM, progressively cooling under magnetic agitation condition: 60～70 ℃ of reaction 2～4h, 50～60 ℃ of reaction 2～4h, 35～50 ℃ of reaction 4～20h;
Three, reaction finishes rear taking-up sample, removes by filter lipase, obtains lard triglyceride.
2. the auxiliary enzyme process glycerine solution of progressively cooling according to claim 1 is prepared the method for lard triglyceride, it is characterized in that described reduced vacuum degree is-100kpa～-30kpa.
3. the auxiliary enzyme process glycerine solution of progressively cooling according to claim 1 is prepared the method for lard triglyceride, it is characterized in that described Heating temperature is 28～90 ℃.
4. the auxiliary enzyme process glycerine solution of progressively cooling according to claim 1 is prepared the method for lard triglyceride, it is characterized in that in described step 2, and magnetic agitation speed is 300～900r/min.
5. the auxiliary enzyme process glycerine solution of progressively cooling according to claim 1 is prepared the method for lard triglyceride, and the mol ratio that it is characterized in that described lard and glycerine is 1: 1.
6. the auxiliary enzyme process glycerine solution of progressively cooling according to claim 1 is prepared the method for lard triglyceride, and the mol ratio that it is characterized in that described lard and glycerine is 2: 1.
7. the auxiliary enzyme process glycerine solution of progressively cooling according to claim 1 is prepared the method for lard triglyceride, it is characterized in that described catalyzer 1, and the add-on of 3-specific lipase is 10% of lard weight.
8. the auxiliary enzyme process glycerine solution of progressively cooling according to claim 1 is prepared the method for lard triglyceride, it is characterized in that described catalyzer 1, and the add-on of 3-specific lipase is 14% of lard weight.
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| CN201410399993.4A CN104152501A (en) | 2014-08-14 | 2014-08-14 | Gradual cooling auxiliary enzymatic method for glycerolysis preparation of lard diglyceride |
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| CN201410399993.4A CN104152501A (en) | 2014-08-14 | 2014-08-14 | Gradual cooling auxiliary enzymatic method for glycerolysis preparation of lard diglyceride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104830920A (en) * | 2015-04-09 | 2015-08-12 | 华南理工大学 | Method for producing diglyceride |
| CN104928326A (en) * | 2015-07-07 | 2015-09-23 | 安徽农业大学 | Preparation method for 1, 3-diglyceride pork fat |
| CN111235190A (en) * | 2020-01-22 | 2020-06-05 | 新疆农业大学 | Horse oil rich in diglyceride and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1267322A (en) * | 1997-08-18 | 2000-09-20 | 花王株式会社 | Process for producing diglycerides |
| US20030054509A1 (en) * | 2001-04-06 | 2003-03-20 | Archer-Daniels-Midland Company | Method for producing fats or oils |
-
2014
- 2014-08-14 CN CN201410399993.4A patent/CN104152501A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1267322A (en) * | 1997-08-18 | 2000-09-20 | 花王株式会社 | Process for producing diglycerides |
| US20030054509A1 (en) * | 2001-04-06 | 2003-03-20 | Archer-Daniels-Midland Company | Method for producing fats or oils |
Non-Patent Citations (3)
| Title |
|---|
| GERALD P. MCNEILL ET AL.: "Selective Distribution of Saturated Fatty Acids into the Monoglyceride Fraction During Enzymatic Glycerolysis", 《J. AM. OIL.CHEM. SOC.》 * |
| TSUNEO YAMANE ET AL.: "High Yield Diacylglycerol Formation by Solid-Phase Enzymatic Glycerolysis of Hydrogenated Beef Tallow", 《J. AM. OIL.CHEM. SOC.》 * |
| 段章群等: "生物酶法制备1,3-甘油二酯", 《化学进展》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104830920A (en) * | 2015-04-09 | 2015-08-12 | 华南理工大学 | Method for producing diglyceride |
| CN104830920B (en) * | 2015-04-09 | 2018-12-11 | 华南理工大学 | A kind of production method of diglyceride |
| CN104928326A (en) * | 2015-07-07 | 2015-09-23 | 安徽农业大学 | Preparation method for 1, 3-diglyceride pork fat |
| CN111235190A (en) * | 2020-01-22 | 2020-06-05 | 新疆农业大学 | Horse oil rich in diglyceride and preparation method thereof |
| CN111235190B (en) * | 2020-01-22 | 2023-11-07 | 新疆农业大学 | Horse oil rich in diglyceride and preparation method thereof |
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