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CN114574281A - Enzymatic degumming method for strong-flavor oil - Google Patents

Enzymatic degumming method for strong-flavor oil Download PDF

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CN114574281A
CN114574281A CN202111476974.3A CN202111476974A CN114574281A CN 114574281 A CN114574281 A CN 114574281A CN 202111476974 A CN202111476974 A CN 202111476974A CN 114574281 A CN114574281 A CN 114574281A
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oil
degumming
enzyme
phospholipase
strong
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程倩
李晓龙
初柏君
王翔宇
王风艳
惠菊
王满意
张宇
杨建维
王磊
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Cofco Grease Guangyuan Co ltd
Cofco Nutrition and Health Research Institute Co Ltd
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Cofco Nutrition and Health Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/003Refining fats or fatty oils by enzymes or microorganisms, living or dead
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/16Refining fats or fatty oils by mechanical means

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Abstract

The invention provides an enzymatic degumming method of strong flavor oil, which firstly uses phospholipase (such as phospholipase used under neutral condition with pH of 6-8) for the first time
Figure DDA0003393831540000011
PLC enzymes and/or
Figure DDA0003393831540000012
3G enzyme) is applied to the enzymatic degumming production of the strong flavor oil, so that free fatty acid is not generated (or used) by utilizing the specific phospholipase
Figure DDA0003393831540000013
3G enzyme generates little free fatty acid), can improve the yield of the oil and fat, quickly separate oil and oil gel, and improve the product quality and the product transmission on the basis of not influencing the flavor of the flavor oil and fatThe system hydration degumming method has no obvious difference and even has more excellent quality.

Description

Enzymatic degumming method for strong-flavor oil
Technical Field
The invention relates to an enzymatic degumming method of strong aromatic flavor oil, belonging to the field of food production.
Background
(1) The kind of common phospholipids
Phospholipids can be classified into glycerophospholipids and neurophosphates according to their structure, with glycerophospholipids being the most common of vegetable oils. Glycerophospholipids are generally composed of 1, 2-difatty acid glycerolipid combined with phosphate radical, then the phosphate radical is combined with small molecular base to form a large class of substances, and different types of glycerophospholipids are formed by different small molecular base substances X combined with phosphate sites (as shown in figure 1). Phospholipids in plants are mainly in the form of Phosphatidylcholine (PC), Phosphatidylinositol (PI), Phosphatidylethanolamine (PE), Phosphatidic Acid (PA), and the like.
(2) Kind and mechanism of action of phospholipase
Phospholipase has various kinds, and can be classified into phospholipase A according to different action sites (see FIG. 2)1(PLA1) And phospholipase A2(PLA2) Phospholipase B (PLB), phospholipase C (PLC), phospholipase D (PLD), etc. PLA (polylactic acid)1、PLA2Respectively hydrolyzing fatty acid at sn-1 and sn-2 positions of phospholipid and generating lysophospholipid with stronger hydrophilicity; PLB can act on Sn-1 and Sn-2 positions simultaneously to hydrolyze phospholipid to generate glycerylphospholipid with stronger hydrophilicity. Phospholipase C (PLC) can specifically act on the glycerol phosphate ester bond at Sn-3 position of phospholipid to generate lipophilic Diglyceride (DAG) and phosphorus-containing group; the product of PLD hydrolysis of phospholipids remains as less hydrophilic phosphatidic acid, and does not function as degumming. Thus, PLA is used1、PLA2The PLB and the PLC can achieve certain degumming effect in different degrees.
TABLE 1 differences in substrate range enzymatic degumming of different phospholipases for phospholipid removal
Figure BDA0003393831520000011
Figure BDA0003393831520000021
The degumming method in the prior art comprises hydration degumming and enzymatic degumming, wherein the hydration degumming is a degumming mode for removing crude oil peptized impurities by using a certain amount of water or electrolyte by utilizing the hydrophilicity of the peptized impurities such as phospholipid. For example, maintaining room temperature environment, adding 0.8-2.0% hot water salt solution (citric acid solution or pure water), allowing sufficient contact reaction for 20-40min, naturally settling or centrifuging to remove phospholipid such as PC, PI and PE, and removing the rest main component such as PA. Enzymatic degumming is a degumming mode for degumming by adopting phospholipase, and the reaction conditions and the phospholipid removal types are determined by the characteristics of enzymes.
At present, the phospholipase with a large using amount in the domestic market is phospholipase PLA1(Lecitase
Figure BDA0003393831520000022
) Phospholipase PLA1(
Figure BDA0003393831520000023
PLA1) Phospholipase PLC (a)
Figure BDA0003393831520000024
PLC and Mixed phospholipase: (
Figure BDA0003393831520000025
3G) In that respect Wherein Lecitase
Figure BDA0003393831520000026
The reaction conditions of the enzyme are that the pH is 4.5-5.5,
Figure BDA0003393831520000027
PLA1the reaction conditions of the enzyme are that the pH is 3.5-4.5, and two kinds of PLA are used1The hydrolysis products of the enzyme are lysophospholipid (easily soluble in water) and free fatty acid (insoluble in water and retained in grease);
Figure BDA0003393831520000028
the optimal pH of PLC is 6.5-7.5, the hydrolysis substrates are mainly PE and PC, and the products are diglyceride (retained in grease) and corresponding phosphorus-containing group (dissolved in water);
Figure BDA0003393831520000029
3G is a mixed enzyme with an optimum pH of 6.5-7.5, the hydrolysis substrates are mainly PE, PC and PI, and the products are diglycerides (retained in fats and oils) and corresponding phosphorus-containing groups (dissolved in water).
According to the difference of the fragrance, the edible oil can be generally divided into common type edible oil and strong-fragrance type edible oil, wherein the common type edible oil generally has no fragrance, such as primary refined soybean oil; the strong-flavor edible oil is edible oil rich in strong flavor, such as strong-flavor peanut oil, strong-flavor rapeseed oil and the like. Whether the edible oil has the fragrance is closely related to whether the seed frying process exists, and in the oil preparation process, if the same raw materials are not fried, the prepared crude oil is common crude oil and generally does not have obvious aromatic fragrance; if the crude oil is fried, the prepared crude oil is strong-flavor crude oil and has obvious rich flavor. The crude oil is further processed by degumming and the like to obtain the finished product of edible oil. Compared with the common edible oil, the aroma type finished edible oil obtained by further processing the aroma type crude oil has unique flavor and rich aroma, so that the aroma type finished edible oil is popular with consumers.
However, the degumming process of the conventional common crude oil cannot be simply applied to the strong aromatic crude oil, because the strong aromatic crude oil has a large amount of flavor substances and strict processing requirements, unlike the common crude oil. Besides, the strong-flavor oil needs to meet the conventional indexes such as acid value, peroxide value, color value and moisture, and also needs to meet the requirements of good flavor and flavor stability after degumming. In the existing strong aromatic flavor oil enzymatic degumming technology, attention is focused on the aspect of high oil yield, and the quality of products, particularly the flavor and the stability of the flavor are rarely evaluated. In particular, the existing enzymatic degumming scheme of the strong aromatic flavor oil mainly has the following problems:
1.PLA1the reaction condition of the enzyme is acidic, corresponding acid and alkali are required to be added to adjust the pH value so as to ensure the reaction condition, and the addition of the acid and the alkali can influence the flavor of the thick sesame oil and even generate adverse effect;
2.PLA1the reaction product of the enzyme has free fatty acid, the increase of the fatty acid can cause the increase of acid value, and the raw material with poor quality can hardly meet the quality requirement; in addition, the fatty acid has a rancid flavor and the flavor of the oil is easily influenced;
3. in the traditional hydration degumming method, if citric acid solution is added for degumming, the original flavor of the aromatic oil can be changed; if the salt solution is added, the flavor of the thick sesame oil is slightly influenced, but the thick sesame oil is also influenced to a certain extent, and chloride ions are introduced, so that risk factors of eating safety are brought;
4. many enzymes are used to add acid and alkali to adjust the pH, and in the application of the existing enzymatic degumming technology of strong-flavor oil, only the influence of the enzymatic degumming technology on the oil yield is concerned, and the influence on the flavor and the product quality (acid value) is not concerned.
Therefore, the prior art needs an enzymatic degumming technology which does not influence the flavor and the quality of the strong aromatic flavor oil.
Disclosure of Invention
In order to solve the above problems, the present inventors have conducted intensive studies on a strong flavor oil and fat and have first studied a phospholipase (e.g., phospholipase used under neutral conditions at pH 6 to 8) used under neutral conditions
Figure BDA0003393831520000031
PLC enzymes and/or
Figure BDA0003393831520000032
3G enzyme) is applied to the enzymatic degumming production of the strong aromatic flavor oil, thereby providing an enzymatic degumming technology of the strong aromatic flavor oil, which has high oil yield and product quality which is not inferior to or even superior to that of the traditional hydration degumming method on the basis of not influencing the flavor of the flavor oil.
Specifically, the invention is realized by the following aspects:
in a first aspect, the invention provides a preparation method of a strong aromatic edible vegetable oil product, which comprises the following steps:
(1) weighing 0.8-1.2Kg of strong aromatic plant crude oil, and keeping the temperature at 25-60 ℃;
(2) adding 0.8-2.0% water and 50-200ppm phospholipase (such as phospholipase used under neutral pH of 6-8)
Figure BDA0003393831520000041
PLC enzymes and/or
Figure BDA0003393831520000042
3G enzyme) are fully mixed;
(3) and after mixing, fully reacting for 1-5h, and separating oil from oleogum through natural sedimentation or centrifugal separation to obtain the strong-flavor edible oil product.
In a second aspect, the invention provides an enzymatic degumming method for strong aromatic plant crude oil, which comprises the following steps:
(1) weighing 0.8-1.2Kg of strong aromatic plant crude oil, and keeping the temperature at 25-60 ℃;
(2) adding 0.8-2.0% water and 50-200ppm phospholipase (such as phospholipase used under neutral pH of 6-8)
Figure BDA0003393831520000043
PLC enzymes and/or
Figure BDA0003393831520000044
3G enzyme) are fully mixed;
(3) and after mixing, fully reacting for 1-5h, and separating oil from oil gum through natural sedimentation or centrifugal separation to realize degumming of the strong aromatic plant crude oil.
In a third aspect, the invention provides a phospholipase for use at neutral pH of 6 to 8 (e.g., a phospholipase for use at pH 6 to 8
Figure BDA0003393831520000045
PLC enzymes and/or
Figure BDA0003393831520000046
3G enzyme) in preparing strong aromatic edible vegetable oil products and/or carrying out enzymatic degumming on strong aromatic vegetable crude oil.
Advantageous effects
The invention selects phospholipase under neutral condition (pH 6-8), especially PLC enzyme or mixture of PLC enzymes (such as
Figure BDA0003393831520000047
3G enzyme, wherein,
Figure BDA0003393831520000048
the 3G enzyme is the existing PLC enzyme, PI-PLC enzyme and a trace amount of PLA2Enzyme mixed enzyme preparation), the present invention does not produce free fatty acid by using PLC enzyme (or is in use)
Figure BDA0003393831520000049
3G enzyme produces very little free fatty acid), the following beneficial technical effects can be achieved: (1) the method has the advantages that the yield of the oil is improved, meanwhile, (2) the acid value of the oil is not obviously increased, and (3) the flavor of the oil is not influenced because acid and alkali are not required to be added.
Drawings
Fig. 1 is a schematic diagram showing the molecular structure of phospholipid.
Fig. 2 is a schematic diagram showing the action site of phospholipase.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
In one embodiment, the present invention provides a method for preparing a highly flavored edible vegetable oil product, comprising the steps of:
(1) weighing 0.8-1.2Kg of strong aromatic plant crude oil, and keeping the temperature at 25-60 ℃;
(2) adding 0.8-2.0% water and 50-200ppm phospholipase (such as phospholipase used under neutral pH of 6-8)
Figure BDA0003393831520000051
PLC enzymes and/or
Figure BDA0003393831520000052
3G enzyme) are fully mixed;
(3) and after mixing, fully reacting for 1-5h, and separating oil from oleogum through natural sedimentation or centrifugal separation to obtain the strong-flavor edible oil product.
In another embodiment, the invention provides a method for degumming a strong aromatic vegetable crude oil by an enzyme method, which comprises the following steps:
(1) weighing 0.8-1.2Kg of strong aromatic plant crude oil, and keeping the temperature at 25-60 ℃;
(2) adding 0.8-2.0% water and 50-200ppm phospholipase (such as phospholipase used under neutral pH of 6-8)
Figure BDA0003393831520000053
PLC enzymes and/or
Figure BDA0003393831520000054
3G enzyme) are fully mixed;
(3) and after mixing, fully reacting for 1-5h, and separating oil from oil gum through natural sedimentation or centrifugal separation to realize degumming of the strong aromatic plant crude oil.
In the present invention, the terms "highly flavored vegetable crude oil" and "edible vegetable oil product" are used in terms of taste to refer to vegetable crude oil and edible vegetable edible oil, respectively, having a flavor of the type of highly flavored, burnt, sauced, scented, etc., such as: strong-flavor peanut oil, strong-flavor rapeseed oil, strong-flavor corn oil, strong-flavor soybean oil, strong-flavor sunflower seed oil and the like.
In the invention, in terms of production process, the term "strong aromatic plant crude oil" is used to refer to plant crude oil obtained by stir-frying and squeezing plant raw materials; the term "strong aromatic edible vegetable oil product" refers to a vegetable oil product obtained by subjecting strong aromatic vegetable crude oil to hydration degumming or enzymatic degumming.
In a preferred embodiment, in step (1), the aromatic vegetable crude oil includes, but is not limited to, one or more of aromatic peanut oil, aromatic rapeseed oil, aromatic soybean oil and the like.
In a preferred embodiment, in the step (1), 1-1.2Kg of the aromatic plant crude oil is weighed, and the temperature is kept at 25-30 ℃. If the temperature in step (1) is higher than 60 ℃, the activity of the enzyme preparation in the degumming process is affected.
In the present invention, the term "degumming" is used to refer to a process for removing peptized impurities (phospholipids, proteins, etc.) from crude oil. The traditional degumming methods mainly comprise hydration degumming and acid degumming. The enzymatic degumming has high oil yield, less acid and alkali addition and wasteThe method has the advantages of low water discharge, mild reaction conditions and the like, is economic and environment-friendly, can be widely applied and rapidly developed in the oil processing industry, and can be applied to flavor oil. The processing method of the strong-flavor edible vegetable oil with strong flavor generally adopts pure water, salt water or citric acid aqueous solution for degumming, commonly called hydration degumming. However, the strong aromatic edible vegetable oil has strict requirements on processing conditions, and few researches on the production of the strong aromatic edible vegetable oil by enzymatic degumming without influencing the flavor and stability of the strong aromatic edible vegetable oil are carried out in the prior art. In addition, most of the phospholipase and the process adopted in the existing process for producing the strong aromatic edible vegetable oil have adverse effects on the flavor of the strong aromatic edible vegetable oil, and the strong aromatic edible vegetable oil finished product is difficult to obtain under the condition of not influencing the strong flavor of the strong aromatic edible vegetable oil. At present, no domestic manufacturers use phospholipases which are used at pH 6-8 neutral conditions (e.g.phospholipase
Figure BDA0003393831520000061
PLC enzymes and/or
Figure BDA0003393831520000062
3G enzyme) for degumming strong aromatic crude oil by enzyme method, PLA is mostly used1Enzymes (used under acidic conditions) perform enzymatic degumming on soybean oil.
The present inventors have found that a phospholipase used at pH 6-8 neutral conditions (e.g., phospholipase may be used
Figure BDA0003393831520000063
PLC enzymes and/or
Figure BDA0003393831520000064
3G enzyme) is applied to the enzymatic degumming production of the strong aromatic flavor oil, wherein,
Figure BDA0003393831520000065
PLC enzymes and/or
Figure BDA0003393831520000066
The reaction condition of the 3G enzyme is relatively mild, the optimal pH is about 7, and no acid is neededThe addition of alkali can achieve the effects of not affecting the flavor of the thick sesame oil and improving the yield of the oil.
In a preferred embodiment, in step (2), 0.8-1.0% of water and 150-200ppm of water are added
Figure BDA0003393831520000067
PLC enzymes and/or
Figure BDA0003393831520000068
The 3G enzyme was mixed well. The present inventors found that, if the amount of water added in step (2) is more than 2.0%, on the one hand, the input cost of water and the cost of wastewater treatment at the later stage increase; on the other hand, too much water can generate more oil-in-water/water-in-oil emulsification systems, which is not beneficial to improving the yield of the grease and causes the waste of the grease.
In a preferred embodiment, in step (3), the mixture is allowed to react for a further 2 to 4 hours, followed by said natural sedimentation or centrifugation.
The centrifugal method adopts a centrifugal machine to assist oil-water separation, and can realize continuous instant separation.
In one embodiment, the invention provides a phospholipase for use at pH 6-8 neutral conditions (e.g., pH 6-8)
Figure BDA0003393831520000071
PLC enzymes and/or
Figure BDA0003393831520000072
3G enzyme) in preparing strong aromatic edible vegetable oil products and/or carrying out enzymatic degumming on strong aromatic vegetable crude oil.
Therefore, the enzymatic degumming method provided by the invention can not influence the flavor and stability of the strong aromatic flavor oil on the basis of improving the oil yield. The method can improve the yield of the oil without influencing the flavor, and the separation speed of the oil and the oil glue is accelerated under the condition of adopting a natural sedimentation method, thereby greatly improving the production efficiency.
Examples
The present invention will be described in further detail with reference to examples, but the present invention is not limited to these examples. The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials, devices and the like used in the following examples are commercially available or can be prepared by those skilled in the art according to the ordinary skill in the art, unless otherwise specified. The PLC enzyme of the present invention (trade name
Figure BDA0003393831520000073
PLC)、PLA1Enzyme (trade name
Figure BDA0003393831520000074
PLA1) And 3G enzyme (trade name
Figure BDA0003393831520000075
3G) Supplied by imperial (china) ltd. Unless otherwise indicated,% as used herein refers to wt%.
Method for calculating oil yield
Centrifugal separation method:
the samples treated in the following examples were each subjected to separation of oil m1And gum m2And weighing, measuring the water content x and the acid value y in the oil by using a Karl's moisture meter, measuring the water content in the oil gel by using a rapid moisture meter, and measuring the oil content in the gel.
Figure BDA0003393831520000076
In the formula:
m1for oil weight separation, unit is g;
x is the water content in the oil;
y is the acid value in mg/g.
A natural sedimentation method:
after the reaction, the mixture is transferred to a 100mL measuring cylinder for natural sedimentation, and the volume V of the mixed solution is recorded1Recording the oil residue in the cylinder after 7 days of settlingVolume V2And transferring an upper oil sample after the oil rate is calculated, taking a small amount of the upper oil sample to measure the water content, recording the water content as w, and sampling to measure the phosphorus content after degumming.
Oil yield is (V)1-V2)/V1(formula 2)
Example 1
Degumming by a PLC (programmable logic controller) enzyme method: weighing 1Kg of strong aromatic small crude oil of mustard seed oil, maintaining the temperature at 30 deg.C, adding 1.5% of water and 200ppm of crude oil
Figure BDA0003393831520000081
After the PLC enzymes are fully mixed, the mixture is fully reacted for 3 hours, and is centrifuged at 4500rpm for 10 minutes, the oil and the oil gum are separated to obtain the degummed oil, and the degummed result is shown in a table 2.
3G enzymatic degumming: degumming was performed in the same manner as the PLC enzymatic method described above, except that the PLC enzyme was replaced with 3G enzyme, to obtain degummed oil, and the degumming results are shown in table 2.
Comparative example 1
Degumming by a traditional method: weighing 1Kg of strong aromatic small crude oil of tuber mustard seed oil, keeping the temperature at 30 ℃, adding 0.8% aqueous solution, then fully reacting for 3h for degumming, centrifuging at 4500rpm for 10min to obtain the degumming oil, and the degumming result is shown in Table 2.
PLA1Degumming by an enzymatic method: weighing 1Kg of strong aromatic small crude oil of tuber mustard seed oil, maintaining the temperature at 30 deg.C, adding 0.8% water solution and 100ppm of PLA1After fully mixing the enzyme and 0.04% citric acid, fully reacting for 3h, centrifuging at 4500rpm for 10min to obtain the degumming oil, and the degumming result is shown in Table 2.
TABLE 2 results of degumming on strong-scented rapeseed oil with the conventional method and different enzyme preparations (centrifugation)
Figure BDA0003393831520000082
Example 2
Degumming by a PLC (programmable logic controller) enzyme method: weighing 1Kg of strong aromatic type small crude oil of tuber mustard seed oil, keeping the temperature at 30 ℃, adding 1.5% of water and 100ppm of PLC enzyme, fully mixing, fully reacting for 2 hours, and naturally settling for 7 days to obtain the degummed oil, wherein the degummed oil has the degumming result shown in Table 3.
3G enzymatic degumming: degumming was performed in the same manner as the PLC enzymatic method described above, except that the PLC enzyme was replaced with 3G enzyme, to obtain degummed oil, and the degumming results are shown in table 3.
Comparative example 2
Degumming by a traditional method: weighing 1Kg of strong aromatic type small crude oil of mustard seed oil, keeping the temperature at 30 ℃, adding 1.5% of 10% salt solution, fully mixing, fully reacting for 2h, and naturally settling for 7d to obtain the degummed oil, wherein the degummed oil has the degumming result shown in Table 3.
PLA1Degumming by an enzymatic method: weighing 1Kg of strong-flavor small crude oil of tuber mustard seed oil, keeping the temperature at 30 ℃, and 50ppm of PLA1And fully mixing the enzyme and 0.04% citric acid, then fully reacting for 2 hours, naturally settling for 7 days to obtain the degummed oil, wherein the degumming result is shown in Table 3.
TABLE 3 results of degumming on strong-scented rapeseed oil with the conventional method and different enzyme preparations (natural sedimentation method)
Figure BDA0003393831520000091
Example 3
Degumming by a PLC (programmable logic controller) enzyme method: weighing 1Kg of strong aromatic peanut crude oil, keeping the temperature at 45 ℃, adding 1.2% of water and 200ppm of PLC enzyme, fully mixing, then fully reacting for 2.5h, and centrifuging at 4500rpm for 10min to obtain the degumming oil, wherein the degumming effect is shown in Table 4.
3G enzymatic degumming: degumming was performed in the same manner as the PLC enzymatic method described above, except that the PLC enzyme was replaced with 3G enzyme, to obtain degummed oil, and the degumming results are shown in table 4.
Comparative example 3
Degumming by a traditional method: weighing 1Kg of strong aromatic peanut crude oil, maintaining the temperature at 45 deg.C, adding 1.2% of 10% saline solution and 50ppm of PLA1After fully mixing the enzyme and 0.04% citric acid, fully reacting for 2h, centrifuging at 4500rpm for 10min, separating oil and oil colloid to obtain degummed oil, and the degumming effect is shown in Table 4.
PLA1Degumming by an enzymatic method: weighing 1Kg of strong aromatic peanut crude oil, keeping the temperature at 45 ℃, adding 0.8% aqueous solution and 75ppm PLA1After fully mixing the enzyme and 0.04% citric acid, fully reacting for 3h, centrifuging at 4500rpm for 10min to obtain the degumming oil, and the degumming result is shown in Table 4.
TABLE 4 results of degumming on aromatic peanut oil with the conventional method and different enzyme preparations (centrifugation)
Figure BDA0003393831520000101
Example 4
Degumming by a PLC (programmable logic controller) enzyme method: weighing 1Kg of strong aromatic peanut crude oil, keeping the temperature at 40 ℃, adding 1% of water and 160ppm of PLC enzyme, fully mixing, fully reacting for 5 hours, and naturally settling for 7 days to obtain the degummed oil, wherein the degummed oil has the degummed effect shown in Table 5.
3G enzymatic degumming: degumming was performed in the same manner as the PLC enzymatic method described above, except that the PLC enzyme was replaced with 3G enzyme, to obtain degummed oil, and the degumming results are shown in table 5.
Comparative example 4
Degumming by a traditional method: weighing 1Kg of strong aromatic peanut crude oil, keeping the temperature at 40 ℃, adding 1% of saline solution with the concentration of 10% or adding 0.8% of aqueous solution, fully mixing, then fully reacting for 2 hours, naturally settling for 7 days, and separating oil from oil gum to obtain the degummed oil, wherein the degumming effect is shown in Table 5.
PLA1Degumming by an enzymatic method: weighing 1Kg of strong-flavor small crude oil of tuber mustard seed oil, keeping the temperature at 40 ℃, and 60ppm of PLA1After fully mixing the enzyme and 0.04% citric acid, fully reacting for 2 hours, and naturally settling for 7 days to obtain the degummed oil, wherein the degummed result is shown in a table 5.
TABLE 5 results of degumming on aromatic peanut oil with the conventional method and with different enzyme preparations (natural sedimentation method)
Figure BDA0003393831520000102
Example 5
Degumming by a PLC (programmable logic controller) enzyme method: weighing 1Kg of strong aromatic soybean crude oil, keeping the temperature at 50 ℃, adding 2% of water and 200ppm of PLC enzyme, fully mixing, then fully reacting for 2.5h, and centrifuging at 4500rpm for 10min to obtain the degumming oil, wherein the degumming effect is shown in Table 6.
3G enzymatic degumming: degumming was performed in the same manner as the PLC enzymatic method described above, except that the PLC enzyme was replaced with 3G enzyme, to obtain degummed oil, and the degumming results are shown in table 6.
Comparative example 5:
degumming by a traditional method: weighing 1Kg of strong aromatic soybean crude oil, keeping the temperature at 50 ℃, adding 0.8% of 10% salt solution, fully mixing, then fully reacting for 2.5h, and centrifuging at 4500rpm for 10min to obtain the degumming oil, wherein the degumming effect is shown in Table 6.
PLA1Degumming by an enzymatic method: weighing 1Kg of strong aromatic soybean crude oil, keeping the temperature at 50 ℃, and 70ppm of PLA1After fully mixing the enzyme and 0.04% citric acid, fully reacting for 2.5h, centrifuging at 4500rpm for 10min to obtain the degumming oil, and the degumming effect is shown in Table 6.
TABLE 6 results of degumming of conventional methods and different enzyme preparations on strong-flavor soybean oil (centrifugation)
Figure BDA0003393831520000111
The 3G enzyme is a conventional PLC enzyme, PI-PLC enzyme and PLA2Enzyme preparations comprising a mixture of enzymes. As shown in table 2 to table 6 above, the present inventors found that the oil yield of 3G enzymatic degumming and PLC enzymatic degumming is higher than that of conventional degumming and DA enzymatic degumming, and the oil yield of 3G enzymatic degumming is higher than that of PLC enzymatic degumming.
Examples of effects
The PLC enzyme-process degummed oil and the 3G enzyme-process degummed oil obtained in example 1, and the conventional-process degummed oil and PLA obtained in comparative example 11The enzymatic degummed oil was evaluated for flavor and stability as follows.
The flavor was evaluated as described below, followed by a shelf life test to follow the product quality and flavor profile, and the results are shown in tables 7-9 below.
Effect example 1 flavor evaluation
The flavor evaluation method comprises the following steps: and (3) performing flavor difference test on the enzyme-method degummed oil and the traditional degummed oil by adopting a sensory evaluation triangle test method, performing sample preparation according to an ABB AAB ABA BAA BBA BAB sequence, and randomly distributing the samples to not less than 24 evaluators to require the evaluators to select different samples. And counting the number of correct results, and performing significance difference analysis on the two samples according to the requirement of determining the minimum number of correct answers required by the significance difference by using a triangular test.
TABLE 7 Effect of different phospholipases on the flavour of Thick sesame oils
Figure BDA0003393831520000121
Note: the number of the people who answer the pair shows that people with flavor difference between the people can be accurately judged, and the more people who answer the pair, the more obvious the flavor difference between the people.
TABLE 8 flavor preference ranking of thick sesame oils made by degumming with different phospholipases
Classes of enzyme preparations By conventional means PLA1 PLC 3G
Score of 2.33 2.63 2.67 2.38
As can be seen from the data in tables 7 and 8, the flavor of the enzyme degummed oil is better than that of the conventional degummed oil, wherein the flavor of the PLC enzyme degummed oil is the best, and the PLA is1The second enzyme, the third 3G enzyme, the lowest score for flavor preference of the degummed oil by the traditional method.
Effect example 2 stability evaluation
Shelf life test: determining a test sample and a reference sample, making a sampling plan comprising a starting point, a test period and a preset test interval according to a test purpose, completing sampling according to the sampling plan, and evaluating the sample by adopting methods such as descriptive inspection, differential inspection and the like. In evaluating the shelf life test results, variations due to factors such as test interval design and storage condition differences should be taken into account.
TABLE 9 Effect of different degumming methods on the storage stability of aroma oils
Figure BDA0003393831520000122
Figure BDA0003393831520000131
The two indexes of peroxide value and acid value are main indexes for judging the stability of the grease, and the indexes of the two are unchanged or change the smaller the better in the long-term storage process of the grease product. As shown in table 9, the index changes of the degummed oil by the enzymatic method are not significantly different from the degummed oil (W) by the traditional method, and the change trends are consistent, which means that the enzymatic degumming technology has no negative influence on the quality of the aroma oil product.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition. In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (10)

1. A preparation method of a strong aromatic edible vegetable oil product comprises the following steps:
(1) weighing 0.8-1.2Kg of strong aromatic plant crude oil, and keeping the temperature at 25-60 ℃;
(2) adding 0.8-2.0 wt% of water and 50-200ppm of phospholipase used under neutral condition with pH of 6-8, and mixing thoroughly;
(3) and after mixing, fully reacting for 1-5h, and separating oil from oleogum through natural sedimentation or centrifugal separation to obtain the strong-flavor edible oil product.
2. An enzymatic degumming method of strong aromatic plant crude oil comprises the following steps:
(1) weighing 0.8-1.2Kg of strong aromatic plant crude oil, and keeping the temperature at 25-60 ℃;
(2) adding 0.8-2.0 wt% of water and 50-200ppm of phospholipase used under neutral condition with pH of 6-8, and mixing thoroughly;
(3) and after mixing, fully reacting for 1-5h, and separating oil from oil gum through natural sedimentation or centrifugal separation to realize degumming of the strong aromatic plant crude oil.
3. The method of claim 1 or 2, wherein in step (1), the phospholipase is phospholipase C or a mixture thereof;
preferably, the phospholipase is
Figure FDA0003393831510000011
PLC enzymes and/or
Figure FDA0003393831510000012
A 3G enzyme;
preferably, the strong aromatic vegetable crude oil is selected from one or more of strong aromatic rapeseed oil, strong aromatic soybean oil, strong aromatic sunflower oil, strong aromatic peanut oil and strong aromatic corn oil.
4. The method according to any one of claims 1 to 3, wherein in step (1), 1 to 1.2Kg of said aromatic crude plant oil is weighed, and said temperature is maintained at 25 to 30 ℃.
5. The method as claimed in claim 3 or 4, wherein in step (2), 0.8-1.0% of water and 150-200ppm of water are added
Figure FDA0003393831510000013
PLC enzymes and/or
Figure FDA0003393831510000014
The 3G enzyme was mixed well.
6. The method according to any one of claims 1 to 5, wherein in the step (3), the mixture is allowed to react for 1 to 5 hours after mixing, and then the natural sedimentation or centrifugal separation is performed.
7. The method of any one of claims 1-6, wherein in step (3), the natural settling is performed for 1-7 days.
8. The method according to any one of claims 3-7, comprising the steps of:
(1) weighing 1Kg of strong aromatic plant crude oil, and keeping the temperature at 30 ℃;
(2) adding 0.8 wt% of water and 200ppm of
Figure FDA0003393831510000021
PLC enzymesAnd/or
Figure FDA0003393831510000022
Fully mixing the 3G enzyme;
(3) after mixing, the mixture reacts for 2 hours, and the oil colloid are separated by natural sedimentation for 7 days.
9. Use of a phospholipase used at a pH of 6-8 neutral conditions in the preparation of a Luzhou flavor edible vegetable oil product and/or in enzymatic degumming of Luzhou flavor crude vegetable oil.
10. The use of claim 9, wherein the phospholipase is a phospholipase
Figure FDA0003393831510000023
PLC enzymes and/or
Figure FDA0003393831510000024
3G enzyme.
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