阅读说明：本技术 一种水溶性好耐高温磷脂的生产方法 (Production method of phospholipid with good water solubility and high temperature resistance ) 是由 吕鹏姗 王彦 葛萌 段妍聪 于 2020-07-22 设计创作，主要内容包括：本发明公开了一种水溶性好耐高温磷脂的生产方法,包括以下步骤：S1,粗磷脂,升温；S2,与乳酸溶液混合,控制温度,搅拌；S3,在一定时间内,与双氧水混合,升温,搅拌；S4,在一定时间内,与氢氧化钠水溶液,控制温度,搅拌；S5,调节温度,加入磷脂酶,反应一段时间；S6,抽真空脱水,得到改性的磷脂。本发明的水溶性好耐高温磷脂的生产方法,先羟基化,后酶解,对磷脂进行改性,以期获得水溶性好耐高温的改性磷脂。对磷脂的羟基化中,以乳酸为催化剂,催化磷脂与双氧水反应,以氢氧化钠中和反应。酶解中,添加磷脂酶A2,对羟基改性的磷脂进行酶解,进一步改性,最终得到的改性磷脂是水溶性和耐高温性能优良。(The invention discloses a production method of phospholipid with good water solubility and high temperature resistance, which comprises the following steps: s1, heating crude phospholipid; s2, mixing the lactic acid solution with the mixture, controlling the temperature and stirring the mixture; s3, mixing with hydrogen peroxide in a certain time, heating and stirring; s4, mixing with sodium hydroxide water solution in a certain time, controlling the temperature and stirring; s5, adjusting the temperature, adding phospholipase, and reacting for a period of time; and S6, vacuumizing and dehydrating to obtain the modified phospholipid. The production method of the phospholipid with good water solubility and high temperature resistance firstly hydroxylates and then carries out enzymolysis to modify the phospholipid so as to obtain the modified phospholipid with good water solubility and high temperature resistance. In hydroxylation of phospholipid, lactic acid is used as a catalyst to catalyze the reaction of phospholipid and hydrogen peroxide, and sodium hydroxide is used for neutralization reaction. In the enzymolysis, phospholipase A2 is added to carry out enzymolysis on the hydroxyl modified phospholipid for further modification, and the finally obtained modified phospholipid has excellent water solubility and high temperature resistance.)

1. A production method of phospholipid with good water solubility and high temperature resistance comprises the following steps:

s1, heating crude phospholipid;

s2, mixing the lactic acid solution with the mixture, controlling the temperature and stirring the mixture;

s3, mixing with hydrogen peroxide in a certain time, heating and stirring;

s4, mixing with sodium hydroxide water solution in a certain time, controlling the temperature and stirring;

s5, adjusting the temperature, adding phospholipase, and reacting for a period of time;

and S6, vacuumizing and dehydrating to obtain the modified phospholipid.

2. The method according to claim 1, wherein the temperature is increased to 50-60 ℃ in the step of S1.

3. The method according to claim 1 or 2, wherein in the step of S2, the temperature is controlled to be 50-60 ℃, and stirring is performed for 1.5-2.5 h;

and/or, in the step S2, the lactic acid solution is 3-4% by weight of the crude phospholipid, and the concentration of the lactic acid solution is 30% by weight.

4. The method according to any one of claims 1 to 3, wherein in the step S3, the mixture is mixed with hydrogen peroxide within more than 30min, the temperature is raised to 68-72 ℃, and the mixture is stirred for 3.5-4.5 h;

and/or in the step S3, hydrogen peroxide accounts for 8-10% of the crude phospholipid by weight, and the concentration of the hydrogen peroxide by weight is 35%.

5. The method according to any one of claims 1 to 4, wherein in the step S4, the mixture is mixed with the sodium hydroxide aqueous solution for more than 30min, the temperature is controlled between 68 ℃ and 72 ℃, and the mixture is stirred for 4.5 to 5.5 hours;

and/or, in the step S4, the weight percentage of the sodium hydroxide is 3-5% of that of the crude phospholipid, and the weight percentage of the sodium hydroxide solution is 32%.

6. The method according to any one of claims 1 to 5, wherein in the step of S5, the temperature is adjusted to 56 to 60 ℃, phospholipase A2 is added, and the mixture is stirred and reacted for 9 to 11 hours;

and/or, in the step of S5, the phospholipase is added in an amount of 0.02-0.04% by weight based on the crude phospholipid.

7. The method according to any one of claims 1 to 6, wherein in the step S6, the temperature during vacuum dehydration is less than 80 ℃ and the dehydration is carried out until the moisture is less than or equal to 1.5%.

8. The method of any one of claims 1-7, further comprising the step of adding EDTA-Ca and a modified phospholipid prior to the step of S5.

9. The method according to any one of claims 1 to 8, wherein the concentration of EDTA-Ca added to the system is 0.5 to 5 mmol/L.

10. The method according to any one of claims 1 to 9, wherein the modified phospholipid is added in an amount of 0.1 to 1% by weight based on the crude phospholipid.

Technical Field

The invention belongs to the technical field of phospholipid processing, and relates to a production method of phospholipid with good water solubility and high temperature resistance.

Background

Phospholipids (phospholipids), also known as phospholipids or phospholipids, are lipids containing phosphoric acid and belong to complex lipids. Phospholipids are amphiphilic molecules with a hydrophilic nitrogen or phosphorus containing head at one end and a long hydrophobic (lipophilic) hydrocarbyl chain at the other end. Phospholipids are widely used in the feed industry, food industry, pharmaceutical and health products, cosmetics industry, textile industry, leather industry.

Natural phospholipid is easy to darken at high temperature, cannot resist high temperature and is generally insoluble in water. This severely limits the use of phospholipids in aqueous, high temperature processing processes. Modification of natural phospholipids is an important direction of research in phospholipid processing.

Disclosure of Invention

Aiming at the problems, the invention provides a production method of phospholipid with good water solubility and high temperature resistance, which comprises the steps of hydroxylating crude phospholipid and then carrying out enzymolysis, wherein the obtained phospholipid can be well dissolved in water, and the color value is not changed at high temperature. So that the modified phospholipid can be widely applied to aqueous solution and high-temperature processing technology.

The invention discloses a production method of phospholipid with good water solubility and high temperature resistance, which comprises the following steps:

s1, heating crude phospholipid;

s2, mixing the lactic acid solution with the mixture, controlling the temperature and stirring the mixture;

s3, mixing with hydrogen peroxide in a certain time, heating and stirring;

s4, mixing with sodium hydroxide water solution in a certain time, controlling the temperature and stirring;

s5, adjusting the temperature, adding phospholipase A2, and reacting for a period of time;

and S6, vacuumizing and dehydrating to obtain the modified phospholipid.

The production method of the phospholipid with good water solubility and high temperature resistance adopts a method of firstly hydroxylating and then carrying out enzymolysis to modify the phospholipid so as to obtain the modified phospholipid with good water solubility and high temperature resistance. In hydroxylation of phospholipid, lactic acid is used as a catalyst to catalyze the reaction of phospholipid and hydrogen peroxide, and sodium hydroxide is used for neutralization reaction. In the enzymolysis, phospholipase A2 is added to carry out enzymolysis on the hydroxyl modified phospholipid for further modification, and the finally obtained modified phospholipid has excellent water solubility and high temperature resistance.

In some embodiments of the invention, the temperature is raised to 50-60 ℃ in step S1.

In some embodiments of the present invention, in the step of S2, the temperature is controlled to be 50 to 60 ℃, and the stirring is performed for 1.5 to 2.5 hours.

In some embodiments of the present invention, in the S2 step, the lactic acid is 3-4% by weight of the crude phospholipid, and the lactic acid solution has a concentration of 30% by weight.

In some embodiments of the invention, in the step S3, the mixture is mixed with hydrogen peroxide for more than 30min, the temperature is raised to 68-72 ℃, and the mixture is stirred for 3.5-4.5 h.

In some embodiments of the present invention, in the step S3, the hydrogen peroxide is 8-10% by weight of the crude phospholipid, and the concentration of the hydrogen peroxide is 35% by weight.

In some embodiments of the present invention, in the step of S4, the mixture is mixed with the aqueous solution of sodium hydroxide for more than 30min, the temperature is controlled between 68 ℃ and 72 ℃, and the mixture is stirred for 4.5 to 5.5 h.

In some embodiments of the present invention, in the step of S4, the sodium hydroxide is 3-5% by weight of the crude phospholipid, and the sodium hydroxide solution has a concentration of 32% by weight.

In some embodiments of the present invention, in the step of S5, the temperature is adjusted to 56-60 ℃, phospholipase A2 is added, and the mixture is stirred and reacted for 9-11 h.

In some embodiments of the present invention, in the S5 step, the phospholipase is added in an amount of 0.02 to 0.04% by weight based on the crude phospholipid.

In some embodiments of the present invention, in the step of S6, the temperature during the vacuum dehydration is less than 80 ℃ and the dehydration is carried out until the moisture is less than or equal to 1.5%.

In some embodiments of the present invention, before the step of S5, a step of adding EDTA-Ca and modified phospholipids is further included.

Phospholipase A2 is a key factor in enzymatic hydrolysis. Ca²⁺And Mg²⁺The enzyme activity of phospholipase A2 can be improved, and EDTA can reduce the enzyme activity of phospholipase A2. When EDTA-Ca and modified phospholipid are added into the enzymolysis step, the surprising discovery shows that the enzymolysis time can be greatly shortened. Meanwhile, the effect is greatly improved by the treatment of the EDTA-Ca and the phospholipid obtained by modification, and the effect is synergisticAnd (5) acting together.

In some preferred embodiments of the present invention, the concentration of EDTA-Ca added to the system is 0.5 to 5 mmol/L.

In some preferred embodiments of the present invention, the modified phospholipid is added in an amount of 0.1 to 1% by weight based on the crude phospholipid.

When the concentration of EDTA-Ca in the system is 0.5-5mmol/L, the added modified phospholipid is 0.1-1% of the crude phospholipid by weight, the effect of EDTA-Ca and the modified phospholipid for shortening the enzymolysis time is obvious, and when the concentration of EDTA-Ca in the system is less than 0.1mmol/L or the added modified phospholipid is less than 0.05% of the crude phospholipid, the effect of shortening the enzymolysis time is not obvious.

In some preferred embodiments of the present invention, in step S5, the portion of the phospholipase may be controlled by the reaction rate, which comprises the following steps:

step a1, the reaction rate is determined according to the following equation:

wherein R represents the heating rate, T represents the reaction temperature, the molecular diameter of the phospholipase d, M represents the rate constant, and V represents the reaction rate obtained by solving;

and A2, according to the reaction rate V obtained in the step A1, reducing the amount of the phospholipase when the reaction rate V is greater than a preset threshold, and increasing the amount of the phospholipase when the reaction rate V is less than the preset threshold.

The beneficial technical effects of the invention are as follows:

the production method of the phospholipid with good water solubility and high temperature resistance firstly hydroxylates and then carries out enzymolysis to modify the phospholipid so as to obtain the modified phospholipid with good water solubility and high temperature resistance. In hydroxylation of phospholipid, lactic acid is used as a catalyst to catalyze the reaction of phospholipid and hydrogen peroxide, and sodium hydroxide is used for neutralization reaction. In the enzymolysis, phospholipase A2 is added to carry out enzymolysis on the hydroxyl modified phospholipid for further modification, and the finally obtained modified phospholipid has excellent water solubility and high temperature resistance.

According to the production method of the phospholipid with good water solubility and high temperature resistance, EDTA-Ca and the modified phospholipid are added, so that the enzymolysis time can be obviously shortened.

Detailed Description

The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.

The following examples and comparative examples are parallel runs, with the same processing steps and parameters, unless otherwise indicated. The weight percentage concentration of the lactic acid solution is 30%, the weight percentage concentration of the hydrogen peroxide is 35%, and the weight percentage concentration of the sodium hydroxide solution is 32%. The crude phospholipid is oil residue separated in the soybean oil refining process or edible soybean phospholipid, and is obtained by dehydration, decolorization and impurity removal steps, wherein the content of acetone insoluble phospholipid is about 60% by weight, and the content of triglyceride and free fatty acid is about 40% by weight. The product obtained was a viscous liquid product except that in example 5, the product was defatted to a solid powder with acetone. The enzyme activity of the phospholipase A2 is 12000U/ml.