CN103074153A - Method for leaching vegetable oil by vegetable oil materials through protease enzymolysis - Google Patents

Abstract

The invention discloses a method for leaching vegetable oil by vegetable oil materials through protease enzymolysis. The method comprises the steps that a vegetable oil material is dried to be with a moisture content lower than 15% and/or squeezed by an oil press to prepare oil, the vegetable oil material is smashed and subjected to 20 to 40 meshes, oil particles are obtained, a protease water solution with the pH ranging from 6.5 to 7.5 is added to the oil particles and is stirred uniformly, the mixture has an enzymolysis reaction for 8 hours to 16 hours at a temperature ranging from 30 DEG C to 45 DEG C, oil after the enzymolysis reaction is dried to be with a moisture content lower than 10% at a temperature of 100 DEG C, No. 6 extraction solvent oil is used to leach vegetable oil. The method is based on a technology of vegetable oil material cold squeezing to prepare oil, squeezed oil protein is subjected to protease enzymolysis, and protein of the vegetable oil materials with an oil content being lower than 20% is directly subjected to protease enzymolysis, so that the oil can meet requirements of oil leaching extraction methods without being subjected to high-temperature steaming and frying, the benzopyrene content of the leached vegetable oil is within 2mcg/L, and edible safety of the vegetable oil is improved greatly.

Description

A kind of method of protease enzymatic hydrolysis vegetable oil material leaching vegetable oil

(1) Technical field

The invention relates to a method for extracting vegetable oil, in particular to a method for enzymatically hydrolyzing vegetable oil material with protease to extract vegetable oil.

(2) Background technology

At present, there are two large-scale industrial methods used in the production of vegetable oil at home and abroad, one is the mechanical pressing method, and the other is the solvent leaching method. For vegetable oils with higher oil content, such as rapeseed and camellia oleifera, the method of pressing first and then leaching is also used. In order to improve the yield of vegetable oil, all kinds of oil production methods need to steam and fry vegetable oil at high temperature until the oil protein is highly denatured. As the oil is steamed and fried at high temperature until the protein is highly denatured, a strong carcinogen benzopyrene will be produced. No matter the vegetable oil obtained by the pressing method or the leaching method contains a certain amount of benzopyrene, especially the oil obtained by the solvent leaching method, benzopyrene The pyrene content is significantly higher than that of pressed oil, which has a serious impact on food safety. Already countries and organizations in the world have limited the content of benzopyrene in edible vegetable oil to within 2 micrograms per liter (the current national standard in my country is within 10 micrograms per liter). can not achieve. Instead of steaming and frying the vegetable oil at high temperature until the protein is highly denatured, according to the technology of the current oil production method, the content of benzopyrene in the edible oil can be controlled within 2 micrograms per liter, but the oil extraction rate will be significantly reduced, which is a waste of vegetable oil resources.

(3) Contents of the invention

The purpose of the present invention is to provide a method for protease enzymatic hydrolysis of vegetable oil to extract vegetable oil, that is, the method of protease enzymolysis of vegetable oil and then solvent leaching. The method of the present invention reduces the content of strong carcinogen benzopyrene in edible vegetable oil to achieve low At the same time, the oil extraction rate of vegetable oils is guaranteed, so that the residual oil content of vegetable oils after oil extraction is within 1.0%. It is of great significance to improve the food safety of edible vegetable oil and ensure the utilization efficiency of vegetable oil.

The technical scheme adopted in the present invention is:

The invention provides a method for leaching vegetable oil from vegetable oil with protease enzymolysis. The method comprises: drying vegetable oil with an oil content of less than 20% until the water content is less than 15%, pulverizing, and passing through a 20-40 mesh sieve to obtain oil granules a, then add the protease aqueous solution a with a pH value of 6.5~7.5 into the oil granule a, stir evenly, and perform the enzymatic hydrolysis reaction at 30~45°C for 8~16h (preferably 12h at 40°C). The oil is dried at 100°C until the moisture content is less than 10%, and then the vegetable oil a is extracted with No. 6 extraction solvent oil; the amount of protease in the protease aqueous solution a is 100~200U/g oil particle a based on the enzyme activity of the protease.

The main components of the No. 6 extraction solvent oil are 74% of n-hexane (C ₆ H ₁₄ ) and 16% of cyclohexane (C ₆ H ₁₂ ).

Further, the protease in the protease aqueous solution a is a protease with an optimum pH value of 6.0-8.0 for enzymolysis reaction.

Further, the vegetable oil with an oil content lower than 20% is soybean or rice bran.

Further, the method of extracting vegetable oil a with No. 6 extraction solvent oil is as follows: dry the oil after the enzymatic hydrolysis reaction at 100°C until the water content is less than 10%, then add it to a horizontal rotary extractor, and use No. 6 extraction solvent The oil is extracted at 45-50°C to obtain vegetable oil a.

The present invention also provides another method for protease enzymatic hydrolysis of vegetable oils to extract vegetable oils. The method is: drying vegetable oils with an oil content of more than 20% until the water content is less than 15%, and then drying the oil in the oil press chamber at a temperature of less than 90 Under the condition of ℃ (preferably 78~88℃), use oil press to press oil to obtain oil cake and vegetable oil b, crush the oil cake, and pass through 20~40 mesh sieve to obtain oil plant particles b; Add to oil granules b, stir evenly, perform enzymatic hydrolysis at 30-45°C for 8-16 hours (preferably 12 hours at 40°C), dry the oil after enzymatic hydrolysis at 100°C until the water content is less than 10%, and then The vegetable oil c is leached with No. 6 extraction solvent oil; the amount of protease in the protease aqueous solution b is 100-200 U/g oil particle b based on the enzyme activity of the protease.

Further, the vegetable oil with an oil content above 20% is camellia seed, peanut, walnut or rapeseed.

Further, the oil press is used to press the oil under the condition that the temperature in the chamber of the oil press is 78-88°C, and the oil content of the oil cake after pressing is 10-19%.

Further, the protease in the protease aqueous solution b is a protease with an optimum pH value of 6.0-8.0 for the enzymatic hydrolysis reaction.

Further, the method for leaching vegetable oil c with No. 6 extraction solvent oil is as follows: dry the oil after the enzymolysis reaction at 100°C until the water content is less than 10%, then add it to a flat-rotary extractor, and use No. 6 extraction solvent The oil is extracted at 45-50°C to obtain vegetable oil c.

The appearance of No. 6 extraction solvent oil of the present invention is a colorless transparent liquid, which is a mixture of various lower alkanes. The product standard is GB 16629-96, and it is recommended to use Jiangsu Taizhou Kaiyuan Chemical Co., Ltd. to produce.

The protease aqueous solution a and the protease aqueous solution b of the present invention are all protease aqueous solutions, which are named for the convenience of distinguishing the different protease aqueous solutions used in different methods. The letters themselves have no meaning, and the protease aqueous solution is adjusted to pH with 1 mol/liter of NaOH or HCl .

The oil granule a and the oil granule b in the present invention are all oil granules pulverized in different steps, and are named for the convenience of distinguishing the different oil granules obtained by different methods, and the letters themselves have no meaning.

The vegetable oil a, vegetable oil b and vegetable oil c described in the present invention are all vegetable oils, which are named for the convenience of distinguishing the different amounts of vegetable oil obtained in different steps, and the letters themselves have no meaning.

The amount of residual oil after enzymolysis and leaching of the vegetable oil of the present invention is detected by the Soxhlet extraction method, and the content of benzopyrene in the oil is detected according to the method of the national standard GBT22509-2008. The Soxhlet extraction method was carried out according to the operation requirements stipulated in the national standard GB19644-2010.

Compared with the prior art, the beneficial effects of the present invention are mainly reflected in:

The present invention is based on the cold-pressed oil production technology of vegetable oils, enzymatically hydrolyzes the protein of the pressed oil with protease, or directly enzymatically hydrolyzes the protein of vegetable oils with an oil content below 20%, so that the oil can reach The requirements of oil extraction by leaching, and the existing equipment for leaching vegetable oil can be directly used. The benzopyrene content of the extracted vegetable oil is within 2 micrograms per liter, which greatly improves the edible safety of the vegetable oil. The economic value of the oil that has not been steamed and fried at high temperature is also improved after oil extraction.

(4) Specific implementation methods

The present invention is further described below in conjunction with specific embodiment, but protection scope of the present invention is not limited thereto:

Example 1:

Camellia oleifera seeds (produced in Quzhou City, Zhejiang Province) are sun-dried to a moisture content of 14.7% and an oil content of 31.5%. Take 500 kg at room temperature and use an oil press produced by Wuhan Grain and Agriculture Machinery Manufacturing Co., Ltd. to perform mechanical pressing to make oil (press once). %. Get 400 kilograms of tea seed cakes after oil extraction, mechanically pulverize, pass through a 40-mesh sieve, add a protease aqueous solution with a pH value of 7.0, the addition amount is 160 liters, and the protease (Xingtai Taihe Biochemical Technology Co., Ltd.) The content is 500 units/ml. After stirring evenly, enzymolysis reaction was carried out at 40° C. for 8 hours. Dry the enzymatically hydrolyzed oil at 100°C to a water content of 8.2%, then add it to a horizontal extractor (produced by Henan Mengzhou Chengde Oil Equipment Co., Ltd.), and use 360 liters of No. 6 to extract solvent oil (Jiangsu Taizhou (manufactured by Kaiyuan Chemical Co., Ltd.) was extracted at 45°C, and the oil after extraction was determined by Soxhlet extraction method, and the residual oil rate was 0.86%.

The same batch of Camellia oleifera seeds was squeezed and extracted 400 kg, and directly dried at 100°C to a water content of 8.3% without enzymatic hydrolysis by protease. Under the same conditions, the oil was leached with No. 6 extraction solvent oil, and the residual oil rate in the oil was 3.3%. The camellia oil produced by the two technical methods is tested according to the national standard GBT22509-2008 method, and the content of benzopyrene in the oil is 1.78 micrograms/liter and 1.84 micrograms/liter respectively.

Example 2:

Camellia oleifera seeds (produced in Quzhou City, Zhejiang Province) are baked at 90°C until the water content is 14.5% and the oil content is 30.6%. Get 500 kilograms and use the oil press machine produced by Wuhan Food and Agriculture Machinery Manufacturing Co., Ltd. to press at room temperature to make oil. The temperature in the chamber of the oil press is 86 ° C, and the oil content of the tea seed cake after pressing and extracting oil is 12.4%. Get 400 kilograms of tea seed cakes after oil extraction, mechanically pulverize, pass through a 20-mesh sieve, add a protease aqueous solution with a pH value of 7.5, and the addition amount is 80 liters, and the protease (Xingtai Taihe Biochemical Technology Co., Ltd.) The content is 500 units/ml. After stirring evenly, keep the enzymolysis reaction at 30°C for 16 hours. Dry the enzymatically hydrolyzed oil at 100°C to a water content of 8.5%, add it to a horizontal extractor (produced by Henan Mengzhou Chengde Oil Equipment Co., Ltd.), and use 320 liters of No. 6 to extract solvent oil (Jiangsu Taizhou Kaiyuan Chemical Co., Ltd. Co., Ltd.) extracted at 50 ° C, the extracted oil was determined by Soxhlet extraction method, and the residual oil rate was 0.93%.

The same batch of Camellia oleifera seeds was squeezed and 400 kg was taken after extracting oil, and directly dried at 100°C to a water content of 8.6% without enzymatic hydrolysis by protease. Under the same conditions, No. 6 extraction solvent oil was used to extract the oil, and the residual oil rate in the oil was 3.2%. . The camellia oil produced by the two technical methods is tested according to the national standard GBT22509-2008 method, and the content of benzopyrene in the oil is 1.76 micrograms/liter and 1.85 micrograms/liter respectively.

Example 3:

Camellia oleifera seeds (produced in Quzhou City, Zhejiang Province) are sun-dried to a moisture content of 14.8% and an oil content of 31.2%. Get 500 kilograms and use the oil press machine produced by Wuhan Grain and Agriculture Machinery Manufacturing Co., Ltd. to press at room temperature to make oil. The temperature in the chamber of the oil press is 88 ° C, and the oil content of the tea seed cake after pressing and extracting oil is 13.1%. Get 400 kilograms of tea seed cakes after oil extraction, mechanically pulverize, pass through a 30-mesh sieve, add a protease aqueous solution with a pH value of 6.5, and the addition amount is 120 liters, and the protease (Xingtai Taihe Biochemical Technology Co., Ltd.) The content is 500 units/ml. After stirring evenly, keep the enzymolysis reaction at 45°C for 12 hours. Dry the enzymatically hydrolyzed oil at 100°C to a water content of 8.7%, add it to a horizontal extractor (produced by Henan Mengzhou Chengde Oil Equipment Co., Ltd.) and use 400 liters of No. 6 solvent oil (Jiangsu Taizhou Kaiyuan Chemical Co., Ltd. produced by the company) at 40°C. After leaching, the oil was determined by Soxhlet extraction method, and the residual oil rate was 0.85%.

The same batch of Camellia oleifera seeds was squeezed to extract 400 kg of oil, directly dried at 100°C to a water content of 8.6% without enzymatic hydrolysis by protease, and extracted under the same conditions to make oil, the residual oil rate in the oil was 3.5%. The camellia oil produced by the two technical methods is tested according to the national standard GBT22509-2008 method, and the content of benzopyrene in the oil is 1.72 micrograms/liter and 1.81 micrograms/liter respectively.

Example 4:

Rapeseed (produced in Huzhou City, Zhejiang Province) is sun-dried to a moisture content of 14.8% and an oil content of 38.5%. Take 600 kilograms and use the oil press machine produced by Wuhan Grain and Agriculture Machinery Manufacturing Co., Ltd. to press at room temperature to make oil. The temperature in the chamber of the oil press is 87 ° C, and the oil content of the rapeseed cake after pressing and extracting oil is 16.2%. Take 400 kg of rapeseed cake after oil extraction, mechanically pulverize, pass through a 30-mesh sieve, add a protease aqueous solution with a pH value of 7.0, the addition amount is 120 liters, and the protease (Xingtai Taihe Biochemical Technology Co., Ltd.) The content is 500 units/ml. After stirring evenly, keep the enzymolysis reaction at 40°C for 12 hours. Dry the enzymatically hydrolyzed oil at 100°C to a water content of 8.6%, add it to a horizontal extractor (produced by Henan Mengzhou Chengde Oil Equipment Co., Ltd.) and use 440 liters of No. 6 solvent oil (Jiangsu Taizhou Kaiyuan Chemical Co., Ltd. produced by the company) at 45°C. The extracted oil was determined by Soxhlet extraction method, and the residual oil rate was 0.91%.

400 kg of the same batch of rapeseeds were squeezed and extracted, and directly dried at 100°C to a water content of 8.8% without enzymatic hydrolysis by protease. The oil was leached under the same conditions, and the residual oil rate in the oil was 4.7%. The rapeseed oil prepared by the two technical methods is tested according to the national standard GBT22509-2008 method, and the content of benzopyrene in the oil is 1.83 μg/L and 1.80 μg/L respectively.

Example 5:

Rapeseed (produced in Huzhou City, Zhejiang Province) is baked at 90°C until the moisture content is 14.6% and the oil content is 38.7%. Take 600 kilograms and use the oil press machine produced by Wuhan Grain and Agriculture Machinery Manufacturing Co., Ltd. to press at room temperature to make oil. The temperature in the chamber of the oil press is 86 ° C, and the oil content of the rapeseed cake after pressing and extracting oil is 16.3%. Take 400 kg of rapeseed cake after oil extraction, mechanically crush, pass through a 40-mesh sieve, add a protease aqueous solution with a pH value of 7.5, the addition amount is 130 liters, the protease (Xingtai Taihe Biochemical Technology Co., Ltd.) in the protease aqueous solution The content is 500 units/ml. After stirring evenly, keep the enzymolysis reaction at 45°C for 11 hours. Dry the enzymatically hydrolyzed oil at 100°C to a water content of 8.4%, add it to a horizontal extractor (produced by Henan Mengzhou Chengde Oil Equipment Co., Ltd.) and use 400 liters of No. 6 solvent oil (Jiangsu Taizhou Kaiyuan Chemical Co., Ltd. produced by the company) at 50°C. After leaching, the oil was determined by Soxhlet extraction method, and the residual oil rate was 0.94%.

The same batch of rapeseeds was pressed and extracted with 400 kg of oil, and directly dried at 100°C to a water content of 8.5% without enzymatic hydrolysis by protease. Under the same conditions, No. 6 extraction solvent oil was used to extract the oil, and the residual oil rate in the oil was 4.8%. The rapeseed oil prepared by the two technical methods is tested according to the national standard GBT22509-2008 method, and the content of benzopyrene in the oil is 1.85 micrograms/liter and 1.83 micrograms/liter respectively.

Example 6:

Soybean (produced in Jilin City, Jilin Province) has a moisture content of 13.6% and an oil content of 17.5%. Take 400 kg, mechanically crush through a 40-mesh sieve, add a protease aqueous solution with a pH value of 7.0, the addition amount is 120 liters, and the content of protease (Xingtai Taihe Biochemical Technology Co., Ltd.) in the aqueous solution is 500 units/ml. After stirring evenly, keep the enzymolysis reaction at 45°C for 12 hours. Dry the enzymatically hydrolyzed oil at 100°C to a water content of 8.7%, add it to a horizontal extractor (produced by Henan Mengzhou Chengde Oil Equipment Co., Ltd.) and use 400 liters of No. 6 solvent oil (Jiangsu Taizhou Kaiyuan Chemical Co., Ltd. produced by the company) at 40°C. After leaching, the oil was determined by Soxhlet extraction method, and the residual oil rate was 0.93%.

Take 400 kg of the same batch of soybeans, without enzymatic hydrolysis by protease, and directly dry them at 100°C to a water content of 8.6%. Under the same conditions, No. 6 extraction solvent oil is used to extract oil, and the residual oil rate in the oil is 4.2%. The soybean oil prepared by the two technical methods was tested according to the national standard GBT22509-2008 method, and the content of benzopyrene in the oil was 1.75 micrograms/liter and 1.83 micrograms/liter respectively.

Claims (9)

1. the method for a protease hydrolyzed vegetable oil material extracted plant oil, it is characterized in that described method is: oleaginousness is lower than 20% vegetable oil material and is dried to moisture content less than 15%, pulverize, cross 20 ~ 40 mesh sieves, obtain oil plant particle a, then the aqueous solution of protease a with pH value 6.5 ~ 7.5 adds among the oil plant particle a, stir, at 30 ~ 45 ℃ of lower enzyme digestion reaction 8 ~ 16h, oil plant behind the enzyme digestion reaction is dried to moisture content less than 10% at 100 ℃, then uses soybean extracting solvent no.6 extracted plant oil a; The consumption of proteolytic enzyme is take the enzyme work of proteolytic enzyme as 100-200U/g oil plant particle a among the described aqueous solution of protease a.

2. the method for protease hydrolyzed vegetable oil material extracted plant oil as claimed in claim 1 is characterized in that proteolytic enzyme is that the peak enzymolysis-ability pH value in reaction is 6.0 ~ 8.0 proteolytic enzyme among the described aqueous solution of protease a.

3. the method for protease hydrolyzed vegetable oil material extracted plant oil as claimed in claim 1 is characterized in that it is soybean or rice bran that described oleaginousness is lower than 20% vegetable oil material.

4. the method for protease hydrolyzed vegetable oil material extracted plant oil as claimed in claim 1, it is characterized in that described method with soybean extracting solvent no.6 extracted plant oil a is: with the oil plant behind the enzyme digestion reaction 100 ℃ be dried to moisture content less than 10% rear adding flat rotary extractor in, 45 ~ 50 ℃ of lixiviates, obtain vegetables oil a with soybean extracting solvent no.6.

5. the method for a protease hydrolyzed vegetable oil material extracted plant oil, it is characterized in that described method is: oleaginousness is dried to moisture content less than 15% at the vegetable oil material more than 20%, then temperature is squeezed liquefaction less than employing oil press zhai under 90 ℃ of conditions in the oil press zhai thorax, obtain oil cake and vegetables oil b, oil cake is pulverized, cross 20 ~ 40 mesh sieves, obtain oil plant particle b; The aqueous solution of protease b of pH value 6.5 ~ 7.5 is added among the oil plant particle b, stir, at 30 ~ 45 ℃ of lower enzyme digestion reaction 8 ~ 16h, the oil plant behind the enzyme digestion reaction is dried to moisture content less than 10% at 100 ℃, use again soybean extracting solvent no.6 extracted plant oil c; The consumption of proteolytic enzyme is take the enzyme work of proteolytic enzyme as 100 ~ 200U/g oil plant particle b among the described aqueous solution of protease b.

6. the method for protease hydrolyzed vegetable oil material extracted plant oil as claimed in claim 5 is characterized in that described oleaginousness is tea seed, peanut, walnut or Semen Brassicae campestris at the vegetable oil material more than 20%.

7. the method for protease hydrolyzed vegetable oil material extracted plant oil as claimed in claim 5 is characterized in that adopting oil press zhai squeezing liquefaction in the described oil press zhai thorax under 78 ~ 88 ℃ of conditions of temperature, and the oil cake oleaginousness is 10 ~ 19% after the squeezing.

8. the method for protease hydrolyzed vegetable oil material extracted plant oil as claimed in claim 5 is characterized in that proteolytic enzyme is the proteolytic enzyme of peak enzymolysis-ability pH value in reaction 6.0 ~ 8.0 among the described aqueous solution of protease b.

9. the method for protease hydrolyzed vegetable oil material extracted plant oil as claimed in claim 5, it is characterized in that described method with soybean extracting solvent no.6 extracted plant oil c is: with the oil plant behind the enzyme digestion reaction 100 ℃ be dried to moisture content less than 10% rear adding flat rotary extractor in, 45 ~ 50 ℃ of lixiviates, obtain vegetables oil c with soybean extracting solvent no.6.