CN104004105A - Preparation method of amylose soybean lecithin inclusion complex - Google Patents
Preparation method of amylose soybean lecithin inclusion complex Download PDFInfo
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Abstract
The invention discloses a preparation method of an amylose soybean lecithin inclusion complex. The method comprises the following steps: firstly performing enzymatic hydrolysis of a starch raw material to prepare an amylose solution; adjusting the temperature of the amylose solution to 30-80 DEG C, dropwise adding a soybean lecithin tetrahydrofuran solution with a soybean lecithin mass percent of 20-30%, performing heat insulation and stirring for reacting for 1-4 hours, wherein 0.4-0.6 g of the soybean lecithin tetrahydrofuran solution is added into each gram of dry starch; cooling to room temperature, performing refrigeration in a refrigerator at 4-10 DEG C for 18-36 hours; and performing centrifugation, washing, drying, and crushing to obtain a light yellow powdery product. The product of the invention has good stability; the method of the invention overcomes the disadvantages of liability to moisture absorption and oxidation of soybean lecithin, and has important value on improving the using characteristics of soybean lecithin and enlarging the application scope of soybean lecithin.
Description
Technical field
The present invention relates to the production method of modified starch, specifically refer to that utilizing biotechnology and chemical process to combine prepares the method for amylose starch soybean lecithin inclusion compound.
Background technology
Soybean lecithin (claiming again phosphatidylcholine) is the byproduct in refined soybean oil process, is a kind of lipoid cpd with important physiological function.It is one of important component of biomass cells, has the tissue of enhancing and cellularstructure, strengthens cell information transfer capacity, improves brain vigor, and improves the effects such as metabolism of fat.Can play human body and delay senility, regulate blood fat, reduce cholesterol, strengthen the health-care effects such as brain increased functionality memory.Soybean lecithin has been used in plurality kinds of health care product as health-care components.Soybean lecithin or a kind of very good natural cosmetics raw material, regulating the important roles such as body cell metabolism and cell membrane permeability, it has good moisture retention and perviousness to human body skin, can play moistening, emulsification, dispersion, moisturizing, the several functions such as anti-oxidant, antistatic.Soybean lecithin is also widely used in foodstuffs industry as a kind of natural emulsifying agent and antioxidant.In addition, soybean lecithin is also widely used in the industries such as paint, coatings industry, petrochemical complex, textiles, leather, rubber, plastics.
But; natural soybean lecithin is because containing a large amount of unsaturated fatty acidss, phosphatidyl in molecule; be subject to the impact such as temperature, moisture, thereby make soybean lecithin there is the easy moisture absorption, the shortcoming such as perishable, its application in industry is limited by very large.
Summary of the invention
The object of the invention is to prepare the amylose starch soybean lecithin inclusion compound of the low good stability of a kind of production cost, to improve service performance and the range of application of soybean lecithin.
Amylose starch is the straight chain molecule being formed by connecting by α-Isosorbide-5-Nitrae glycosidic link by D-glucopyranose units.Under proper condition, amylose molecule can with inorganic or organic molecular complex, form spirrillum Inclusion Complexes.The formation of Inclusion Complexes has great importance for the service performance aspect (as improved stability, controlling release) of improving guest molecule.At present domestic is raw material to the amylose starch of preparing taking enzyme process, and itself and the report of soybean lecithin complexing formation amylose starch soybean lecithin Inclusion Complexes be yet there are no.Amylose starch iron Inclusion Complexes prepared by the present invention, soybean lecithin inclusion is in the spiraled cavity of amylose starch, and the combination of soybean lecithin and amylose starch is tightr.
Object of the present invention is achieved through the following technical solutions:
The preparation method of amylose starch soybean lecithin inclusion compound, comprises the steps:
(1) starch material (50g, butt) to be made into mass percent concentration with Sodium phosphate dibasic-sodium dihydrogen phosphate buffer be 5%～12% starch milk, and regulate pH to 4.5～6.5, be placed in encloses container and at 95～99 DEG C, stir gelatinization 30～60min; After gelatinization completes, dextrin is cooling, add debranching factor, consumption is that every gram of dry starch adds debranching factor 10～30u, stirring reaction 1～3 hour at 45～65 DEG C; Regulate pH to 5.5～7.0, add α-amylase, consumption is every gram of dry starch 1～10u, and stirring reaction 1～10 minute at 45～110 DEG C regulates pH to 2.5～3.0 and keeps 10～15 minutes enzymes that go out, and obtains amylose starch solution;
(2) temperature of step (1) gained amylose starch solution is adjusted to 30～80 DEG C, dripping and being dissolved with mass percent is 20%～30% soybean lecithin tetrahydrofuran solution, insulated and stirred reaction 1～4 hour; Be cooled to after room temperature, put into 4～10 DEG C of refrigerator and cooled and hide 18～36 hours; Every gram of dry starch adds soybean lecithin tetrahydrofuran solution (0.4～0.6) g;
(3), by centrifugal the product of step (2), washing, obtains pale yellow powder shape product after dry, pulverize.
In order better to realize the present invention, the described starch material of step (1) is the one in waxy corn starch, Waxy wheat starch, tapioca (flour), W-Gum, yam starch and wheat starch.The described debranching factor of step (1) is Pullulanase or isoamylase.The described α-amylase of step (1) is middle temperature or high temperature resistant α-amylase.The described washing of step (3) is for repeatedly centrifugal with deionized water wash, until noresidue tetrahydrofuran (THF) in solution.
Compared with prior art, tool has the following advantages and beneficial effect in the present invention:
(1) adopt biological enzymolysis technology to carry out modification to starch material, obtain having the amylose starch of good inclusion complexation function, be applied to inclusion complexation soybean lecithin; After measured find, starch after enzymolysis processing, the amylose starch soybean lecithin inclusion compound preparing, in every gram of inclusion compound, the content of soybean lecithin can reach 106 milligrams, and mostly Yelkin TTS stability improve.
(2) to have production efficiency high in the present invention, and cost is low, the feature of good product quality.
Brief description of the drawings
Fig. 1 is the infared spectrum of inclusion retrogradation potato amylose and embodiment 1 gained amylose starch soybean lecithin inclusion compound not
Fig. 2 invents respectively the X-ray diffracting spectrum of relevant not inclusion retrogradation potato amylose and embodiment 1 gained amylose starch soybean lecithin inclusion compound.
Embodiment
For better understanding the present invention, below in conjunction with embodiment, the present invention is described further.The present invention has many successful embodiment, enumerates six specific embodiments below, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1
It is 12% starch milk that the first step yam starch (50g, butt) is made into mass percent concentration with Sodium phosphate dibasic-sodium dihydrogen phosphate buffer, and regulates pH to 4.5, is placed in encloses container and at 99 DEG C, stirs gelatinization 60min; After gelatinization completes, dextrin is cooling, add Pullulanase (OPTIMAX L-1000, Jie Nengke biotechnology company limited), consumption is that every gram of dry starch adds Pullulanase 10u, stirring reaction 3 hours at 65 DEG C; Regulate pH to 5.5, add high temperature resistant α-amylase (Liquozyme Supra, Novozymes company), consumption is that every gram of dry starch adds α-amylase 5u, stirring reaction 2 minutes at 110 DEG C, regulates pH to 2.5 and keeps 10 minutes enzymes that go out, and obtains amylose starch solution;
The temperature of step (1) gained amylose starch solution is adjusted to 50 DEG C by second step, is that 20% soybean lecithin tetrahydrofuran solution 30g is added dropwise in above-mentioned solution by being dissolved with mass percent, insulated and stirred reaction 2 hours; Be cooled to after room temperature, put into 4 DEG C of refrigerator and cooled and hide 18 hours;
The 3rd step is by centrifugal the product of step (2), and washing, obtains pale yellow powder shape product after dry, pulverize.The product obtaining is measured and is shown through molybdenum blue spectrophotometric method after wet method digestion, and in every gram of product, the content of soybean lecithin is 106 milligrams.Measure by accelerating acid number and the peroxide value of storage experiment to this product, result show this product 50 DEG C storage 20 days after, its acid number and peroxide value are respectively 2.8 and 1.2, with the Yelkin TTS mass content former yam starch/soybean lecithin mixture (acid number 5.5 that is 106mg/g, peroxide value 2.4) to compare, stability obviously improves.
Molybdenum blue spectrophotometric method is the common method of measuring lecithin content, concrete measuring method is: accurately take 0.5g inclusion compound, by sample after wet method digestion, Digestive system is settled in 100mL volumetric flask, after dilution suitable multiple, get 10mL in 50mL Erlenmeyer flask with transfer pipet, add 5mL Sodium orthomolybdate dilution heat of sulfuric acid, shake up and leave standstill after several seconds, add 2mL ascorbic acid solution, mix and be placed in more than 90 DEG C water-bath 10min, take out after cooling and be settled in 50mL volumetric flask, after shaking up, measure its absorbance at wavelength 826nm place with spectrophotometer, reference standard curve, the method of calculation of soybean lecithin content are as follows:
X＝(C
1×V
1×N×25)/(m
0×V
2)
In formula: X is the content of soybean lecithin in every gram of sample, mg/g; C
1for the phosphorus content in sample liquid definite from typical curve, mg/mL; V
1for the cumulative volume of constant volume after treatments of the sample, mL; m
0for sample quality, g; V
2for from V
1the sample volume of middle absorption, mL; N is the extension rate after Digestive system constant volume; 25 are converted into the coefficient of soybean lecithin for phosphorus.
In the time that the soybean lecithin of inclusion complexation in amylose starch reaches a certain amount of, can record the variation of its structure by infrared spectra, main manifestations is at 1736cm
-1there is a new soybean lecithin carbonyl absorption peak (as Fig. 1) in left and right.Amylose starch inclusion complexation organism forms after inclusion compound, and its crystalline texture is generally typical V-type, as shown in Figure 2, different from the Type B crystalline texture of the retrogradation amylose starch of inclusion not,
Gained inclusion complexation product of the present invention, its crystalline texture is obvious V-type.
Acid number and peroxide value are to weigh the important indicator of soybean lecithin deterioration by oxidation degree.Accelerating storage experiment is the common experimental method of measuring Oil stability, concrete grammar is: get appropriate inclusion compound sample and ative starch/lecithin mixture, be placed in respectively white tool plug vial, in 50 DEG C of thermostat containers, preserve, in the 20th day, its peroxide value and acid number are measured.The measuring method of peroxide value and acid number is respectively with reference to GB/T5530-2005 and GB/T5538-2005.
Embodiment 2
It is 10% starch milk that the first step waxy corn starch (50g, butt) is made into mass percent concentration with Sodium phosphate dibasic-sodium dihydrogen phosphate buffer, and regulates pH to 6.5, is placed in encloses container and at 98 DEG C, stirs gelatinization 50min; After gelatinization completes, dextrin is cooling, add isoamylase (Pseudomonas sp, Sigma-Aldrich company), consumption is that every gram of dry starch adds isoamylase 20u, stirring reaction 2 hours at 45 DEG C; Regulate pH to 6.5, add mesophilicα-diastase (CLARASE L, Jie Nengke biotechnology company limited), consumption is that every gram of dry starch adds α-amylase 10u, stirring reaction 1 minute at 45 DEG C, regulates pH to 3.0 and keeps 15 minutes enzymes that go out, and obtains amylose starch solution;
The temperature of step (1) gained amylose starch solution is adjusted to 60 DEG C by second step, is that 30% soybean lecithin tetrahydrofuran solution 20g is added dropwise in above-mentioned solution by being dissolved with mass percent, insulated and stirred reaction 1 hour; Be cooled to after room temperature, put into 6 DEG C of refrigerator and cooled and hide 24 hours;
The 3rd step is by centrifugal the product of step (2), and washing, obtains pale yellow powder shape product after dry, pulverize.The product obtaining is measured (measuring method is with embodiment 1) through molybdenum blue spectrophotometric method and is shown after wet method digestion, and in every gram of product, the content of soybean lecithin is 88 milligrams.Measure by accelerating acid number and the peroxide value of storage experiment to this product, result show this product 50 DEG C storage 20 days after, its acid number and peroxide value are respectively 2.2 and 1.0, with the Yelkin TTS mass content former waxy corn starch/soybean lecithin mixture (acid number 5.0 that is 88mg/g, peroxide value 2.6) to compare, stability obviously improves.
Embodiment 3
It is 8% starch milk that the first step W-Gum (50g, butt) is made into mass percent concentration with Sodium phosphate dibasic-sodium dihydrogen phosphate buffer, and regulates pH to 5.5, is placed in encloses container and at 95 DEG C, stirs gelatinization 40min; After gelatinization completes, dextrin is cooling, add Pullulanase (OPTIMAX L-1000, Jie Nengke biotechnology company limited), consumption is that every gram of dry starch adds Pullulanase 10u, stirring reaction 3 hours at 55 DEG C; Regulate pH to 7.0, add high temperature resistant α-amylase (Liquozyme Supra, Novozymes company), consumption is that every gram of dry starch adds α-amylase 2u, stirring reaction 5 minutes at 95 DEG C, regulates pH to 2.7 and keeps 12 minutes enzymes that go out, and obtains amylose starch solution;
The temperature of step (1) gained amylose starch solution is adjusted to 30 DEG C by second step, is that 20% soybean lecithin tetrahydrofuran solution 30g is added dropwise in above-mentioned solution by being dissolved with mass percent, insulated and stirred reaction 4 hours; Be cooled to after room temperature, put into 10 DEG C of refrigerator and cooled and hide 36 hours;
The 3rd step is by centrifugal the product of step (2), and washing, obtains pale yellow powder shape product after dry, pulverize.The product obtaining is measured (measuring method is with embodiment 1) through molybdenum blue spectrophotometric method and is shown after wet method digestion, and in every gram of product, the content of soybean lecithin is 96 milligrams.Measure by accelerating acid number and the peroxide value of storage experiment to this product, result show this product 50 DEG C storage 20 days after, its acid number and peroxide value are respectively 2.3 and 1.1, with the Yelkin TTS mass content former W-Gum/soybean lecithin mixture (acid number 5.2 that is 96mg/g, peroxide value 2.7) to compare, stability obviously improves.
Embodiment 4
It is 5% starch milk that the first step wheat starch (50g, butt) is made into mass percent concentration with Sodium phosphate dibasic-sodium dihydrogen phosphate buffer, and regulates pH to 5.0, is placed in encloses container and at 96 DEG C, stirs gelatinization 30min; After gelatinization completes, dextrin is cooling, add isoamylase (Pseudomonas sp, Sigma-Aldrich company), consumption is that every gram of dry starch adds isoamylase 30u, stirring reaction 1 hour at 50 DEG C; Regulate pH to 5.5～7.0, add mesophilicα-diastase (CLARASE L, Jie Nengke biotechnology company limited), consumption is that every gram of dry starch adds α-amylase 1u, stirring reaction 10 minutes at 65 DEG C, regulates pH to 2.5 and keeps 10 minutes enzymes that go out, and obtains amylose starch solution;
The temperature of step (1) gained amylose starch solution is adjusted to 80 DEG C by second step, is that 25% soybean lecithin tetrahydrofuran solution 25g is added dropwise in above-mentioned solution by being dissolved with mass percent, insulated and stirred reaction 3 hours; Be cooled to after room temperature, put into 8 DEG C of refrigerator and cooled and hide 30 hours;
The 3rd step is by centrifugal the product of step (2), and washing, obtains pale yellow powder shape product after dry, pulverize.The product obtaining is measured (measuring method is with embodiment 1) through molybdenum blue spectrophotometric method and is shown after wet method digestion, and in every gram of product, the content of soybean lecithin is 102 milligrams.Measure by accelerating acid number and the peroxide value of storage experiment to this product, result show this product 50 DEG C storage 20 days after, its acid number and peroxide value are respectively 2.4 and 1.2, with the Yelkin TTS mass content former W-Gum/soybean lecithin mixture (acid number 5.4 that is 102mg/g, peroxide value 2.8) to compare, stability obviously improves.
Embodiment 5
It is 10% starch milk that the first step Waxy wheat starch (50g, butt) is made into mass percent concentration with Sodium phosphate dibasic-sodium dihydrogen phosphate buffer, and regulates pH to 4.5, is placed in encloses container and at 99 DEG C, stirs gelatinization 50min; After gelatinization completes, dextrin is cooling, add Pullulanase (OPTIMAX L-1000, Jie Nengke biotechnology company limited), consumption is that every gram of dry starch adds Pullulanase 20u, stirring reaction 2 hours at 55 DEG C; Regulate pH to 6.5, add high temperature resistant α-amylase (Liquozyme Supra, Novozymes company), consumption is that every gram of dry starch adds α-amylase 5u, stirring reaction 2 minutes at 100 DEG C, regulates pH to 2.8 and keeps 12 minutes enzymes that go out, and obtains amylose starch solution;
The temperature of step (1) gained amylose starch solution is adjusted to 70 DEG C by second step, is that 30% soybean lecithin tetrahydrofuran solution 20g is added dropwise in above-mentioned solution by being dissolved with mass percent, insulated and stirred reaction 2 hours; Be cooled to after room temperature, put into 4 DEG C of refrigerator and cooled and hide 18 hours;
The 3rd step is by centrifugal the product of step (2), and washing, obtains pale yellow powder shape product after dry, pulverize.The product obtaining is measured (measuring method is with embodiment 1) through molybdenum blue spectrophotometric method and is shown after wet method digestion, and in every gram of product, the content of soybean lecithin is 92 milligrams.Measure by accelerating acid number and the peroxide value of storage experiment to this product, result show this product 50 DEG C storage 20 days after, its acid number and peroxide value are respectively 2.2 and 1.0, with the Yelkin TTS mass content former W-Gum/soybean lecithin mixture (acid number 5.1 that is 92mg/g, peroxide value 2.6) to compare, stability obviously improves.
Embodiment 6
It is 12% starch milk that the first step tapioca (flour) (50g, butt) is made into mass percent concentration with Sodium phosphate dibasic-sodium dihydrogen phosphate buffer, and regulates pH to 6.0, is placed in encloses container and at 98 DEG C, stirs gelatinization 60min; After gelatinization completes, dextrin is cooling, add isoamylase (Pseudomonas sp, Sigma-Aldrich company), consumption is that every gram of dry starch adds isoamylase 30u, stirring reaction 1 hour at 45 DEG C; Regulate pH to 5.5, add mesophilicα-diastase (CLARASE L, Jie Nengke biotechnology company limited), consumption is that every gram of dry starch adds α-amylase 2u, stirring reaction 5 minutes at 60 DEG C, regulates pH to 2.5 and keeps 10 minutes enzymes that go out, and obtains amylose starch solution;
The temperature of step (1) gained amylose starch solution is adjusted to 60 DEG C by second step, is that 25% soybean lecithin tetrahydrofuran solution 25g is added dropwise in above-mentioned solution by being dissolved with mass percent, insulated and stirred reaction 3 hours; Be cooled to after room temperature, put into 4 DEG C of refrigerator and cooled and hide 18 hours;
The 3rd step is by centrifugal the product of step (2), and washing, obtains pale yellow powder shape product after dry, pulverize.The product obtaining is measured (measuring method is with embodiment 1) through molybdenum blue spectrophotometric method and is shown after wet method digestion, and in every gram of product, the content of soybean lecithin is 104 milligrams.Measure by accelerating acid number and the peroxide value of storage experiment to this product, result show this product 50 DEG C storage 20 days after, its acid number and peroxide value are respectively 2.4 and 1.2, with the Yelkin TTS mass content former W-Gum/soybean lecithin mixture (acid number 5.5 that is 104mg/g, peroxide value 2.8) to compare, stability obviously improves.
As mentioned above, can implement preferably the present invention.
Claims (5)
1. a preparation method for amylose starch soybean lecithin inclusion compound, is characterized in that comprising the steps:
(1) to be made into mass percent concentration with Sodium phosphate dibasic-sodium dihydrogen phosphate buffer be 5%～12% starch milk to starch material, and regulate pH to 4.5～6.5, is placed in encloses container and stirs gelatinization 30～60min at 95～99 DEG C; After gelatinization completes, dextrin is cooling, add debranching factor, consumption is that every gram of dry starch adds debranching factor 10～30u, stirring reaction 1～3 hour at 45～65 DEG C; Regulate pH to 5.5～7.0, add α-amylase, consumption is that every gram of dry starch adds α-amylase 1～10u, and stirring reaction 1～10 minute at 45～110 DEG C regulates pH to 2.5～3.0 and keeps 10～15 minutes, and the enzyme that goes out, obtains amylose starch solution;
(2) temperature of gained amylose starch solution is adjusted to 30～80 DEG C, dripping and being dissolved with mass percent is 20%～30% soybean lecithin tetrahydrofuran solution, insulated and stirred reaction 1～4 hour; Be cooled to after room temperature, put into 4～10 DEG C of refrigerator and cooled and hide 18～36 hours; Every gram of dry starch adds soybean lecithin tetrahydrofuran solution (0.4～0.6) g;
(3), by centrifugal the product of step (2), washing, obtains pale yellow powder shape product after dry, pulverize.
2. the preparation method of amylose starch soybean lecithin inclusion compound according to claim 1, is characterized in that: the described starch material of step (1) is the one in W-Gum, waxy corn starch, wheat starch, Waxy wheat starch, tapioca (flour) and yam starch.
3. the preparation method of amylose starch soybean lecithin inclusion compound according to claim 1, is characterized in that: the described debranching factor of step (1) is Pullulanase or isoamylase.
4. the preparation method of amylose starch soybean lecithin inclusion compound according to claim 1, is characterized in that: the described α-amylase of step (1) is middle temperature or high temperature resistant α-amylase.
5. the preparation method of amylose starch soybean lecithin inclusion compound according to claim 1, is characterized in that: the described washing of step (3) for deionized water wash repeatedly, until noresidue tetrahydrofuran (THF) in solution.
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| CN111617262A (en) * | 2020-05-21 | 2020-09-04 | 华南理工大学 | Starch-based colon-targeted controlled-release crystal inclusion compound and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105777919A (en) * | 2016-03-10 | 2016-07-20 | 华南理工大学 | High-efficient and stable-state preparation method of soybean lecithin |
| CN105777919B (en) * | 2016-03-10 | 2018-01-16 | 华南理工大学 | The efficient stable state preparation method of soybean lecithin |
| CN105942415A (en) * | 2016-05-19 | 2016-09-21 | 福家欢食品股份有限公司 | Preparation method of instant noodle seasoning packet rich in efficient steady-state beta-carotene |
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| CN106359973A (en) * | 2016-08-27 | 2017-02-01 | 天长市金农农业发展有限公司 | Nutritionally balanced special feed for piglets |
| CN107028185A (en) * | 2017-03-23 | 2017-08-11 | 上海应用技术大学 | A kind of amylose curcumin inclusion compound and preparation method thereof |
| CN107028185B (en) * | 2017-03-23 | 2021-01-08 | 上海应用技术大学 | Amylose-curcumin inclusion compound and preparation method thereof |
| CN108244645A (en) * | 2018-01-15 | 2018-07-06 | 沈阳师范大学 | The preparation method of little particle amylose-DHA/ resveratrol inclusion compounds |
| CN111617262A (en) * | 2020-05-21 | 2020-09-04 | 华南理工大学 | Starch-based colon-targeted controlled-release crystal inclusion compound and preparation method thereof |
| CN111617262B (en) * | 2020-05-21 | 2021-05-25 | 华南理工大学 | Starch-based colon-targeted controlled-release crystal inclusion compound and preparation method thereof |
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