Extraction method of goose liver lecithin

Abstract

The invention belongs to the technical field of phospholipid preparation, and particularly relates to an extraction method of goose liver lecithin. The invention provides an extraction method of goose liver lecithin. The extraction method comprises the following steps: S1, pretreatment; s2, performing centrifugal treatment; s3, ultrasonic treatment; s4, centrifuging again; and S5, concentrating and drying. According to the invention, a single-factor experiment is carried out on five factors, namely ultrasonic time, temperature, power and ethanol concentration and dosage, and the extraction conditions of the goose liver lecithin are optimized on the basis of the lecithin extraction rate. The result of the embodiment shows that the optimal parameters for extracting the goose liver lecithin are as follows: the ultrasonic temperature is 33 DEG C, the ultrasonic time is 45min, the ethanol concentration is 100% and the ethanol dosage is 15ml, and the extraction rate of experimental lecithin is verified to reach 72.46% under the parameters. The extraction method is simple in process, high-precision extraction is realized, and the yield of lecithin is remarkably improved.

Description

Technical Field

[0001] The invention belongs to the technical field of phospholipid preparation, and particularly relates to a method for extracting goose liver lecithin. Background Art

[0002] Phosphatidylcholine (PC) is widely used in the food and pharmaceutical industries for its emulsifying properties and health benefits. Currently, lecithin on the market mainly comes from plant sources such as soybeans, while animal-derived lecithin is gaining more attention due to its different properties. However, there are still some technical challenges in effectively extracting high-purity lecithin from goose liver.

[0003] In terms of production scale, the production volume of ordinary goose liver in China has shown a steady growth trend in the past decade. However, the ordinary goose liver industry in China faces a challenge: the market share of ordinary goose liver in China is still small, the goose liver industry chain is short, and most ordinary goose livers are still used as feed or directly discarded. Therefore, the ecological and environmental protection issues in the production and waste process are also challenges that must be faced. How to reduce the impact on the environment and improve the sustainable development capacity of the industry are the key to the future development of the ordinary goose liver industry in China.

[0004] Research on the utilization and processing of beneficial ingredients in ordinary goose liver can effectively solve existing problems. However, there are few results in the utilization and processing of ordinary goose liver on the market. The current utilization rate of ordinary goose liver is low, and research on goose liver mostly remains in the experimental research of processing technology. There is no clear conclusion on the identification of its specific component structure, especially the chemical composition and properties of goose liver need further research, and the industrial chain is short. Summary of the invention

[0005] The purpose of the present invention is to provide a method for extracting goose liver lecithin. The present invention optimizes the extraction conditions by conducting single factor experiments on five factors, namely, ultrasonic time, temperature, power, and ethanol concentration and dosage, to solve the above-mentioned problems.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] In one aspect, the present invention provides a method for extracting goose liver lecithin, comprising the following steps:

[0008] S1. Pretreatment: Take goose liver, chop it into pieces, add deionized water, perform high-speed homogenization, place it in a centrifuge tube, then add ethyl acetate dropwise and stir to obtain a mixture, and let it stand;

[0009] S2. Centrifugation: The mixture obtained in S1 is centrifuged to separate the supernatant;

[0010] S3. Ultrasonic treatment: Add ethanol solution to the supernatant obtained by centrifugation in S2, stir evenly, and ultrasonically treat to obtain a mixture;

[0011] S4. Centrifuge again: Centrifuge the mixture in S3 again to separate the supernatant;

[0012] S5. Concentration and drying: The supernatant separated in S4 is further concentrated and nearly dried to obtain light yellow lecithin.

[0013] Furthermore, the ultrasonic treatment is to add a certain amount of ethanol solution of a certain concentration to the processed goose liver, and use different ultrasonic time, ultrasonic temperature and ultrasonic power for treatment.

[0014] Furthermore, the concentrated drying uses a rotary evaporation method to precipitate lecithin as much as possible to reduce loss.

[0015] Preferably, the amount of ethyl acetate added in step S1 is 10%-30% of the volume of the goose liver homogenate.

[0016] Preferably, in the step S2, the centrifugal treatment is performed with a centrifugal force of 3000-5000 r / min.

[0017] Preferably, the concentration of ethanol in step S3 is 85%-100%; the amount of ethanol added is 25%-125% of the volume of ethyl acetate.

[0018] Preferably, the ultrasonic treatment time in step S3 is 20-60 min; the ultrasonic temperature is 15-55° C.; and the ultrasonic power is 200-350 W.

[0019] Preferably, the concentration of ethanol in step S3 is 100%; the amount of ethanol added is 100% of the volume of ethyl acetate.

[0020] Preferably, the ultrasonic temperature in step S3 is 33° C. and the ultrasonic time is 45 min.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] (1) Improved extraction efficiency: The extraction rate of lecithin was significantly improved by optimizing the ultrasonic treatment parameters such as time, temperature, power, and ethanol concentration. The application of response surface design further optimized the process conditions, making the extraction process more efficient.

[0023] (2) Improved product purity: Multiple centrifugation separations effectively remove impurities, and combined with rotary evaporation and vacuum drying technology, the high purity of crude lecithin is ensured.

[0024] (3) Improved environmental performance: By recycling solvents and reducing solvent usage, the impact on the environment is reduced. At the same time, the optimized process reduces energy consumption and improves overall environmental performance.

[0025] (4) Improved economic benefits: Due to the improvement of extraction efficiency and product purity, production costs are reduced and product added value is increased.

[0026] (5) Innovative process design: Ultrasonic-assisted extraction technology is used to achieve fine control of the extraction process by adjusting ultrasonic parameters. DETAILED DESCRIPTION

[0027] In one aspect, the present invention provides a method for extracting goose liver lecithin, comprising the following steps:

[0028] S1. Pretreatment: Take goose liver, chop it into pieces, add deionized water, perform high-speed homogenization, place it in a centrifuge tube, then add ethyl acetate dropwise and stir to obtain a mixture, and let it stand;

[0029] S2. Centrifugation: The mixture obtained in S1 is centrifuged to separate the supernatant;

[0030] S3. Ultrasonic treatment: Add ethanol solution to the supernatant obtained by centrifugation in S2, stir evenly, and ultrasonically treat to obtain a mixture;

[0031] S4. Centrifugal filtration again: The mixture in S3 is centrifuged again to separate the supernatant;

[0032] S5. Concentration and drying: The supernatant separated in S4 is further concentrated and nearly dried to obtain light yellow lecithin.

[0033] Furthermore, the amount of ethyl acetate added in step S1 is 10%-30% of the volume of the goose liver homogenate, preferably 10%.

[0034] In the step S2, the centrifugal treatment is performed at a centrifugal force of 3000-5000 r / min, preferably 4000 r / min.

[0035] In step S3, the concentration of ethanol is 85%-100%; the amount of ethanol added is 25%-125% of the volume of ethyl acetate, and the ethanol concentration is preferably 85%, 90%, 95%, 100%; the amount of ethanol added is preferably 25%, 50%, 75%, 100%, 125%. The most preferred ethanol concentration is 100% and the amount added is 100% of the volume of ethyl acetate.

[0036] Preferably, the ultrasonic treatment time in step S3 is 20-60 min; the ultrasonic temperature is 15-55°C; the ultrasonic power is 200-350 W, the time is preferably 20, 30, 40, 50, 60 min; the temperature is 15, 25, 35, 45, 55°C, and the power is 200, 250, 300, 350 W. The most preferred ultrasonic temperature is 33°C and the time is 45 min.

[0037] In order to further illustrate the present invention, the technical solutions provided by the present invention are described in detail below in conjunction with embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0038] The production processes, experimental methods or detection methods involved in the embodiments of the present invention, unless otherwise specified, are all conventional methods in the prior art, and their names and / or abbreviations are all conventional names in the field, and are very clear and unambiguous in the relevant application fields. Technical personnel in the field can understand the conventional process steps based on the names and apply the corresponding equipment, and implement them according to conventional conditions or the conditions recommended by the manufacturer.

[0039] The various instruments, equipment, raw materials or reagents used in the embodiments of the present invention are not particularly limited in terms of their sources, and are all conventional products that can be purchased through regular commercial channels, or can be prepared according to conventional methods well known to those skilled in the art.

[0040] Example 1

[0041] A method for extracting goose liver lecithin comprises the following steps:

[0042] S1. Pretreatment: Take goose liver, chop it and add deionized water, perform high-speed homogenization, accurately weigh 5g, place it in a 50ml centrifuge tube, then add 20ml of ethyl acetate dropwise, stir to obtain a mixture, and let it stand;

[0043] S2. Centrifugation: The mixture obtained in S1 was centrifuged at 4000 r / min for 15 min to separate the supernatant;

[0044] S3. Ultrasonic treatment: add 100% ethanol solution, ethanol in an amount of 20 ml, and stir evenly, ultrasonic power 200 W, to obtain a mixture;

[0045] S4. Centrifugal filtration again: The mixture in S3 is centrifuged again to separate the supernatant;

[0046] S5. Concentration and drying: The supernatant separated in S4 is further concentrated and nearly dried to obtain light yellow lecithin.

[0047] Example 2

[0048] Determination of lecithin extraction rate

[0049] The lecithin obtained in Example 1 was digested with nitric acid and then measured by IPC method to calculate the lecithin extraction rate.

[0050] Example 3

[0051] Single factor effect experiment

[0052] The invention conducts single factor experiments on five factors, namely, ultrasonic time, temperature, power, ethanol concentration and dosage, and conducts experiments based on the lecithin extraction rate.

[0053] ① Ultrasonic temperature

[0054] The steps are basically the same as those in Example 1, except that the ultrasonic temperature is 15, 25, 35, 45, and 55° C., the ultrasonic power is 200 W, the ultrasonic frequency is 28 Hz, the ultrasonic time is 30 min, the ethanol concentration is 95%, and the ethanol amount is 20 mL.

[0055] Results: When the ultrasonic temperature is low, the lipid bilayer fluidity of the cell membrane is poor, and the ultrasonic vibration effect is difficult to play, resulting in a low extraction rate; as the ultrasonic temperature increases, the lipid bilayer fluidity of the cell membrane is enhanced, the ultrasonic vibration effect is more sufficient, and the extraction rate also increases. However, when the ultrasonic temperature is too high, lecithin will denature, resulting in a decrease in the extraction rate. The extraction rate of goose liver lecithin increases with the increase of ultrasonic temperature. When the temperature is 35℃, the extraction rate reaches the highest. When it exceeds 35℃, the extraction rate gradually decreases with the increase of temperature.

[0056] ②Ultrasound time

[0057] The steps are basically the same as those in implementation 1, except that the ultrasonic time is 20, 30, 40, 50, and 60 min, the ultrasonic power is 200 W, the ultrasonic frequency is 28 Hz, the ultrasonic temperature is 35° C., the ethanol concentration is 95%, and the ethanol amount is 20 mL.

[0058] Results analysis: With the extension of ultrasonic time, the extraction rate of goose liver lecithin continued to increase. The longer the ultrasonic time, the higher the lecithin extraction rate in the sample. This is because the longer the ultrasonic action time, the more collisions the lecithin molecules and the solvent molecules, and the faster the dissolution rate. At the same time, the ultrasonic wave has a more complete destructive effect on the cell membrane, which is conducive to the release of lecithin. However, after the extraction time exceeds 30 minutes, the trend of increasing extraction rate is no longer significant. This is because if the ultrasonic action time is too long, it may cause the sample to overheat, causing the molecular structure of lecithin to change, and the extraction rate will decrease instead. Therefore, the optimal extraction time is selected as 30 minutes.

[0059] ③ Ultrasonic power

[0060] The steps are basically the same as those in Example 1, except that the ultrasonic power is 200, 250, 300, and 350 W, the ultrasonic frequency is 28 Hz, the ultrasonic temperature is 35° C., the ultrasonic time is 40 min, the ethanol concentration is 95%, and the ethanol amount is 15 mL.

[0061] Result analysis: When the ultrasonic power was between 200 and 350 W, the PC extraction rate did not change significantly, so 200 W was used as the power for ultrasonic extraction of goose liver lecithin in subsequent experiments.

[0062] ④Ethanol concentration

[0063] The steps are basically the same as those in Example 1, except that the ethanol concentration is 85%, 90%, 95%, and 100%, the ultrasonic power is 200 W, the ultrasonic frequency is 28 Hz, the ultrasonic temperature is 35° C., the ultrasonic time is 40 min, and the ethanol amount is 20 mL.

[0064] Results: With the increase of ethanol concentration, the extraction rate of lecithin continued to increase, and the extraction rate reached the highest when the ethanol concentration was 95%. When 85% and 90% ethanol was used for extraction, ethanol could effectively stabilize the extracted lecithin and prevent its decomposition and oxidation. The addition of ethanol could promote the formation of colloidal particles of phospholipid molecules in the solution and separate them from the solution by precipitation. However, when anhydrous ethanol was used for extraction, the extraction rate of lecithin decreased instead. This is because anhydrous ethanol can cause excessive precipitation of phospholipid molecules and even form flocs, which may destroy the molecular structure of lecithin, affect its stability and activity, and affect the extraction purity. Therefore, 95% ethanol was selected as the optimal ethanol concentration for extraction.

[0065] ⑤Amount of ethanol

[0066] The steps are basically the same as those in Example 1, except that the amount of ethanol added is 25%, 50%, 75%, 100%, and 125% of ethyl acetate, that is, the amount of ethanol is 5, 10, 15, 20, and 25 mL, the ultrasonic power is 200 W, the ultrasonic frequency is 28 Hz, the ultrasonic temperature is 35° C., the ultrasonic time is 40 min, and the ethanol concentration is 95%.

[0067] Results analysis: With the increase of solvent dosage, the lecithin extraction rate increased, and the increasing trend became gentle after the ethanol dosage reached 15mL. The experimental results show that the amount of ethanol solvent used for extraction is small, and the solubility of ethanol is not enough to destroy the cell membrane. More impurities may also be introduced during the extraction process, reducing the purity of lecithin and resulting in a lower extraction rate. From the perspective of selecting a high extraction rate and reducing solvent costs, the optimal ethanol dosage is 15mL.

[0068] Example 4

[0069] Response Surface Design

[0070] On the basis of single factor, the response surface was used to optimize the extraction of goose liver lecithin. The experimental factors and coding table are shown in Table 1 (response surface factor level coding table). Preliminary experiments have shown that the ultrasonic power of 200-350W has little effect on the extraction rate of goose liver lecithin, so the lowest power is selected considering the cost.

[0071] Table 1

[0072]

[0073] Response surface experiment results and analysis

[0074] Using Design-Expert 8Trial 120 software, multiple regression fitting was performed on the data in Table 2 (ultrasonic-assisted extraction of goose liver lecithin process response surface scheme and experimental results), and the multiple quadratic regression model equation (1) was obtained: Y = 55.32-1.27A-0.2275B+2.42C-7.47D-4.79AB+4.32AC+2.97AD-1.46BC-2.84BD-0.9650CD-0.3724A 2 -0.3612B 2 +1.77C 2 +2.51D 2 In equation (1), Y is the lecithin extraction rate, A represents the ultrasonic temperature, B represents the ultrasonic time, C represents the ethanol concentration, and D represents the ethanol dosage.

[0075] Table 2

[0076]

[0077]

[0078] In summary, the present invention provides a method for extracting goose liver lecithin, which utilizes five factors, namely, ultrasonic temperature, time, power, ethanol dosage, and concentration, to regulate the extraction efficiency. In particular, under the conditions of ultrasonic temperature of 33°C, ultrasonic time of 45min, ethanol concentration of 100%, and ethanol addition of 100% of the volume of ethyl acetate, this parameter has been experimentally verified, and the extraction rate of lecithin can reach 72.46%.

[0079] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention, not all of the embodiments. People can also obtain other embodiments based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A method for extracting goose liver lecithin, characterized in that: The extraction method comprises the following steps: S1. Pretreatment: Take goose liver, chop it into pieces, add deionized water, perform high-speed homogenization, place it in a centrifuge tube, then add ethyl acetate dropwise and stir to obtain a mixture, and let it stand; S2. Centrifugation: The mixture obtained in S1 is centrifuged to separate the supernatant; S3. Ultrasonic treatment: add ethanol solution to the supernatant obtained by centrifugation of S2, stir evenly, and ultrasonically treat to obtain a mixture; S4. Centrifuge again: Centrifuge the mixture in S3 again to separate the supernatant; S5. Concentration and drying: The supernatant separated in S4 is further concentrated and nearly dried to obtain light yellow lecithin.

2. The extraction method according to claim 1, characterized in that The amount of ethyl acetate added in step S1 is 10%-30% of the volume of the goose liver homogenate.

3. The extraction method according to claim 1, characterized in that The centrifugal treatment in step S2 has a centrifugal force of 3000-5000 r / min.

4. The extraction method according to claim 2, characterized in that The concentration of ethanol in step S3 is 85%-100%; the amount of ethanol added is 25%-125% of the volume of ethyl acetate.

5. The extraction method according to claim 1, characterized in that The ultrasonic treatment time in step S3 is 20-60 min; the ultrasonic temperature is 15-55° C.; and the ultrasonic power is 200-350 W.

6. The extraction method according to claim 1, characterized in that The concentration of ethanol in step S3 is 100%; the amount of ethanol added is 100% of the volume of ethyl acetate.

7. The extraction method according to claim 1, characterized in that The ultrasonic temperature in step S3 is 33° C. and the ultrasonic time is 45 min.

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