Method for separating and extracting grease from procambarus clarkii heads

Abstract

The invention discloses a method for separating and extracting grease from procambarus clarkia heads, which comprises the following steps of: smashing the procambarus clarkia heads into paste, and adding n-hexane in a corresponding proportion; the cavitation effect of ultrasonic waves is combined, so that the cell structure is destroyed, and the dissolution of lipid molecules in cells is increased; the microwave method can quickly heat polar molecules to quickly gasify intracellular water molecules so as to shorten the extraction time, and the shrimp head grease is obtained by filtering and evaporating a solvent. The extraction method provided by the invention is short in time consumption, high in efficiency and high in extraction rate.

Description

Technical Field

[0001] The invention belongs to the field of food and chemical industry, and particularly relates to a method for separating and extracting oil from Procambarus clarkii shrimp heads. Background Art

[0002] Procambarus clarkii (Procambarus clarkii) Commonly known as crayfish, its by-products account for about 45-75%, and crude fat accounts for about 1.5-4.0% of the wet weight. These fats are rich in nutrients such as polyunsaturated fatty acids (PUFA) and astaxanthin, which can be used in food, health products and biomedicine. However, in actual production, the commonly used method for separating and extracting oils is to use a cooking method combined with a centrifugation method. This method causes thermal oxidation degradation of polyunsaturated fatty acids at high temperatures and reduces the quality of oils, so it can only be used as feed.

[0003] In summary, a method for preparing oil from Procambarus clarkii heads with high extraction efficiency and high oil quality is needed. Summary of the invention

[0004] The present invention provides a method and application for separating and extracting oil from the head of Procambarus clarkii. The purpose is to improve the utilization rate of by-products and the quality of oil by using green, efficient, low-cost and easy-to-operate oil separation and extraction technology, so as to achieve high-quality and high-value utilization of by-products.

[0005] The present invention is achieved through the following technical solutions: A method for separating and extracting oil from the head of a Procambarus clarkii shrimp comprises the following steps: (1) First, the crayfish heads were pre-processed and crushed using a grinder after thawing; (2) using n-hexane as a solvent and fully mixing and stirring at a solid-liquid ratio of 1:10 to 1:20 g / mL; (3) The mixed solution is separated and extracted simultaneously at an ultrasonic power of 400-600 W and a microwave power of 500-900 W at a temperature of 40° C. for 10-30 min; (4) After solid-liquid separation, the supernatant is filtered, and the solid residue is washed three times with n-hexane, and the combined solution is collected; (5) removing the solvent by rotary evaporation at 35-45° C. and 70-90 r / min to obtain the crayfish head oil; Preferably, in step 1, the crayfish heads are thawed at room temperature.

[0006] Preferably, in step 2, 10 g of raw material mass and n-hexane volume are added in a ratio of 1:10 to 1:20 g / mL.

[0007] Preferably, in step 2, n-hexane is used as a solvent and the mixture is fully stirred under the condition of a material-liquid ratio of 1:15 g / mL.

[0008] Preferably, reagent-grade n-hexane with a concentration of 97% which is easy to recycle, has high stability and low cost is adopted.

[0009] Preferably, in step 3, the mixed solution is synchronously separated and extracted for 20 min under the conditions of an ultrasonic power of 500 W, a microwave power of 700 W, and a temperature of 40 °C; Preferably, the ultrasonic mode in step 3 is intermittent ultrasonic with an interval of 2 s and an intermittent time of 3 s to prevent lipid oxidation caused by excessive temperature.

[0010] Compared with the prior art, the beneficial effects of the present invention are as follows: (a) The ultrasonic and microwave synergistic technology is adopted to extract oil from shrimp heads, which improves the extraction rate of shrimp oil to more than 95%, and reduces the solvent usage amount and extraction time.

[0011] (b) Controlling the extraction temperature at 35-45 °C can effectively reduce oil oxidation and improve the oil quality.

[0012] (c) The ultrasonic power and microwave power suitable for extracting oil from the heads of Procambarus clarkii are determined.

[0013] (d) The optimal solvent ratio suitable for extracting oil from the heads of Procambarus clarkii is determined. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 It is a schematic diagram of the single-factor experiment results under different material-liquid ratio conditions in an embodiment of the present invention.

[0015] Figure 2 It is a schematic diagram of the single-factor experiment results with different ultrasonic powers in an embodiment of the present invention.

[0016] Figure 3 It is a schematic diagram of the single-factor experiment results with different microwave powers in an embodiment of the present invention.

[0017] Figure 4 It is a schematic diagram of the single-factor experiment results with different extraction times in an embodiment of the present invention.

[0018] Figure 5 It is a schematic diagram of the process structure of the method for separating and extracting oil in an embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0019] The following describes the embodiments of the present invention in detail with reference to the drawings: The present embodiment is implemented on the premise of the technical solution of the present invention, and detailed implementation manners and specific operation processes are given, but the protection scope of the present invention is not limited to the following embodiments.

[0020] In the embodiments of the present invention, the method for detecting the crude fat content refers to the national standard GB5009.6-2016; In the embodiments of the present invention, the method for detecting the moisture content refers to the national standard GB5009.3-2016; In the embodiments of the present invention, the extraction rate (%) of Procambarus clarkii shrimp oil = the content of the obtained shrimp oil / the crude fat content × 100% The following further elaborates on the present invention in conjunction with the drawings and implementation methods: Example 1:

[0021] To explore the influence of the solid-liquid ratio on the extraction amount of shrimp head oil, a single-factor experiment was designed, repeated three times, and the average value was taken. 10.0 g of shrimp heads were weighed and crushed, and the solid-liquid ratio (1:5 g / mL, 1:10 g / mL, 1:15 g / mL, 1:20 g / mL, 1:25 g / mL) was set as the single-factor condition.

[0022] From Figure 1 , 5 It can be seen that there is a significant correlation between the extraction rate of Procambarus clarkii shrimp head oil and the solid-liquid ratio. When the solid-liquid ratio is 1:15 g / mL, the extraction rate reaches the peak, indicating that the oil has basically dissolved into n-hexane and the solution is in a saturated state. Adjusting the solid-liquid ratio affects the solubility of lipids. Finally, the solid-liquid ratio for extracting Procambarus clarkii shrimp head oil is determined to be 1:15 g / mL. Example 2:

[0023] To explore the influence of ultrasonic power on the extraction rate of Procambarus clarkii shrimp head oil, a single-factor experiment was designed, repeated three times, and the average value was taken. 10.0 g of shrimp heads were weighed and crushed, and the ultrasonic power (200W, 300W, 400W, 500W, 600W) was set.

[0024] From Figure 2 , 5 It can be seen that there is a significant correlation between the extraction rate of Procambarus clarkii shrimp head oil and the ultrasonic power. When the ultrasonic power reaches 500W, the highest extraction rate is obtained. The oil cannot be fully dissolved at a lower power, resulting in a low extraction rate. Finally, the optimal ultrasonic power for extracting Procambarus clarkii shrimp head oil is determined to be 500W. Example 3:

[0025] To explore the influence of microwave power on the extraction rate of Procambarus clarkii shrimp head oil, a single-factor experiment was designed, repeated three times, and the average value was taken. The microwave power (400W, 500W, 600W, 700W, 800W) was set.

[0026] From Figure 3 , 5It can be seen that the extraction rate of the fat from the heads of Procambarus clarkii first increases and then decreases as the microwave power increases. When the microwave power reaches 700 W, the extraction rate is the highest. After 700 W, the fat extraction rate begins to decline. The reason is that the microwave power affects the movement of polar molecules in the sample, resulting in the insufficient dissolution of fat. Too low microwave power will also affect the heat transfer, thereby reducing the extraction efficiency. Finally, the optimal microwave power for the heads of Procambarus clarkii is determined to be 700 W. Example 4:

[0027] To explore the effect of extraction time on the fat extraction rate from the heads of Procambarus clarkii, a single-factor experiment was designed, repeated three times, and the average value was taken. The working times (10 min, 15 min, 20 min, 25 min, 30 min) were set.

[0028] From Figure 4 and 5 it can be seen that there is a significant correlation between the fat extraction rate from the heads of Procambarus clarkii and the extraction time. When the working time reaches 20 min, the highest extraction rate is obtained. After 20 min, the extraction rate begins to decline. This is because long-term ultrasonic microwave work will cause excessive heat, resulting in lipid decomposition, thus reducing the extraction rate. Finally, the optimal extraction time for the fat from the heads of Procambarus clarkii is determined to be 20 min.

[0029] According to the above implementation conditions, under the conditions of a material-liquid ratio of 1:15 g / mL, an ultrasonic power of 500 W, a microwave power of 700 W, and an extraction time of 20 min, under these optimized conditions, the extraction rate of the fat from the heads of Procambarus clarkii reaches the highest value, and the process is stable and efficient, suitable for industrial production. This process can not only significantly improve the fat extraction rate, but also effectively reduce energy consumption and the amount of solvent used, with high economic benefits and environmental friendliness.

[0030] The above shows and describes the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. What is described in the above embodiments and the specification only illustrates the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the scope of the present invention claimed. The scope of protection claimed by the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for separating and extracting oil from the head of Procambarus clarkii, characterized in that: The following steps are involved: (1) First, the crayfish heads were pre-processed and crushed using a grinder after thawing; (2) using n-hexane as a solvent and fully mixing and stirring at a solid-liquid ratio of 1:10 to 1:20 g / mL; (3) The mixed solution is separated and extracted simultaneously at an ultrasonic power of 400-600 W and a microwave power of 500-900 W at a temperature of 40° C. for 10-30 min; (4) After solid-liquid separation, the supernatant is filtered, and the solid residue is washed three times with n-hexane, and the combined solution is collected; (5) The crayfish head oil is obtained by rotary evaporation at 35-45°C and 70-90 r / min.

2. The method for separating and extracting oil from the head of Procambarus clarkii according to claim 1, characterized in that: In the step (1), the crayfish heads are thawed at room temperature.

3. The method for separating and extracting oil from Procambarus clarkii shrimp heads according to claim 1, characterized in that: In the step (2), 10 g of the raw material mass and the volume of n-hexane are added in a ratio of 1:10 to 1:20 g / mL.

4. The method for separating and extracting oil from Procambarus clarkii shrimp heads according to claim 1, characterized in that: In the step (2), n-hexane is used as the solvent and the mixture is fully mixed and stirred at a solid-liquid ratio of 1:15 g / mL.

5. The method for separating and extracting oil from Procambarus clarkii shrimp heads according to claim 1, characterized in that: The reagent grade concentration of 97% n-hexane is used, which is easy to recover, highly stable and low-cost.

6. The method for separating and extracting oil from Procambarus clarkii shrimp heads according to claim 1, characterized in that: In the step (3), the mixed solution is separated and extracted simultaneously under the conditions of an ultrasonic power of 500 W and a microwave power of 700 W and a temperature of 40° C. for 20 minutes.

7. The method for separating and extracting oil from Procambarus clarkii shrimp heads according to claim 1, characterized in that: The ultrasound mode in step (3) is intermittent ultrasound for 2 seconds and then for 3 seconds to prevent lipid oxidation caused by excessive temperature.

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