Process for preparing low-fluorine euphausia superba oil

Abstract

The invention relates to the technical field of food processing, in particular to a process for preparing low-fluorine euphausia superba oil, which comprises the following steps: S1, selecting euphausia superba powder with low fluorine content as a raw material; s2, grinding or crushing the euphausia superba powder to ensure the efficiency and uniformity of the extraction process; s3, soaking the euphausia superba powder in a solution containing calcium ions for defluorination treatment; s4, carrying out enzymatic hydrolysis on the krill powder to release grease; s5, extracting grease from the krill subjected to enzymolysis by using a supercritical CO2 technology; s6, carrying out molecular distillation refining on the extracted grease; s7, detecting the fluorine content of the refined krill oil; s8, finally, the krill oil which is detected to be qualified is subjected to sterile packaging and storage. According to the method, by optimizing the defluorination step and the extraction method, the fluorine content is effectively reduced, meanwhile, the nutritional value and safety of the oil product are kept, and the method is environmentally friendly in process, low in cost and suitable for large-scale production.

Description

Technical Field

[0001] The invention relates to the technical field of food processing, and in particular to a process for preparing low-fluorine Antarctic krill oil. Background Art

[0002] Antarctic krill oil is widely used in the fields of healthy food and healthcare due to its rich nutrients such as omega-3 fatty acids and phospholipids. However, Antarctic krill in the natural environment often contain high levels of fluoride. This high fluoride content not only affects the safety of krill oil, but also limits its application in food safety and medical fields. Although various methods have been used to reduce the fluoride content in Antarctic krill oil, including physical and chemical methods, these traditional methods often involve high energy consumption, high cost and unstable efficiency, and cannot effectively meet the needs of industrial production.

[0003] Current technical issues mainly focus on how to reduce the fluoride content in Antarctic krill oil in an efficient, low-cost and environmentally friendly way while ensuring the nutritional value and safety of the oil. Existing technologies are still insufficient in processing efficiency and cost control, making it difficult to achieve large-scale production while ensuring product quality. In addition, existing defluorination processes often require the use of high temperatures or strong chemical reagents, which may destroy sensitive nutrients in krill oil and reduce the health value of the final product.

[0004] Therefore, developing a new method for preparing low-fluoride Antarctic krill oil, which can effectively reduce the fluorine content while maintaining the nutrition and safety of the oil, is extremely important for expanding its market application. Summary of the invention

[0005] Based on the above purpose, the present invention provides a process for preparing low-fluorine Antarctic krill oil.

[0006] A process for preparing low-fluorine Antarctic krill oil comprises the following steps:

[0007] S1: Choose Antarctic krill meal with low fluoride content as raw material, and make sure to use krill meal that has been quality controlled to ensure that its fluoride content is low;

[0008] S2: Grinding or crushing the Antarctic krill powder to ensure the efficiency and uniformity of the extraction process;

[0009] S3: Soaking the Antarctic krill powder in a solution containing calcium ions for defluorination treatment to help remove surface impurities and reduce fluorine content;

[0010] S4: Enzymatic hydrolysis of defluorinated Antarctic krill meal to release oil;

[0011] S5: Using supercritical CO 2 Technology extracts oil from enzymatically hydrolyzed krill;

[0012] S6: The extracted oil is molecularly distilled and refined to remove residual impurities and trace fluorine;

[0013] S7: Test the fluorine content of the refined krill oil to ensure that it meets the predetermined standards;

[0014] S8: Finally, the krill oil that passes the test is aseptically packaged and stored.

[0015] Furthermore, the fluorine content of the Antarctic krill selected in S1 does not exceed 2 mg / kg, and the krill is quick-frozen at -20°C to -30°C for 1 to 2 hours.

[0016] Furthermore, the water temperature used for low-temperature water washing in S2 is 0°C to 5°C, the washing time is 5 to 10 minutes, and the water flow rate is 1 to 2 L / min.

[0017] Furthermore, the concentration of the calcium ion solution in S3 is 0.1M to 0.5M, the soaking time is 2 to 4 hours, the soaking temperature is 15°C to 25°C, and stirring is maintained during the soaking.

[0018] Furthermore, the enzyme used for enzymatic hydrolysis in S4 is protease, the addition amount is 0.5% to 1% of the weight of the krill meal, the hydrolysis temperature is 40° C. to 50° C., the pH value is 6.5 to 7.5, and the hydrolysis time is 4 to 6 hours.

[0019] Furthermore, the pressure of the supercritical CO2 extraction in S5 is 25MPa to 30MPa, the extraction temperature is 35°C to 45°C, the extraction time is 2 to 3 hours, and the CO2 purity is 99.9%.

[0020] Furthermore, the temperature of the molecular distillation in S6 is 150° C. to 160° C., the vacuum degree is 0.05 kPa to 0.1 kPa, and the distillation time is 1 to 2 hours.

[0021] Furthermore, the fluorine content in the S7 is detected using high performance liquid chromatography-mass spectrometry technology, and the standard for the detected fluorine content is lower than 0.1 mg / kg.

[0022] Furthermore, the packaging material used for the aseptic packaging in S8 is a high temperature resistant and antioxidant food grade plastic, and the storage temperature is 0°C to 5°C.

[0023] Beneficial effects of the present invention:

[0024] The present invention integrates defluorination treatment, supercritical CO 2Extraction and molecular distillation refining are used to systematically reduce the fluorine content in krill oil. Through these steps, not only the fluorine content is significantly reduced, but also the integrity of nutrients such as ω-3 fatty acids and phospholipids in the oil is maintained, thereby improving the nutritional value and safety of the product. In addition, the treatment method used is simpler in operation, energy-saving and environmentally friendly, reduces production costs, and is suitable for application on an industrial scale.

[0025] The present invention, by optimizing the traditional defluorination process, effectively reduces the impact on the environment and the use of chemical reagents, making the entire production process more environmentally friendly. Accurate fluorine content detection and aseptic packaging further ensure the high quality and long-term safe storage of krill oil products. Through the process of the present invention, while ensuring the quality of Antarctic krill oil, it is possible to meet the market demand for healthy and low-pollution products, which has important commercial value and social significance. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only for the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0027] Figure 1 This is a schematic diagram of the process for preparing low-fluorine Antarctic krill oil according to an embodiment of the present invention. DETAILED DESCRIPTION

[0028] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0029] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in the present invention should be understood by people with ordinary skills in the field to which the present invention belongs. The "first", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0030] Example 1

[0031] like Figure 1 As shown, a process for preparing low-fluorine Antarctic krill oil comprises the following steps:

[0032] S1: Choose Antarctic krill meal with low fluoride content as raw material, and make sure to use krill meal that has been quality controlled to ensure that its fluoride content is low;

[0033] S2: Grinding or crushing the Antarctic krill powder to ensure the efficiency and uniformity of the extraction process;

[0034] S3: Soaking the Antarctic krill powder in a solution containing calcium ions for defluorination treatment to help remove surface impurities and reduce fluorine content;

[0035] S4: Enzymatic hydrolysis of defluorinated Antarctic krill meal to release oil;

[0036] S5: Using supercritical CO 2 Technology extracts oil from enzymatically hydrolyzed krill;

[0037] S6: The extracted oil is molecularly distilled and refined to remove residual impurities and trace fluorine;

[0038] S7: Test the fluorine content of the refined krill oil to ensure that it meets the predetermined standards;

[0039] S8: Finally, the krill oil that passes the test is aseptically packaged and stored.

[0040] The fluorine content of the Antarctic krill meal selected in S1 does not exceed 1.5 mg / kg.

[0041] The concentration of the calcium ion solution in S3 is 0.3 M, the immersion time is 3 hours, the immersion temperature is 20° C., and stirring is maintained during the period.

[0042] The enzyme used for enzymatic hydrolysis in S4 is protease, the addition amount is 0.75% of the weight of the krill powder, the hydrolysis temperature is 45°C, the pH value is 7.0, and the hydrolysis time is 5 hours.

[0043] S5 Supercritical CO 2 The extraction pressure was 28 MPa, the extraction temperature was 40 °C, the extraction time was 2.5 hours, and the CO 2 The purity is 99.9%.

[0044] The temperature of molecular distillation in S6 was 155°C, the vacuum degree was 0.075 kPa, and the distillation time was 1.5 hours.

[0045] The fluorine content in S7 was detected using high performance liquid chromatography-mass spectrometry (HPLC-MS), and the detected fluorine content was 0.05 mg / kg.

[0046] The packaging material used for aseptic packaging in S8 is high temperature resistant, antioxidant food grade plastic, and the storage temperature is 2°C.

[0047] Example 2

[0048] S1: Antarctic krill powder with a fluorine content of 1 mg / kg is selected as raw material;

[0049] S2: Grinding or crushing the Antarctic krill powder to ensure the efficiency and uniformity of the extraction process;

[0050] S3: soaking the Antarctic krill powder in a 0.1 M calcium ion solution for 2 hours at a temperature of 15°C, and keeping stirring;

[0051] S4: adding 0.5% protease for enzymatic hydrolysis at a hydrolysis temperature of 45°C, the hydrolysis temperature is 40°C, the pH value is controlled at 6.5, and the hydrolysis time is 4 hours;

[0052] S5: Supercritical CO using a pressure of 25 MPa and a temperature of 35 °C 2 Extraction, extraction time is 2 hours;

[0053] S6: molecular distilling the extracted oil and fat, refining at a temperature of 150° C. and a vacuum degree of 0.05 kPa, and the distillation time is 1 hour;

[0054] S7: HPLC-MS / MS was used to detect the fluorine content, and the fluorine content was 0.08 mg / kg.

[0055] S8: The krill oil that has passed the test will be aseptically packaged using high-temperature resistant, antioxidant food-grade plastic and stored at 0°C.

[0056] Example 3

[0057] S1: Antarctic krill powder with a fluorine content of 2 mg / kg is selected as raw material;

[0058] S2: Grinding or crushing the Antarctic krill powder to ensure the efficiency and uniformity of the extraction process;

[0059] S3: soaking the Antarctic krill powder in a 0.5M calcium ion solution for 4 hours at a temperature of 25°C, and keeping stirring;

[0060] S4: adding 1% protease for enzymatic hydrolysis at a hydrolysis temperature of 45°C, the hydrolysis temperature is 50°C, the pH value is controlled at 7.5, and the hydrolysis time is 6 hours;

[0061] S5: Supercritical CO using a pressure of 30 MPa and a temperature of 45 °C 2 Extraction, extraction time is 3 hours;

[0062] S6: molecular distilling the extracted oil and fat, refining it at a temperature of 160° C. and a vacuum degree of 0.1 kPa, and the distillation time is 2 hours;

[0063] S7: HPLC-MS / MS was used to detect the fluorine content, and the fluorine content was 0.1 mg / kg.

[0064] S8: The krill oil that has passed the inspection shall be aseptically packaged using high temperature resistant and antioxidant food grade plastic and stored at 5°C.

[0065] Table 1 Comparison of finished product formation parameters

[0066] Compare Projects Example 1 Example 2 Example 3 Fluoride content (mg / kg) 0.05 0.08 0.1 Oil yield (%) 20.5 18.7 17.3 Color (Lab*) 55.2,12.3,5.6 54.8,12.1,5.8 54.5,11.9,5.9 Odor score (1-10) 9 8 7 Oxidation stability (h) 25 20 18 Impurity content (%) 0.02 0.03 0.05

[0067] It can be seen from Table 1 above that Example 1 is superior to the other two examples in terms of fluorine content, oil yield, odor score, oxidation stability and impurity content. Specifically, Example 1 has the lowest fluorine content, which is only 0.05 mg / kg, much lower than Example 2 and Example 3; Example 1 has the highest oil yield, reaching 20.5%, which is significantly higher than Example 2 and Example 3; Example 1 has an odor score of 9, which is better than Example 2 and Example 3; Example 1 has the longest oxidation stability, which is 25 hours, which is better than the other two examples; Example 1 has the lowest impurity content, which is only 0.02%.

[0068] Therefore, Example 1 is the best example, which not only effectively controls the fluorine content, but also significantly improves the yield and quality of oil, and is suitable as a preparation process for low-fluorine Antarctic krill oil.

[0069] The present invention is intended to cover all such substitutions, modifications and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A process for preparing low-fluorine Antarctic krill oil, characterized in that: The following steps are involved: S1: Choose Antarctic krill meal with low fluoride content as raw material, and make sure to use krill meal that has been quality controlled to ensure that its fluoride content is low; S2: Grinding or crushing the Antarctic krill powder to ensure the efficiency and uniformity of the extraction process; S3: Soaking the Antarctic krill powder in a solution containing calcium ions for defluorination treatment to help remove surface impurities and reduce fluorine content; S4: Enzymatic hydrolysis of defluorinated Antarctic krill meal to release oil; S5: Extracting oil from enzymatically hydrolyzed Antarctic krill powder using supercritical CO2 technology; S6: The extracted oil is molecularly distilled and refined to remove residual impurities and trace fluorine; S7: Test the fluorine content of the refined krill oil to ensure that it meets the predetermined standards; S8: Finally, the krill oil that passes the test is aseptically packaged and stored.

2. A process for preparing low-fluorine Antarctic krill oil according to claim 1, characterized in that: The fluorine content of the Antarctic krill powder selected in S1 does not exceed 2 mg / kg.

3. A process for preparing low-fluorine Antarctic krill oil according to claim 1, characterized in that: The concentration of the calcium ion solution in S3 is 0.1M to 0.5M, the soaking time is 2 to 4 hours, the soaking temperature is 15°C to 25°C, and stirring is maintained during the soaking.

4. A process for preparing low-fluorine Antarctic krill oil according to claim 1, characterized in that: The enzyme used for enzymatic hydrolysis in S4 is protease, the addition amount is 0.5% to 1% of the weight of the krill powder, the hydrolysis temperature is 40° C. to 50° C., the pH value is 6.5 to 7.5, and the hydrolysis time is 4 to 6 hours.

5. A process for preparing low-fluorine Antarctic krill oil according to claim 1, characterized in that: The pressure of the supercritical CO2 extraction in S5 is 25MPa to 30MPa, the extraction temperature is 35°C to 45°C, the extraction time is 2 to 3 hours, and the CO2 purity is 99.9%.

6. A process for preparing low-fluorine Antarctic krill oil according to claim 1, characterized in that: The temperature of the molecular distillation in S6 is 150° C. to 160° C., the vacuum degree is 0.05 kPa to 0.1 kPa, and the distillation time is 1 to 2 hours.

7. A process for preparing low-fluorine Antarctic krill oil according to claim 1, characterized in that: The fluorine content in the S7 is detected using high performance liquid chromatography-mass spectrometry technology, and the standard for the detected fluorine content is less than 0.1 mg / kg.

8. A process for preparing low-fluorine Antarctic krill oil according to claim 1, characterized in that: The packaging material used for aseptic packaging in S8 is high temperature resistant and antioxidant food grade plastic, and the storage temperature is 0°C to 5°C.

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