Method for extracting ricinine from castor bean meal

Abstract

The invention discloses a method for extracting ricinine in castor bean meal, which comprises the following steps: step 1, adding castor bean meal and water into an extraction tank according to a weight ratio of 1: (5-10), setting the temperature to be 100-120 DEG C and the pressure to be 0.1-0.5 Mpa, extracting for 10-15 minutes, and centrifuging to obtain a first centrifugate; 2, adding water with the same weight as that in the step 1 into the precipitate obtained after centrifugation in the step 1, setting the temperature to be 100-120 DEG C and the pressure to be 0.1-0.5 Mpa, extracting for 10-15 minutes, and centrifuging to obtain second centrifugate; and 3, combining the first centrifugate and the second centrifugate, and concentrating into paste to be purified. According to the extraction method disclosed by the invention, continuous twice high-pressure high-temperature water extraction is adopted, the extraction rate is high, rapidness and high efficiency are realized, no organic solvent is left, ricinine can be industrially extracted, and the nutritional value of castor bean meal is not influenced.

Description

Technical Field

[0001] The invention relates to the field of ricin extraction, in particular to a method for extracting ricin from castor meal. Background Art

[0002] Castor (Ricinus communis L.) is a plant of the genus Ricinus in the family Euphorbiaceae and is one of the world's top ten oil crops. Castor meal, a byproduct of castor oil extraction, is rich in crude protein and minerals such as calcium and phosphorus, but also contains many toxic substances, such as toxic proteins, ricinine, allergens, lectins, etc., so removing ricinine from castor meal is of great significance for the application of castor meal. Ricinine, as a natural active alkaloid, also has potential application value, such as being used as a biological pesticide, a liver protectant at low doses, and improving memory. Therefore, the maximum value of castor meal can be brought into play only when ricinine is extracted from castor meal without affecting the safety of castor meal. The main methods for extracting ricinine are: heating extraction (water extraction and alcohol extraction), ultrasonic extraction, and microwave extraction. Zhu Qingli and others found through experiments that ultrasound and microwave assisted in the extraction of ricinine, with an extraction rate of 78.2% and one ethanol recrystallization, with a ricinine purity of 97.7%. Zhao Zenglin used water extraction method, with extraction for 1 hour, water temperature of 95°C, solid-liquid ratio of 1:10, extraction level of 3, and an extraction rate of 99.69%.

[0003] However, the current ricin extraction method, alcohol extraction, is prone to organic solvent residues, and organic solvent treatment is prone to environmental pollution; water extraction takes a long time, is complicated to operate, and requires three extraction stages, which affects the nutritional value of castor meal; ultrasonic, microwave, or ultrasonic-microwave methods are short in time, but have low extraction rates and are not conducive to industrialization. Castor meal has high residual toxins, which is not conducive to the utilization of castor meal. Therefore, in response to the above problems, it is necessary to find a method that is fast, efficient, has no solvent residues, can be industrialized to extract ricin from castor meal, and retains the nutritional value of castor meal. Summary of the invention

[0004] The purpose of the present invention is to provide a method for extracting ricin from castor meal in view of the deficiencies in the prior art.

[0005] To achieve the above object, the technical solution adopted by the present invention is:

[0006] A method for extracting ricin from castor meal is provided, comprising the following steps:

[0007] Step 1: adding castor meal and water in a weight ratio of 1:(5-10) into an extraction tank, setting the temperature to 100-120° C., the pressure to 0.1-0.5 MPa, extracting for 10-15 minutes, centrifuging to obtain a first centrifuge;

[0008] Step 2: Add the same weight of water as in step 1 to the precipitate obtained after centrifugation in step 1, set the temperature to 100-120°C, the pressure to 0.1-0.5Mpa, extract for 10-15min, centrifuge to obtain a second centrifuge liquid;

[0009] Step 3: Combine the first centrifuge liquid and the second centrifuge liquid, and concentrate them into a paste for purification.

[0010] Furthermore, the method for extracting ricinine from castor meal also includes:

[0011] Step 4: Place the paste in a Soxhlet extractor with a non-woven fabric, add petroleum ether, and defat;

[0012] Step 5: After defatting and washing away the fat, add chloroform to extract ricinine, ensure reflux 60 times, and collect the crude ricinine extract;

[0013] Step 6: The crude ricinine extract is completely dissolved in anhydrous ethanol, filtered, and recrystallized until the crystallization is complete;

[0014] Step 7: Centrifuge to obtain the precipitate, and dry at low temperature to obtain ricinine.

[0015] Furthermore, in the step 2, the precipitate obtained by centrifugation is dried and used as a feed raw material.

[0016] Furthermore, in the step 1, the weight ratio of castor meal to water is 1:5.

[0017] Furthermore, in the step 4, the degreasing temperature is 50-60°C.

[0018] Furthermore, in the step five, the extraction temperature is 75-80°C.

[0019] Furthermore, in step six, the recrystallization temperature is -20°C.

[0020] The present invention adopts the above technical solution, and has the following technical effects compared with the prior art:

[0021] The extraction method of the invention adopts two consecutive high-pressure and high-temperature water extractions, has a high extraction rate, is fast and efficient, has no organic solvent residue, can extract ricinine industrially, and does not affect the nutritional value of castor meal. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The present invention is a flow chart of the method for extracting ricinine from castor meal. DETAILED DESCRIPTION

[0023] The present invention is further described below in conjunction with the accompanying drawings and specific embodiments, but is not intended to be limiting of the present invention. It should be noted that the embodiments and features in the embodiments of the present invention may be combined with each other without conflict.

[0024] Example 1

[0025] refer to Figure 1 This embodiment provides a method for extracting ricinine from castor meal, and the specific steps are as follows:

[0026] Step 1: adding castor meal and water in a weight ratio of 1:5 into an extraction tank, setting the temperature to 100° C. and the pressure to 0.1 MPa, extracting for 10 minutes, and centrifuging to obtain a first centrifuge;

[0027] Step 2: Add the same weight of water as in step 1 to the precipitate obtained after centrifugation in step 1, set the temperature to 100°C, the pressure to 0.1 MPa, extract for 10 minutes, centrifuge to obtain a second centrifuge liquid; dry the precipitate obtained by centrifugation as a feed raw material;

[0028] Step 3: Combine the first centrifuge liquid and the second centrifuge liquid and concentrate them into a paste;

[0029] Step 4: Place the paste in a Soxhlet extractor with a non-woven fabric, add petroleum ether, and degrease at 50°C;

[0030] Step 5: After defatting and washing away the fat, add chloroform, extract ricinine at 80°C, ensure reflux 60 times, and collect the crude ricinine extract;

[0031] Step 6: The crude ricinine extract is completely dissolved in anhydrous ethanol, filtered, and then placed in a -20°C refrigerator for recrystallization until the crystallization is complete;

[0032] Step 7: Centrifuge to obtain the precipitate, and dry at low temperature to obtain ricinine.

[0033] In the present invention, ricinine is determined by a liquid chromatograph, the liquid chromatograph is UltiMate3000 of Thermo Fisher Scientific, the detection conditions are: UV detector, wavelength 308nm, column temperature 30°C, mobile phase: acetonitrile: water = 1:10, flow rate 1mL / min, injection volume 10μL. The specific method is a conventional technical means in the art, and the present invention will not make too many descriptions.

[0034] In this embodiment, the extraction rate of ricinine is 98.65%, and the purity of ricinine is 96.5%.

[0035] Comparative Example 1

[0036] The difference from Example 1 is that the weight ratio of castor meal to water in this comparative example is 1:3.

[0037] In this comparative example, the extraction rate of ricinine is 72.54%, and the purity of ricinine is 87.1%.

[0038] It can be seen that a higher solid-liquid ratio leads to a higher extraction rate.

[0039] Comparative Example 2

[0040] The difference from Example 1 is that the comparative example only uses one high temperature and high pressure heat extraction, specifically:

[0041] Step 1: Add castor meal and water in a weight ratio of 1:5 into an extraction tank, set the temperature to 100°C, the pressure to 0.1Mpa, extract for 10 minutes, centrifuge to obtain a centrifuge;

[0042] Step 2: Concentrate the centrifuge liquid to a paste;

[0043] Step 3: Place the paste in a Soxhlet extractor with a non-woven fabric, add petroleum ether, and degrease at 50°C;

[0044] Step 4: After defatting and washing away the fat, add chloroform, extract ricinine at 80°C, ensure reflux 60 times, and collect the crude ricinine extract;

[0045] Step 5: The crude ricinine extract is completely dissolved in anhydrous ethanol, filtered, and then placed in a -20°C refrigerator for recrystallization until the crystallization is complete;

[0046] Step 6: Centrifuge to obtain the precipitate, and dry at low temperature to obtain ricinine.

[0047] In this embodiment, the extraction rate of ricinine is 79.61%, and the purity of ricinine is 90.12%.

[0048] Example 2

[0049] The difference from Example 1 is that in step 1 and step 2, the extraction temperature is set to 110° C. and the extraction time is set to 15 min.

[0050] In this embodiment, the extraction rate of ricinine is 99.78%, and the purity of ricinine is 99.0%.

[0051] Example 3

[0052] The difference from Example 1 is that in step 1 and step 2, the extraction temperature is set to 120°C.

[0053] In this embodiment, the extraction rate of ricinine is 99.68%, and the purity of ricinine is 99.02%.

[0054] The above description is only a preferred embodiment of the present invention, and does not limit the implementation mode and protection scope of the present invention. For those skilled in the art, it should be aware that all solutions obtained by equivalent substitutions and obvious changes made using the contents of the specification and illustrations of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for extracting ricinine from castor meal, characterized in that: The steps include: Step 1: adding castor meal and water in a weight ratio of 1:(5-10) into an extraction tank, setting the temperature to 100-120° C., the pressure to 0.1-0.5 MPa, extracting for 10-15 minutes, centrifuging to obtain a first centrifuge; Step 2: Add the same weight of water as in step 1 to the precipitate obtained after centrifugation in step 1, set the temperature to 100-120°C, the pressure to 0.1-0.5Mpa, extract for 10-15min, centrifuge to obtain a second centrifuge liquid; Step 3: Combine the first centrifuge liquid and the second centrifuge liquid, and concentrate them into a paste for purification.

2. The method for extracting ricinine from castor meal according to claim 1, characterized in that: Also includes: Step 4: Place the paste in a Soxhlet extractor with a non-woven fabric, add petroleum ether, and defat; Step 5: After defatting and washing away the fat, add chloroform to extract ricinine, ensure reflux 60 times, and collect the crude ricinine extract; Step 6: The crude ricinine extract is completely dissolved in anhydrous ethanol, filtered, and recrystallized until the crystallization is complete; Step 7: Centrifuge to obtain the precipitate, and dry at low temperature to obtain ricinine.

3. The method for extracting ricinine from castor meal according to claim 1, characterized in that: In the step 2, the precipitate obtained by centrifugation is dried and used as a feed raw material.

4. The method for extracting ricinine from castor meal according to claim 1, characterized in that: In the step 1, the weight ratio of castor meal to water is 1:

5.

5. The method for extracting ricinine from castor meal according to claim 2, characterized in that: In the step 4, the degreasing temperature is 50-60°C.

6. The method for extracting ricinine from castor meal according to claim 2, characterized in that: In the step 5, the extraction temperature is 75-80°C.

7. The method for extracting ricinine from castor meal according to claim 2, characterized in that: In the step six, the recrystallization temperature is -20°C.

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