A preparation method of high-quality capsanthin with a high light absorption ratio

Abstract

The present invention discloses a preparation method of high-quality capsanthin with a high absorbance ratio, which comprises the following steps: crushing ordinary pigment peppers to obtain crushed pepper powder and mixing it with an adsorbent; the adsorbent is a mixture of bentonite and attapulgite; adjusting the water content of the mixture and the ring film ratio of the granulation equipment, and granulating the mixture; putting the granulated particles into an extraction tank, adding an extraction solvent, leaching and extracting, and after the solvent mixed oil is filtered by a filter, performing vacuum concentration to obtain high-quality capsanthin with an absorbance ratio greater than 1 and a centrifugal precipitate less than 2%. The particles after extraction are replaced with a solvent for secondary extraction to obtain capsanthin with a low absorbance ratio. The preparation method disclosed by the present invention avoids the solvent pollution and secondary loss caused by producing capsanthin with a high absorbance ratio on the basis of ordinary capsanthin; the process is simple and feasible, the yield of capsanthin is high, and the obtained capsanthin with a high absorbance ratio has good stability and low pectin and phospholipid contents.

Description

Technical Field

[0001] The present invention relates to the field of capsanthin extraction, and particularly to a method for preparing high-quality capsanthin with a high absorbance ratio. Background Art

[0002] Capsanthin is a natural pigment extracted from peppers. It has bright color, strong coloring power and high safety. The key index affecting the bright color of capsanthin is the red-yellow ratio, that is, the absorbance ratio. The higher the absorbance ratio, the more red pigment it contains and the brighter the color; the lower the absorbance ratio, the more yellow pigment it contains and the darker the color. At present, the absorbance ratio of mainstream capsanthin products on the market is between 0.975 and 0.985, while high-absorbance capsanthin requires an absorbance ratio > 1.000. The capsanthin produced by conventional production has a high pectin content and poor fluidity, and the centrifugal precipitate is generally above 5%. The centrifugal precipitate of capsanthin used as a high-quality food additive on the market is required to be less than 2%.

[0003] The conventional production process of high-quality and high-absorbance capsanthin in the industry requires specific pepper varieties and subcritical extraction methods, and this production has extremely high requirements for raw materials and extraction equipment. And due to the problems of pectin content and centrifugal precipitate, the directly extracted capsanthin usually needs to be subjected to hydration degumming treatment to meet the requirements of high-quality capsanthin. Patent CN109181353 "A Method for Improving the Absorbance Ratio of Capsanthin" discloses a method for achieving the purpose of improving the absorbance ratio by introducing a mixed gas into the finished capsanthin. This method has a long preparation time because the introduction of oxygen makes capsanthin more prone to oxidation, affecting the quality such as the acid value of the product. Patent CN112029312 "A Method for Preparing High-Absorbance Capsanthin and High-Content Capsorubin" discloses a method for separating high-absorbance capsanthin and high-content capsorubin by dissolving-adsorbing-desorbing the capsanthin finished product. This method dissolves the finished product twice and requires a large amount of solvents and adsorbents. During the process of concentrating and removing the solvent, a part of the capsanthin will be oxidized and decomposed at high temperature. At the same time, a large amount of powdery clay has extremely high requirements for the filtration equipment, and unclean filtration will have an adverse impact on the final product. Summary of the Invention

[0004] To solve the above technical problems, the present invention provides a method for preparing high-quality capsanthin with a high absorbance ratio, which has a simple process, does not require additional equipment, reduces the dissolution of pectin by the solvent while producing high-absorbance capsanthin, and the obtained product has a low pectin content and low phospholipids and does not require degumming treatment.

[0005] To achieve the above object, the technical solution of the present invention is as follows:

[0006] A method for preparing high-quality capsanthin with a high absorbance ratio, comprising the following steps:

[0007] (1) Crush ordinary pigment peppers to obtain chili powder, and mix the chili powder with an adsorbent in a certain proportion; the adsorbent is a mixture of bentonite and attapulgite;

[0008] (2) Adjust the water content of the mixture and the ring film ratio of the granulation equipment, and granulate the mixture;

[0009] (3) Put the granulated particles into an extraction tank, add an extraction solvent, and carry out leaching extraction at a certain temperature. After the solvent mixed oil is filtered by a filter, it is concentrated under reduced pressure to obtain high-quality chili red pigment with an absorbance ratio greater than 1 and a centrifugal precipitate less than 2%.

[0010] In a further technical solution, after obtaining the high-quality chili red pigment with a high absorbance ratio, continue to add acetone to the extraction tank, carry out leaching extraction at a certain temperature, and after the solvent mixed oil is filtered by a filter, it is concentrated under reduced pressure to obtain chili red pigment with a low absorbance ratio.

[0011] In the above solution, the ratio of bentonite to attapulgite is 5:1 - 1:1.

[0012] In the above solution, the ratio of chili powder to the adsorbent is 10:1 - 20:1.

[0013] In the above solution, adjust the water content of the mixture to 9% - 13%, and the ring film ratio to 1:6 - 1:8.

[0014] In the above solution, in step (3), the extraction solvent is one of ethyl acetate and hexane.

[0015] In the above solution, in step (3), the dosage of the extraction solvent is 8 - 10 times the mass of the particles, the extraction temperature is 35°C - 45°C, and the extraction time is 4 - 6 hours.

[0016] In the above solution, the dosage of acetone is 6 - 8 times the mass of the particles, the extraction temperature is 45°C - 55°C, and the extraction time is 4 - 6 hours.

[0017] In the above solution, the ordinary pigment peppers are peppers used for industrial extraction of chili red, with an absorbance ratio of 0.980 - 0.985 and a color value of 14 - 23.

[0018] Through the above technical solution, a preparation method of a high-quality chili red pigment with a high absorbance ratio provided by the present invention has the following

[0019] Beneficial effects:

[0020] 1. The method of the present invention is simple and easy to implement. The overall process flow is: crushing - granulation - extraction - refining, which is the same as the ordinary chili red production equipment in the current industry, and no equipment modification or addition is required.

[0021] 2. The chili raw material used in the method of the present invention is ordinary pigment chili, which is simple and easy to obtain and is the current mainstream planting variety. The light absorption ratio of this pigment chili is 0.980 - 0.985, and the light absorption ratio of chili red obtained by normal process extraction is 0.975 - 0.980. The light absorption ratio of chili red obtained by the technology of the present invention is greater than 1.000, and the centrifugal precipitate is less than 2%.

[0022] 3. The method of the present invention can directly obtain high light absorption ratio products from ordinary light absorption ratio particles without the need for secondary treatment on the basis of ordinary chili red products, avoiding the color value loss and hidden pollution risks of secondary treatment. Moreover, the obtained product has less pectin, low precipitate, and low phospholipid content, and does not require degumming treatment, meeting the requirements of high-end products.

[0023] 4. The method of the present invention concentrates yellow pigments and a large amount of pectin impurities into low light absorption ratio chili red through secondary extraction with acetone. The secondary extraction improves the overall color value yield, and the obtained low color value product meets the feed-grade chili red standard and meets the food-grade standard after further degumming treatment. Specific Embodiments

[0024] The technical solutions in the embodiments of the present invention will be clearly and completely described below.

[0025] The quality indicators of chili red pigment include color value, light absorption ratio, and centrifugal precipitate. The method for determining color value is in accordance with GB1886.34 - 2015. The method for measuring light absorption ratio is the same as the pretreatment method before color value measurement, and the result is the ratio of the absorbance at 470 nm wavelength to the absorbance at 454 nm wavelength. The method for measuring centrifugal precipitate is as follows: Weigh a certain mass of chili red pigment into a centrifuge tube, centrifuge at 4000 rpm for 10 minutes, invert the centrifuge tube for 30 min, and the ratio of the mass of the residue at the bottom to the sample weight is the centrifugal precipitate.

[0026] Example 1:

[0027] Crush the ordinary pigment chili Honglong 23. The measured color value of the crushed chili powder is E17.2, and the light absorption ratio is 0.982. Take 500 kg of chili powder and mix it with 15 kg of bentonite and 15 kg of attapulgite. The water content of the mixed powder is 12%. Adjust the granulation ring film ratio to 1:8 to granulate the mixed powder. Put the obtained granules into the extraction tank, and introduce 1.5 m of ethyl acetate from above 3 , keep the temperature of the extraction tank at 45 °C, stir for 2 hours, then release the solvent into the evaporation system, and introduce new ethyl acetate to repeat the extraction twice. A total of 4.5 m of ethyl acetate is used 3, the extraction time is 6 hours. The evaporation temperature is 55°C, and the solvent residue is removed under a vacuum of -0.06 MPa. Ethyl acetate is recovered to obtain 27 kg of high-quality high-absorbance capsanthin with a color value of E258 and an absorbance ratio of 1.009. The centrifugal precipitate is 1.2%, and the yield is 81%;

[0028] Continue to introduce 1.5 m 3 of acetone into the extraction tank, keep the temperature of the extraction tank at 50°C, stir for 2 hours, then discharge the solvent into the evaporation system, and repeat the extraction once. A total of 3 m 3 of acetone is used. The extraction time is 4 hours. The evaporation temperature is 55°C, and the solvent residue is removed under a vacuum of -0.06 MPa. Acetone is recovered to obtain 19.4 kg of low-absorbance capsanthin with a color value of E69 and an absorbance ratio of 0.930. The yield is 15.5%.

[0029] Example 2:

[0030] Mix 500 kg of the same chili powder as in Example 1 with 40 kg of bentonite and 10 kg of attapulgite. The water content of the mixed powder is 11.6%. Adjust the granulation ring film ratio to 1:8 to granulate the mixed powder. Put the obtained granules into the extraction tank, and introduce 1.5 m 3 of ethyl acetate from above. Keep the temperature of the extraction tank at 40°C, stir for 2 hours, then discharge the solvent into the evaporation system, and repeat the extraction twice by introducing new ethyl acetate. A total of 4.5 m 3 of ethyl acetate is used. The extraction time is 6 hours. The evaporation temperature is 55°C, and the solvent residue is removed under a vacuum of -0.06 MPa. Ethyl acetate is recovered to obtain 25.6 kg of high-quality high-absorbance capsanthin with a color value of E239 and an absorbance ratio of 1.022. The centrifugal precipitate is 1.6%, and the yield is 71%;

[0031] Continue to introduce 1.5 m 3 of acetone into the extraction tank, keep the temperature of the extraction tank at 50°C, stir for 2 hours, then discharge the solvent into the evaporation system, and repeat the extraction once. A total of 3 m 3 of acetone is used. The extraction time is 4 hours. The evaporation temperature is 55°C, and the solvent residue is removed under a vacuum of -0.06 MPa. Acetone is recovered to obtain 23.2 kg of low-absorbance capsanthin with a color value of E77 and an absorbance ratio of 0.922. The yield is 20.7%.

[0032] Example 3:

[0033] Another batch of ordinary pigmented pepper red dragon 23 was pulverized, and the color value of the pulverized pepper powder was measured as E16.7 and the absorbance ratio was 0.985. 500 kg of pepper powder was taken and mixed with 20 kg of bentonite and 20 kg of attapulgite. The water content of the mixed powder was 10.1%. The granulation ring film ratio was adjusted to 1:6 to granulate the mixed powder. The obtained granules were put into an extraction tank, and 1.5 m of hexane was introduced from above 3 , the temperature of the extraction tank was maintained at 45 °C, and after stirring for 2 hours, the solvent was discharged into the evaporation system, and new hexane was introduced to repeat the extraction twice. A total of 4.5 m of hexane was used 3 , and the extraction time was 6 hours. The evaporation temperature was 55 °C, and the solvent residue was removed under a vacuum of -0.06 MPa to recover hexane, obtaining 23.4 kg of high-quality high-absorbance ratio capsanthin with a color value of E277 and an absorbance ratio of 1.015. The centrifugal precipitate was 1.1%, and the yield was 77.6%;

[0034] Continue to introduce 1.5 m of 3 acetone into the extraction tank, maintain the temperature of the extraction tank at 50 °C, and after stirring for 2 hours, discharge the solvent into the evaporation system and repeat the extraction once. A total of 3 m of acetone was used 3 , and the extraction time was 4 hours. The evaporation temperature was 55 °C, and the solvent residue was removed under a vacuum of -0.06 MPa to recover acetone, obtaining 28 kg of capsanthin with a low absorbance ratio with a color value of E55 and an absorbance ratio of 0.926, and the yield was 18.4%.

[0035] Comparative Example 1:

[0036] Comparative Example 1 was a comparative test of Example 1, the difference being the ratio of pepper powder to adsorbent. Comparative Example 1 was 500 kg of pepper powder, 10 kg of bentonite, and 10 kg of attapulgite; the other conditions were exactly the same as those in Example 1. The result was that the absorbance ratio of the high-quality high-absorbance ratio capsanthin in Comparative Example 1 was 0.995. It shows that too little adsorbent dosage cannot obtain high-quality high-absorbance ratio capsanthin with an absorbance ratio greater than 1.000.

[0037] Comparative Example 2:

[0038] Comparative Example 2 was a comparative test of Example 2, the difference being the ratio of pepper powder to adsorbent. Comparative Example 2 was 500 kg of pepper powder, 30 kg of bentonite, and 30 kg of attapulgite; the other conditions were exactly the same as those in Example 2. The result was that the absorbance ratio of the high-quality high-absorbance ratio capsanthin in Comparative Example 2 was 1.026, but the yield of the high-quality high-absorbance ratio capsanthin was only 56%, and the yield of the low-absorbance ratio capsanthin obtained by secondary extraction was 17%. It shows that the improvement of the adsorbent on the absorbance ratio is limited. Too large an adsorbent ratio will interfere with the dissolution of the pigment by the solvent, resulting in incomplete extraction of the pigment and affecting the yield.

[0039] Comparative Example 3:

[0040] Comparative Example 3 was a comparative test of Example 3, with the difference that 40 kg of bentonite was used as the adsorbent; the remaining conditions were exactly the same as those in Example 3. The result was that 36 kg of high-quality and high light absorption ratio capsanthin was obtained in Comparative Example 3, with a color value of E192, a light absorption ratio of 1.018, and a centrifugal precipitate of 6.8%. It shows that bentonite mainly adsorbs pigments and has no adsorption effect on pectin substances. Therefore, pectin substances are extracted, the centrifugal precipitate is high, and the pigment quality decreases.

[0041] Comparative Example 4:

[0042] Comparative Example 4 was a comparative test of Example 3, with the difference that 40 kg of attapulgite was used as the adsorbent; the remaining conditions were exactly the same as those in Example 3. The result was that the light absorption ratio of the high-quality and high light absorption ratio capsanthin in Comparative Example 4 was 0.985, and the centrifugal precipitate was 0.6%. The pigment had less pectin content and good fluidity, indicating that attapulgite mainly has an adsorption effect on pectin substances.

[0043] Comparative Example 5:

[0044] Comparative Example 5 was a comparative test of Example 3, with the difference that 10 kg of bentonite and 30 kg of attapulgite were used as the adsorbents; the remaining conditions were exactly the same as those in Example 3. The result was that the light absorption ratio of the high-quality and high light absorption ratio capsanthin in Comparative Example 5 was 0.998, indicating that the insufficient addition ratio of bentonite limited the increase in the light absorption ratio.

[0045] Comparative Example 6:

[0046] Comparative Example 6 was a comparative test of Example 3, with the difference that 35 kg of bentonite and 5 kg of attapulgite were used as the adsorbents; the remaining conditions were exactly the same as those in Example 3. The result was that the light absorption ratio of the high-quality and high light absorption ratio capsanthin in Comparative Example 6 was 1.012, and the centrifugal precipitate was 2.8%. It shows that the insufficient addition amount of attapulgite affects pectin adsorption, resulting in more colloid in the extracted pigment and a higher centrifugal precipitate.

[0047] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be obvious to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to these embodiments shown herein, but rather to the broadest scope consistent with the principles and novel features disclosed herein.

Claims

1. A preparation method of high-quality capsanthin with a high light absorption ratio, characterized in that, It includes the following steps: (1) Crush ordinary pigment peppers to obtain chili powder, and mix it with an adsorbent in a certain proportion; the adsorbent is a mixture of bentonite and attapulgite; (2) Adjust the water content of the mixture and the ring film ratio of the granulation equipment, and granulate the mixture; (3) Put the granulated particles into an extraction tank, add an extraction solvent, and carry out leaching extraction at a certain temperature. After the solvent mixed oil is filtered by a filter, it is concentrated under reduced pressure to obtain high-quality chili red pigment with an absorbance ratio greater than 1 and a centrifugal precipitate less than 2%; The ratio of bentonite to attapulgite is 5:1 - 1:1; the ratio of chili powder to the adsorbent is 10:1 - 20:

1.

2. The preparation method of a high-quality capsanthin with a high light absorption ratio according to claim 1, wherein After obtaining the high-quality chili red pigment with a high absorbance ratio, continue to add acetone to the extraction tank, and carry out leaching extraction at a certain temperature. After the solvent mixed oil is filtered by a filter, it is concentrated under reduced pressure to obtain chili red pigment with a low absorbance ratio.

3. The preparation method of a high-quality capsanthin with a high light absorption ratio according to claim 1, characterized in that, Adjust the water content of the mixture to 9% - 13%, and the ring film ratio to 1:6 - 1:

8.

4. The preparation method of a high-quality capsanthin with a high light absorption ratio according to claim 1, characterized in that, In step (3), the extraction solvent is one of ethyl acetate and hexane.

5. The preparation method of a high-quality capsanthin with a high light absorption ratio according to claim 1, characterized in that, In step (3), the dosage of the extraction solvent is 8 - 10 times the mass of the particles, the extraction temperature is 35°C - 45°C, and the extraction time is 4 - 6 hours.

6. The preparation method of a high-quality capsanthin with a high light absorption ratio according to claim 2, characterized in that, The dosage of acetone is 6 - 8 times the mass of the particles, the extraction temperature is 45°C - 55°C, and the extraction time is 4 - 6 hours.

7. The preparation method of a high-quality capsanthin with a high light absorption ratio according to claim 1, characterized in that, The ordinary pigment peppers are peppers used for industrial extraction of chili red, with an absorbance ratio of 0.980 - 0.985 and a color value of 14 - 23.