Disclosure of Invention
According to the technical problems, the invention provides an ophiopogon root pet feed additive with a hair beautifying effect, which is characterized in that: the material is prepared by mixing the following raw materials in parts by weight:
35-150 parts of ophiopogon root plant extract, 40-140 parts of liriope spicata plant extract and 0.5-1.5 parts of ophiopogon root bioactive component.
The preparation method of the ophiopogon japonicus plant extract comprises the following steps:
a. drying and crushing tuber of dwarf lilyturf tuber, sieving the tuber of dwarf lilyturf tuber by a 150-mesh standard sieve, adding the powder into water with 25-30 times of volume after sieving, and then performing ultrasonic extraction in mixed liquid, wherein the sound wave power for ultrasonic extraction is 200-500W, the ultrasonic temperature is 30-60 ℃, and the ultrasonic extraction time is 10-60 min; performing pH measurement on the liquid after ultrasonic extraction, performing pH adjustment after measurement, adjusting to 3-6, then respectively adding cellulase, pectinase and papain in a certain enzyme adding sequence at the temperature of 30-60 ℃, performing enzymolysis for 40-100min, cooling, performing suction filtration to obtain an extracting solution, performing vacuum concentration on the extracting solution to 30% of the original volume, centrifuging to obtain a supernatant and a precipitate, extracting the supernatant for 3 times by using equal volume of ethyl acetate, recovering water phase liquid, combining ethyl acetate phase liquid, and performing rotary evaporation to recover ethyl acetate to obtain an ophiopogon japonicus ethyl acetate extract;
b. taking the water phase liquid recovered after extraction in the step a, concentrating the water phase liquid in vacuum to 30% of the original volume, centrifuging to obtain a supernatant and a precipitate, adding 5 times of absolute ethyl alcohol into the supernatant, standing overnight, performing suction filtration to obtain the precipitate, washing the precipitate for 3 times by using the absolute ethyl alcohol and acetone in sequence, and performing vacuum freeze-drying on the precipitate to obtain a radix ophiopogonis water extract;
c. and uniformly mixing the ethyl acetate extract of the dwarf lilyturf tuber and the water extract of the dwarf lilyturf tuber to obtain the dwarf lilyturf tuber plant extract.
The preparation method of the liriope spicata plant extract comprises the following steps:
a. drying and crushing tuber of liriope spicata, sieving the crushed tuber of liriope spicata through a 150-mesh standard sieve, adding the powder into water with the volume of 25-30 times of the tuber of liriope spicata, and then performing ultrasonic extraction in mixed liquid, wherein the ultrasonic extraction is performed at the ultrasonic power of 200-500W and the ultrasonic temperature of 30-60 ℃ for 10-60 min; performing pH measurement on the liquid after ultrasonic extraction, adjusting the pH to 3-6 by using NaOH or HCl solution after the pH measurement, performing enzymolysis on the liquid for 40-100min by using cellulase, pectinase and papain which are added according to a certain enzyme adding sequence at the temperature of 30-60 ℃, cooling and performing suction filtration to obtain an extracting solution, performing vacuum concentration on the extracting solution to 30% of the original volume, centrifuging to obtain a supernatant and a precipitate, extracting the supernatant for 3 times by using ethyl acetate with the same volume, recovering water phase liquid, combining ethyl acetate phase liquid, and performing rotary evaporation to recover ethyl acetate to obtain an ophiopogon japonicus ethyl acetate extract;
b. taking the water phase liquid recovered after extraction in the step a, concentrating the water phase liquid in vacuum to 30% of the original volume, centrifuging to obtain a supernatant and a precipitate, adding 5 times of absolute ethyl alcohol into the supernatant, standing overnight, performing suction filtration to obtain the precipitate, washing the precipitate for 3 times by using the absolute ethyl alcohol and acetone in sequence, and performing vacuum freeze-drying on the precipitate to obtain a liriope spicata water extract;
c. and (3) uniformly mixing the ethyl acetate extract of the liriope spicata and the water extract of the liriope spicata to obtain the liriope spicata plant extract.
The preparation method of the radix ophiopogonis bioactive component comprises the following steps:
dissolving equal amounts of Ophiopogon D powder, Liriope muscarib saponin C powder and Methylphosphinonene A powder in ultrapure water, and spray drying at an air inlet temperature of 160 deg.C and an air outlet temperature of 110 deg.C to obtain radix Ophiopogonis bioactive components.
The enzyme adding sequence is as follows: pectinase → cellulase → papain, the enzyme dosage is 0.4-1.3%, and the conditions of pectinase enzymolysis are as follows: pH 3.4, temperature 52 deg.C, time 34min, enzyme adding amount 0.42%; the conditions of the enzymolysis of the cellulase are as follows: pH 3.8, temperature 34 deg.C, time 37min, enzyme adding amount 0.47%; the enzymolysis conditions of the papain are as follows: pH5.7, temperature 35 deg.C, time 51min, enzyme addition 0.54%.
The adding proportion of the dwarf lilyturf tuber pet feed additive is 0.3-1.5 percent of the total weight of the premix or the batch.
The invention adopts the traditional Chinese medicinal materials of the dwarf lilyturf tuber and the liriope spicata and the extracts thereof as raw materials, can fundamentally meet the hair beautifying requirement of animals, has considerable market prospect, and can play a role in promoting the industrial development of the dwarf lilyturf tuber and the liriope spicata. The invention has simple required equipment and low medicine price, and can realize quick production and quick income. The preparation method has the characteristics of simple preparation process, short production time, less generated wastewater, less environmental pollution and the like. The invention is rich in bioactive components such as polysaccharide, ophiopogonin, ophiopogonone and the like, and can play roles of regulating immunity, promoting growth and the like while beautifying animal hair. The radix ophiopogonis pet feed additive can be added into conventional premix or batch for pets or economic animals, so that the invention also provides the premix or batch containing the radix ophiopogonis pet feed additive.
Detailed Description
The invention is further illustrated by the examples:
ophiogonin D is Ophiopogonin D, Liriope muscaribaily saponin C is Liriope muscari saponin C, and Methylphosphinone A is Liriope muscari dihydrohomoisoflavone A.
Example 1:
the preparation method of the ophiopogon japonicus plant extract, the liriope spicata plant extract and the ophiopogon japonicus bioactive component comprises the following steps:
a. drying tuber of radix Ophiopogonis, pulverizing, sieving with 150 mesh standard sieve, adding into 25-30 times of water, and ultrasonic extracting at 55 deg.C under ultrasonic power of 300W for 43 min; and (4) performing enzymatic extraction on the material liquid mixture after ultrasonic treatment according to the enzyme adding sequence of pectinase → cellulase → papain. Adjusting pH to 3.4, heating to 52 deg.C, adding 0.42% cellulase, and performing enzymolysis for 34 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 3.8 at 34 deg.C, adding 0.47% cellulase, and performing enzymolysis for 37 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 5.7, adjusting temperature to 35 deg.C, adding 0.54% papain for enzymolysis for 51min, and inactivating enzyme in boiling water bath for 5 min. Cooling the mixture, and vacuum filtering to obtain extractive solution. Concentrating the extractive solution in vacuum to 30% of the original volume, and centrifuging to obtain supernatant and precipitate. Extracting the supernatant with equal volume of ethyl acetate for 3 times, mixing the extractive solutions, recovering water phase liquid, and mixing the ethyl acetate phase liquids. And (4) carrying out rotary evaporation on the ethyl acetate phase liquid to recover ethyl acetate to obtain the ethyl acetate extract of the radix ophiopogonis.
b. And (b) combining the recovered aqueous phase liquid after extraction in the step a, concentrating the aqueous phase liquid in vacuum to 30% of the original volume, and centrifuging to obtain a supernatant and a precipitate. And adding 5 times of volume of absolute ethyl alcohol into the supernatant, standing overnight, and performing suction filtration to obtain a precipitate. Washing the precipitate with anhydrous alcohol and acetone for 3 times, and vacuum lyophilizing the precipitate to obtain radix Ophiopogonis water extract.
c. And uniformly mixing the ethyl acetate extract of the dwarf lilyturf tuber and the water extract of the dwarf lilyturf tuber to obtain the dwarf lilyturf tuber plant extract.
The preparation method of the liriope spicata plant extract comprises the following steps:
a. drying tuber of liriope spicata, pulverizing, sieving with 150 mesh standard sieve, adding into 25-30 times of water, and ultrasonic extracting at 55 deg.C under ultrasonic power of 300W for 43 min; and (4) performing enzymatic extraction on the material liquid mixture after ultrasonic treatment according to the enzyme adding sequence of pectinase → cellulase → papain. Adjusting pH to 3.4, heating to 52 deg.C, adding 0.42% cellulase, and performing enzymolysis for 34 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 3.8 at 34 deg.C, adding 0.47% cellulase, and performing enzymolysis for 37 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 5.7, adjusting temperature to 35 deg.C, adding 0.54% papain for enzymolysis for 51min, and inactivating enzyme in boiling water bath for 5 min. Cooling the mixture, and vacuum filtering to obtain extractive solution. Concentrating the extractive solution in vacuum to 30% of the original volume, and centrifuging to obtain supernatant and precipitate. Extracting the supernatant with equal volume of ethyl acetate for 3 times, mixing the extractive solutions, recovering water phase liquid, and mixing the ethyl acetate phase liquids. And (4) carrying out rotary evaporation on the ethyl acetate phase liquid to recover ethyl acetate to obtain the liriope spicata ethyl acetate extract.
b. And (b) taking the water phase liquid recovered after extraction in the step a, concentrating the water phase liquid in vacuum to 30% of the original volume, and centrifuging to obtain a supernatant and a precipitate. And adding 5 times of volume of absolute ethyl alcohol into the supernatant, standing overnight, and performing suction filtration to obtain a precipitate. Washing the precipitate with anhydrous alcohol and acetone for 3 times, and vacuum lyophilizing the precipitate to obtain radix liriopes extract.
c. And (3) uniformly mixing the ethyl acetate extract of the liriope spicata and the water extract of the liriope spicata to obtain the liriope spicata plant extract.
The preparation method of the radix ophiopogonis bioactive component comprises the following steps:
dissolving equal amounts of Ophiopogon D powder, Liriope muscarib saponin C powder and Methylphosphinonene A powder in ultrapure water, and spray drying at an air inlet temperature of 160 deg.C and an air outlet temperature of 110 deg.C to obtain radix Ophiopogonis bioactive components.
Selecting the produced raw materials, selecting the ophiopogon root plant extract, the liriope spicata plant extract and the ophiopogon root bioactive component according to the ratio of 136: 123: 1, mixing the selected raw materials after the selection is finished, and preparing the additive. When in use, the prepared additive is put into pet feed, and the adding proportion of the additive is 0.5 percent of the total amount of the feed.
Example 2:
the preparation method of the ophiopogon japonicus plant extract, the liriope spicata plant extract and the ophiopogon japonicus bioactive component comprises the following steps:
a. drying tuber of radix Ophiopogonis, pulverizing, sieving with 150 mesh standard sieve, adding into 25-30 times of water, and ultrasonic extracting at 55 deg.C under ultrasonic power of 300W for 43 min; and (4) performing enzymatic extraction on the material liquid mixture after ultrasonic treatment according to the enzyme adding sequence of pectinase → cellulase → papain. Adjusting pH to 3.4, heating to 52 deg.C, adding 0.42% cellulase, and performing enzymolysis for 34 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 3.8 at 34 deg.C, adding 0.47% cellulase, and performing enzymolysis for 37 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 5.7, adjusting temperature to 35 deg.C, adding 0.54% papain for enzymolysis for 51min, and inactivating enzyme in boiling water bath for 5 min. Cooling the mixture, and vacuum filtering to obtain extractive solution. Concentrating the extractive solution in vacuum to 30% of the original volume, and centrifuging to obtain supernatant and precipitate. Extracting the supernatant with equal volume of ethyl acetate for 3 times, mixing the extractive solutions, recovering water phase liquid, and mixing the ethyl acetate phase liquids. And (4) carrying out rotary evaporation on the ethyl acetate phase liquid to recover ethyl acetate to obtain the ethyl acetate extract of the radix ophiopogonis.
b. And (b) combining the recovered aqueous phase liquid after extraction in the step a, concentrating the aqueous phase liquid in vacuum to 30% of the original volume, and centrifuging to obtain a supernatant and a precipitate. And adding 5 times of volume of absolute ethyl alcohol into the supernatant, standing overnight, and performing suction filtration to obtain a precipitate. Washing the precipitate with anhydrous alcohol and acetone for 3 times, and vacuum lyophilizing the precipitate to obtain radix Ophiopogonis water extract.
c. And uniformly mixing the ethyl acetate extract of the dwarf lilyturf tuber and the water extract of the dwarf lilyturf tuber to obtain the dwarf lilyturf tuber plant extract.
The preparation method of the liriope spicata plant extract comprises the following steps:
a. drying tuber of liriope spicata, pulverizing, sieving with 150 mesh standard sieve, adding into 25-30 times of water, and ultrasonic extracting at 55 deg.C under ultrasonic power of 300W for 43 min; and (4) performing enzymatic extraction on the material liquid mixture after ultrasonic treatment according to the enzyme adding sequence of pectinase → cellulase → papain. Adjusting pH to 3.4, heating to 52 deg.C, adding 0.42% cellulase, and performing enzymolysis for 34 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 3.8 at 34 deg.C, adding 0.47% cellulase, and performing enzymolysis for 37 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 5.7, adjusting temperature to 35 deg.C, adding 0.54% papain for enzymolysis for 51min, and inactivating enzyme in boiling water bath for 5 min. Cooling the mixture, and vacuum filtering to obtain extractive solution. Concentrating the extractive solution in vacuum to 30% of the original volume, and centrifuging to obtain supernatant and precipitate. Extracting the supernatant with equal volume of ethyl acetate for 3 times, mixing the extractive solutions, recovering water phase liquid, and mixing the ethyl acetate phase liquids. And (4) carrying out rotary evaporation on the ethyl acetate phase liquid to recover ethyl acetate to obtain the liriope spicata ethyl acetate extract.
b. And (b) taking the water phase liquid recovered after extraction in the step a, concentrating the water phase liquid in vacuum to 30% of the original volume, and centrifuging to obtain a supernatant and a precipitate. And adding 5 times of volume of absolute ethyl alcohol into the supernatant, standing overnight, and performing suction filtration to obtain a precipitate. Washing the precipitate with anhydrous alcohol and acetone for 3 times, and vacuum lyophilizing the precipitate to obtain radix liriopes extract.
c. And uniformly mixing the ethyl acetate extract of the radix ophiopogonis and the water extract of the radix ophiopogonis to obtain the liriope spicata plant extract.
The preparation method of the radix ophiopogonis bioactive component comprises the following steps:
dissolving equal amounts of Ophiopogon D powder, Liriope muscarib saponin C powder and Methylphosphinone A powder in ultrapure water, and spray drying at an air inlet temperature of 160 deg.C and an air outlet temperature of 110 deg.C to obtain radix Ophiopogonis bioactive components.
Selecting the produced raw materials, selecting the ophiopogon root plant extract, the liriope spicata plant extract and the ophiopogon root bioactive component according to the ratio of 50: 100: 0.6, mixing the selected raw materials after selection, and preparing the additive. When in use, the prepared additive is put into pet feed, and the adding proportion of the additive is 1 percent of the total amount of the feed.
Example 3:
the preparation method of the ophiopogon japonicus plant extract, the liriope spicata plant extract and the ophiopogon japonicus bioactive component comprises the following steps:
a. drying tuber of radix Ophiopogonis, pulverizing, sieving with 150 mesh standard sieve, adding into 25-30 times of water, and ultrasonic extracting at 55 deg.C under ultrasonic power of 300W for 43 min; and (4) performing enzymatic extraction on the material liquid mixture after ultrasonic treatment according to the enzyme adding sequence of pectinase → cellulase → papain. Adjusting pH to 3.4, heating to 52 deg.C, adding 0.42% cellulase, and performing enzymolysis for 34 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 3.8 at 34 deg.C, adding 0.47% cellulase, and performing enzymolysis for 37 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 5.7, adjusting temperature to 35 deg.C, adding 0.54% papain for enzymolysis for 51min, and inactivating enzyme in boiling water bath for 5 min. Cooling the mixture, and vacuum filtering to obtain extractive solution. Concentrating the extractive solution in vacuum to 30% of the original volume, and centrifuging to obtain supernatant and precipitate. Extracting the supernatant with equal volume of ethyl acetate for 3 times, mixing the extractive solutions, recovering water phase liquid, and mixing the ethyl acetate phase liquids. And (4) carrying out rotary evaporation on the ethyl acetate phase liquid to recover ethyl acetate to obtain the ethyl acetate extract of the radix ophiopogonis.
b. And (b) combining the recovered aqueous phase liquid after extraction in the step a, concentrating the aqueous phase liquid in vacuum to 30% of the original volume, and centrifuging to obtain a supernatant and a precipitate. And adding 5 times of volume of absolute ethyl alcohol into the supernatant, standing overnight, and performing suction filtration to obtain a precipitate. Washing the precipitate with anhydrous alcohol and acetone for 3 times, and vacuum lyophilizing the precipitate to obtain radix Ophiopogonis water extract.
c. And uniformly mixing the ethyl acetate extract of the dwarf lilyturf tuber and the water extract of the dwarf lilyturf tuber to obtain the dwarf lilyturf tuber plant extract.
The preparation method of the liriope spicata plant extract comprises the following steps:
a. drying tuber of liriope spicata, pulverizing, sieving with 150 mesh standard sieve, adding into 25-30 times of water, and ultrasonic extracting at 55 deg.C under ultrasonic power of 300W for 43 min; and (4) performing enzymatic extraction on the material liquid mixture after ultrasonic treatment according to the enzyme adding sequence of pectinase → cellulase → papain. Adjusting pH to 3.4, heating to 52 deg.C, adding 0.42% cellulase, and performing enzymolysis for 34 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 3.8 at 34 deg.C, adding 0.47% cellulase, and performing enzymolysis for 37 min. Inactivating enzyme in boiling water bath for 5min, adjusting pH to 5.7, adjusting temperature to 35 deg.C, adding 0.54% papain for enzymolysis for 51min, and inactivating enzyme in boiling water bath for 5 min. Cooling the mixture, and vacuum filtering to obtain extractive solution. Concentrating the extractive solution in vacuum to 30% of the original volume, and centrifuging to obtain supernatant and precipitate. Extracting the supernatant with equal volume of ethyl acetate for 3 times, mixing the extractive solutions, recovering water phase liquid, and mixing the ethyl acetate phase liquids. And (4) carrying out rotary evaporation on the ethyl acetate phase liquid to recover ethyl acetate to obtain the liriope spicata ethyl acetate extract.
b. And (b) taking the water phase liquid recovered after extraction in the step a, concentrating the water phase liquid in vacuum to 30% of the original volume, and centrifuging to obtain a supernatant and a precipitate. And adding 5 times of volume of absolute ethyl alcohol into the supernatant, standing overnight, and performing suction filtration to obtain a precipitate. Washing the precipitate with anhydrous alcohol and acetone for 3 times, and vacuum lyophilizing the precipitate to obtain radix liriopes extract.
c. And uniformly mixing the ethyl acetate extract of the radix ophiopogonis and the water extract of the radix ophiopogonis to obtain the liriope spicata plant extract.
The preparation method of the radix ophiopogonis bioactive component comprises the following steps:
dissolving equal amounts of Ophiopogon D powder, Liriope muscarib saponin C powder and Methylphosphinonene A powder in ultrapure water, and spray drying at an air inlet temperature of 160 deg.C and an air outlet temperature of 110 deg.C to obtain radix Ophiopogonis bioactive components.
Selecting the produced raw materials, selecting the ophiopogon root plant extract, the liriope spicata plant extract and the ophiopogon root bioactive component according to the ratio of 100: 80: 1.2, mixing the selected raw materials after the selection is finished, and preparing the additive. When in use, the prepared additive is put into pet feed, and the adding proportion of the additive is 1.4 percent of the total amount of the feed.
Example 4
The invention carries out a comparative test on pet dogs, selects 100 healthy and active tydi dogs with the age of more than 12 months, and divides the dogs into 4 groups according to the principle that the weight and the sex ratio are similar, namely a control group, a test group 1, a test group 2 and a test group 3. The control group was fed with basal ration, test group 1 was fed with the ophiopogon root pet feed additive described in example 1, test group 2 was fed with the ophiopogon root pet feed additive described in example 2, and test group 3 was fed with the ophiopogon root pet feed additive described in example 3. The total weight of the feed fed every day is consistent, and the feeding period of the test is 60 days. The basic ration comprises the following formula: 250g of meat, 150g of milk powder, 50g of edible oil, 300g of flour, 1 piece of mineral element and vitamin composite sheet. The tested animals are all raised in the same environment, can move freely and drink water, and are fed three times a day. The effects are shown in table 1.
TABLE 1 results of hair beautification and nose fading resistance of control and test groups
Example 5
The invention carries out comparative test on pet cats, selects 100 healthy and active Persian cats with the age of more than 12 months, and divides the cats into 4 groups according to the principle of similar weight and sex ratio, namely a control group, a test group 1, a test group 2 and a test group 3. The control group was fed with basal ration, test group 1 was fed with the ophiopogon root pet feed additive described in example 1, test group 2 was fed with the ophiopogon root pet feed additive described in example 2, and test group 3 was fed with the ophiopogon root pet feed additive described in example 3. The total weight of the feed fed every day is consistent, and the feeding period of the test is 60 days. The basic ration comprises the following formula: 200g of meat, 200g of milk powder, 30g of edible oil, 250g of flour, and 1 piece of mineral element and vitamin composite sheet. The tested animals are all raised in the same environment, can move freely and drink water, and are fed three times a day. The effect is shown in table 2.
TABLE 2 results of hair beautification and nose fading resistance of control and test groups
Example 6
The invention carries out comparative test on angora rabbits, selects 100 healthy and active angora rabbits with the age of more than 6 months, and divides the angora rabbits into 4 groups according to the principle that the weight and the sex ratio are similar, namely a control group, a test group 1, a test group 2 and a test group 3. The control group was fed with basal ration, test group 1 was fed with the ophiopogon root pet feed additive described in example 1, test group 2 was fed with the ophiopogon root pet feed additive described in example 2, and test group 3 was fed with the ophiopogon root pet feed additive described in example 3.
The total weight of the feed fed every day is consistent, and the feeding period of the test is 60 days. The basic ration comprises the following formula: 25g of corn, 40g of bean cake, 50g of grass meal, 0.2 piece of mineral element and vitamin compound tablet and 800g of fresh grass. The tested animals are all raised in the same environment, can move freely and drink water, and are fed three times a day. The effect is shown in table 3.
TABLE 3 results of hair beautification and anti-nose fading of control and test groups
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications can be made without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.