CN111888387A - Fenugreek essential oil enteric microcapsule preparation and preparation method thereof - Google Patents
Fenugreek essential oil enteric microcapsule preparation and preparation method thereof Download PDFInfo
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- CN111888387A CN111888387A CN202010858437.4A CN202010858437A CN111888387A CN 111888387 A CN111888387 A CN 111888387A CN 202010858437 A CN202010858437 A CN 202010858437A CN 111888387 A CN111888387 A CN 111888387A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
Abstract
The invention discloses a fenugreek essential oil enteric microcapsule preparation and a preparation method thereof. The fenugreek essential oil enteric microcapsule preparation comprises the following components in percentage by mass: 1-20% of fenugreek essential oil; 1-5% of an emulsifier; 1-5% of an antioxidant; 30-80% of a filler; 10-50% of enteric-coated material. Compared with direct material mixing and large-amount administration, the fenugreek essential oil enteric microcapsule preparation provided by the invention can avoid volatilization loss and oxidative deterioration risk of fenugreek stem and leaf essential oil, can be stored for a long time and is convenient to use. The fenugreek essential oil enteric microcapsule preparation prepared by the invention is in the form of powder or spherical fine particles, has the particle size of 40-200 meshes, has good fluidity and dispersibility, and is more beneficial to being uniformly mixed with feed. The selected auxiliary materials can endure strong acid environment in the animal body, and are easy to dissolve out in weak acid environment, so that the drug is prevented from being damaged by enzymes or gastric acid in the stomach in the process of passing through the animal stomach environment, the drug is ensured to be released in the intestinal tract, and is completely released before being discharged out of the intestinal tract, and the utilization rate of the fenugreek essential oil can be improved.
Description
Technical Field
The invention belongs to the technical field of preparation of animal medicines, and particularly relates to a fenugreek stem and leaf essential oil enteric microcapsule preparation and a preparation method thereof.
Background
The Fenugreek (Fenugreek) is a traditional medicine-food dual-purpose resource, is widely planted in China, and has extremely high nutritional value and a plurality of physiological effects. Fenugreek was first used as a spice in its place of origin, especially in india and mediterranean coastal countries. The seeds and leaves of fenugreek have a unique, pungent odor and can be used as a spice material for the cooking of meats, poultry, vegetables, etc. Particularly, fenugreek seeds, which are frequently used in the preparation of various curries, as well as kimchi and sauces in the Indian delicacy; in the region of also and arabian, fenugreek seeds are the most predominant seasoning; in south Asia and Egyptian areas, fresh and tender leaves and sprouts of fenugreek are eaten as vegetables, and the dried leaves are used for being added into various soups and curries, so that the taste of the vegetables is more delicious; in Elite and Elite, fenugreek is used as a supplementary ingredient added to wheat and corn flour for making cakes, improving the color and eating quality of the cakes; in india, fenugreek seed flour is one of the important ingredients in its specialty breads; in China, fenugreek is mainly used as a food colorant, and most of stems and leaves of the fenugreek are ground into powder and then added into various cake foods as an ideal natural colorant.
The fenugreek stem and leaf essential oil is an extract of the stem and leaf of the fenugreek, is a bright yellow oily substance, and has strong inhibition effect on bacillus subtilis, escherichia coli, staphylococcus aureus, penicillium and mucor species bacteria and certain inhibition effect on aspergillus niger, wherein the minimum inhibition concentrations of the fenugreek stem and leaf essential oil are respectively 0.4g/L of the bacillus subtilis, 0.5g/L of the escherichia coli, the staphylococcus aureus and the penicillium, 0.6g/L of the mucor and 1.0g/L of the aspergillus niger.
The fenugreek stem and leaf essential oil is extremely volatile and easy to oxidize, if the fenugreek stem and leaf essential oil is directly mixed with a large amount of feed for administration, the bioavailability is extremely low, intestines and stomach are easy to be stimulated, gastric mucosa is stimulated, anorexia of animals is easy to cause, and the application of the fenugreek stem and leaf essential oil in preventing and treating animal diseases is severely limited. Therefore, a preparation which can be dissolved and released only after entering the biological intestinal tract is urgently needed, so that the loss of the essential oil of the stems and leaves of the fenugreek is prevented as much as possible, the utilization rate is improved, the medication safety is improved, and the effects of preventing and treating the diseases of the livestock and poultry are improved.
Starch Sodium Octenyl Succinate (SSOS) is a modified Starch, which is a white or yellowish powder, flake or granule obtained by esterification of Starch with Octenyl succinic anhydride. When the sodium starch octenyl succinate acts on an oil/water emulsion, hydrophilic carboxylic acid groups of the sodium starch octenyl succinate extend into water, lipophilic octenyl long chains extend into oil, and a tough and unbreakable film is formed on an oil-water interface by long polysaccharide chains, so that dispersed phase particles are difficult to aggregate and separate, and the sodium starch octenyl succinate has very good emulsifying and thickening properties. Most of the traditional modified starches such as oxidized starch, acid modified starch and the like only have single hydrophilic property, the added value of the product is lower, and the sodium octenyl succinate starch (SSOS) has hydrophilic and oleophilic emulsification property, so that the method is a hot spot for research and development of modified starches at home and abroad in recent years.
At present, most sodium starch octenylsuccinate obtained by industrial production has larger molecular weight and lower solubility in water, and is often used as an emulsifier and a thickener only in a small amount. If the amount is increased, a lower molecular weight sodium starch octenyl succinate must be used, or a high molecular weight sodium starch octenyl succinate must be homogenized under high pressure and then used. Under the condition of normal temperature, the sodium starch octenyl succinate with low molecular weight and low viscosity presents a shear thinning phenomenon along with the increase of the shear rate, and has the characteristics of pseudoplastic fluid. The shear thinning phenomenon is explained by h.a. barles et al as follows: the shearing makes the macromolecule extend more in the flowing direction, increases the volume occupied by the molecule, reduces the average number of chain segments in the macromolecule, and simultaneously eliminates the coil expansion caused by the volume effect, thereby reducing the tackifying effect, which causes the viscosity reduction, however, more chain segments are exposed in the external flowing field to increase the resistance. The simultaneous action of these opposing effects causes shear thinning or thickening, the overall effect of which is often shear thinning.
By utilizing the characteristic of shear thinning of the octenyl succinic acid starch sodium, the fenugreek essential oil and the octenyl succinic acid starch sodium with certain viscosity can be homogenized under normal pressure, and then the mixture is granulated by spray drying, so that the microcapsule preparation with enteric property can be obtained.
Disclosure of Invention
The invention provides a fenugreek essential oil enteric microcapsule preparation which is characterized by comprising the following components in percentage by mass: 1-20% of fenugreek essential oil; 1-5% of an emulsifier; 1-5% of an antioxidant; 30-80% of a filler; 10-50% of enteric-coated material. Wherein the semen Trigonellae essential oil is obtained by subjecting stem and leaf of semen Trigonellae to steam distillation, organic solvent extraction, supercritical extraction, subcritical extraction, and molecular distillation; the emulsifier is at least one of sucrose ester, sodium lignosulfonate and tween 80; the antioxidant is at least one of vitamin C, sodium benzoate and ascorbic acid; the filler is at least one of white sugar, maltodextrin and Arabic gum; the enteric material is sodium starch octenyl succinate.
The key of the preparation technology lies in that the shearing thinning phenomenon of octenyl succinic acid starch sodium after reducing molecular weight through ultramicro sanding is utilized, so that the octenyl succinic acid starch sodium can respectively form homogeneous liquid with fenugreek stem and leaf essential oil emulsion and a filling agent, and microcapsule particles obtained after spray drying of the homogeneous liquid have the characteristics of an enteric preparation. The preparation method comprises the following steps:
s1, sequentially weighing a fenugreek essential oil raw material, an emulsifier and an antioxidant according to a proportion, adding the raw material, the emulsifier and the antioxidant into water, and shearing, stirring and emulsifying at normal temperature to obtain a mixture A;
s2, adding sodium starch octenyl succinate into a nano-scale sand mill, adding a proper amount of purified water, and circularly grinding to obtain a mixture B;
s3, adding the mixture A into the mixture B which is sheared and stirred in the step S2, and homogenizing to obtain a mixture C;
s4, adding a filling agent into the mixture C which is subjected to shearing and stirring in the step S3, and homogenizing to obtain a mixture D;
s5, spray drying the mixture D obtained in the step S5, and cooling the mixture D by a fluidized bed to prepare powder particles;
s6, sieving the powder particles obtained in the step S6, and collecting the powder particles with the particle size below 40 meshes.
The stirring, sanding and spray drying described in the present invention are well within the skill of the art and can be performed using any of the devices known in the art that can perform these methods.
Preferably, the shearing and stirring speed in the step S1 is 500-3000 r/min, and the stirring time is 10-600 min.
Preferably, in the step S2, the sodium starch octenylsuccinate accounts for 1-20% of the mass of the mixture B.
Preferably, the grinding conditions of the medium-nanometer-scale sand mill in the step S2 are as follows: the diameter of zirconium beads used for sanding is 0.3-2.0 mm, the rotating speed is 1000-3000 rpm, the material temperature is 30-50 ℃, and the sanding time is 30-600 min.
Preferably, the viscosity of the mixture B in the step S2 is 1000 to 20000 mPas.
Preferably, the shearing and stirring speed in the step S3 is 500-3000 r/min, and the stirring time is 10-600 min.
Preferably, the shearing stirring speed in the step S4 is 500-3000 rpm, and the stirring time is 10-600 min.
Preferably, in the mixture D in the step S4, the mass ratio of water is 40-95%.
Preferably, the outlet temperature of the spray drying in the step S5 is 60-100 ℃, and the pressure of the compressed air is 0.14-0.18 MPa.
Preferably, the linear velocity of the fluidized bed spray droplets in the step S5 is between 55 and 135 m/S.
Preferably, the particle size of the powder particles obtained in step S6 is 40-200 meshes.
Provides the application of the fenugreek essential oil enteric microcapsule preparation in the aspect of livestock and poultry health care medicines.
Compared with the prior art, the invention has the following advantages:
(1) compared with direct material mixing and large-amount administration, the fenugreek essential oil enteric microcapsule preparation provided by the invention can avoid volatilization loss and oxidative deterioration risk of fenugreek stem and leaf essential oil, can be stored for a long time and is convenient to use.
(2) Compared with the traditional premix production process, the fenugreek essential oil enteric microcapsule preparation has the advantages that auxiliary materials are low in price and easy to obtain, and the fenugreek essential oil enteric microcapsule preparation is suitable for industrial production. The prepared fenugreek essential oil enteric microcapsule preparation is spherical fine particles, the particle size is 40-200 meshes, the fluidity and the dispersibility are good, and the uniform mixing with feed is facilitated.
(3) The in vitro release degree experiment of the fenugreek essential oil enteric microcapsule preparation provided by the invention shows that: the enteric microcapsule preparation releases less than 2.5 percent in 0.1mol/L hydrochloric acid for 1 hour, and the microcapsule particles are complete and have no change in appearance; in phosphate buffer pH =6.8, the microcapsule particles erode quickly and the drug dissolves out quickly. Therefore, the selected auxiliary materials can endure a strong acid environment in an animal body, and are easy to dissolve out in a weak acid environment, so that the medicament is prevented from being damaged by enzymes or gastric acid in the stomach in the process of passing through the stomach environment of the animal, the medicament is ensured to be released in the intestinal tract and is completely released before being discharged out of the intestinal tract, and the utilization rate of the fenugreek essential oil can be improved.
Detailed Description
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto.
Example 1
The fenugreek essential oil enteric microcapsule is prepared according to the following steps:
s1, weighing 50g of fenugreek essential oil raw materials, 25g of sucrose ester, 5.0g of sodium benzoate and 100g of purified water, shearing, stirring and emulsifying to obtain a mixture A;
s2, adding 100g of sodium starch octenyl succinate and 400g of purified water into a nano-scale sand mill, and circularly grinding under the following conditions: the diameter of the zirconium beads is 1.0mm, the rotating speed is 2000rpm, the material temperature is 30-40 ℃, and the sanding time is 60 min. After sanding, obtaining a mixture B, wherein the rotational viscosity of the mixture B is 6692mPa & s;
s3, processing the mixture B at a shearing and stirring speed of 4000r/min for 60min, reducing the viscosity to 4160mPa & s, adding the mixture A into the mixture B undergoing shearing and stirring, continuing stirring for 60min after the addition is finished, and homogenizing to obtain a mixture C;
s4, keeping the shearing and stirring speed unchanged, adding 300g of maltodextrin to the mixture C which is sheared and stirred in the step S3, adding 300g of purified water, continuing stirring for 60min after the addition is finished, and homogenizing to obtain a mixture D;
s5, spray-drying the mixture D in the step S4, and cooling the mixture D by a fluidized bed to prepare powder particles, wherein the temperature of fluidizing air is 30 ℃, and the linear velocity is 75 m/S;
s6, sieving the powder particles obtained in the step S5, and collecting the powder particles with the particle size below 40 meshes.
Example 2
The fenugreek essential oil enteric microcapsule is prepared according to the following steps:
s1, weighing 50g of a fenugreek essential oil raw material, 50g of sodium lignosulfonate, 10g of ascorbic acid and 200g of purified water, shearing, stirring and emulsifying to obtain a mixture A;
s2, adding 100g of sodium starch octenyl succinate and 400g of purified water into a nano-scale sand mill, and circularly grinding under the following conditions: the diameter of the zirconium beads is 0.75mm, the rotating speed is 3000rpm, the material temperature is 35-50 ℃, and the sanding time is 120 min. After sanding, obtaining a mixture B, wherein the rotational viscosity of the mixture B is 4230mPa & s;
s3, treating the mixture B at a shearing and stirring speed of 3000r/min for 30min, reducing the viscosity to 3036mPa & s, adding the mixture A into the mixture B undergoing shearing and stirring, continuing stirring for 30min after the addition is finished, and homogenizing to obtain a mixture C;
s4, keeping the shearing and stirring speed unchanged, adding 250g of white sugar into the mixture C which is sheared and stirred in the step S3, adding 250g of purified water, continuing stirring for 30min after the addition is finished, and homogenizing to obtain a mixture D;
s5, spray-drying the mixture D in the step S4, and cooling the mixture D by a fluidized bed to prepare powder particles, wherein the temperature of fluidizing air is 30 ℃, and the linear velocity is 75 m/S;
s6, sieving the powder particles obtained in the step S5, and collecting the powder particles with the particle size below 40 meshes.
Example 3
The fenugreek essential oil enteric microcapsule is prepared according to the following steps:
s1, weighing 50g of fenugreek essential oil raw materials, 8020 g of tween, 10.0g of vitamin C and 100g of purified water, shearing, stirring and emulsifying to obtain a mixture A;
s2, adding 100g of sodium starch octenyl succinate and 400g of purified water into a nano-scale sand mill, and circularly grinding under the following conditions: the diameter of the zirconium beads is 1.5mm, the rotating speed is 2500rpm, the material temperature is 30-40 ℃, and the sanding time is 180 min. After sanding, obtaining a mixture B, wherein the rotational viscosity of the mixture B is 8552mPa & s;
s3, processing the mixture B at a shearing and stirring speed of 4000r/min for 90min until the viscosity of the mixture B is reduced to 5060mPa & s, adding the mixture A into the mixture B undergoing shearing and stirring, continuing stirring for 45min after the addition is finished, and homogenizing to obtain a mixture C;
s4, keeping the shearing and stirring speed unchanged, adding 400g of Arabic gum to the mixture C which is sheared and stirred in the step S3, adding 200g of purified water, continuing stirring for 60min after the addition is finished, and homogenizing to obtain a mixture D;
s5, spray-drying the mixture D in the step S4, and cooling the mixture D by a fluidized bed to prepare powder particles, wherein the temperature of fluidizing air is 30 ℃, and the linear velocity is 75 m/S;
s6, sieving the powder particles obtained in the step S5, and collecting the powder particles with the particle size below 40 meshes.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The fenugreek essential oil enteric microcapsule preparation is characterized by comprising the following components in percentage by mass: 1-20% of fenugreek essential oil; 1-5% of an emulsifier; 1-5% of an antioxidant; 30-80% of a filler; 10-50% of enteric-coated material.
2. The fenugreek essential oil of claim 1, which is obtained by subjecting stems and leaves of fenugreek to at least one of steam distillation, organic solvent extraction, supercritical extraction, subcritical extraction and molecular distillation; the emulsifier is at least one of sucrose ester, sodium lignosulfonate and tween 80; the antioxidant is at least one of vitamin C, sodium benzoate and ascorbic acid; the bulking agent is at least one of white sugar, maltodextrin and acacia; the enteric material is sodium starch octenyl succinate.
3. The preparation method of the fenugreek essential oil enteric microcapsule formulation according to claim 1, comprising the steps of:
step 1) weighing fenugreek essential oil raw materials, an emulsifier and an antioxidant in sequence according to a proportion, adding the raw materials, the emulsifier and the antioxidant into water, and shearing, stirring and emulsifying at normal temperature to obtain a mixture A;
step 2), adding sodium starch octenyl succinate into a nano-scale sand mill, adding a proper amount of purified water, and circularly grinding to obtain a mixture B;
step 3) adding the mixture A to the mixture B which is sheared and stirred in the step 2), and homogenizing to obtain a mixture C;
step 4), adding a filling agent into the mixture C which is subjected to shearing and stirring in the step 3), and homogenizing to obtain a mixture D;
step 5) spray-drying the mixture D obtained in the step 5), and cooling the mixture D by a fluidized bed to prepare powder particles;
and 6) sieving the powder particles obtained in the step 6), and collecting the powder particles with the particle size of below 40 meshes.
4. The method according to claim 3, wherein the shear stirring speed in the step 1) is 500-3000 r/min, and the stirring time is 10-600 min.
5. The method according to claim 3, wherein the sodium starch octenylsuccinate accounts for 1-20% of the mass of the mixture B in the step 2).
6. The method as claimed in claim 3, wherein the grinding conditions of the nano-scale sand mill in the step 2) are as follows: the diameter of zirconium beads used for sanding is 0.3-2.0 mm, the rotating speed is 1000-3000 rpm, the material temperature is 30-50 ℃, and the sanding time is 30-600 min.
7. The process according to claim 3, wherein the viscosity of the mixture B in step 2) is 1000 to 20000 mPas.
8. The method as claimed in claim 3, wherein the shear stirring speed in step 3) is 500-3000 r/min, and the stirring time is 10-600 min.
9. The method according to claim 3, wherein the shear stirring speed in the step 4) is 500-3000 rpm, and the stirring time is 10-600 min.
10. The method according to claim 3, wherein the mixture D in the step 4) contains water in a mass ratio of 40-95%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112586610A (en) * | 2020-12-15 | 2021-04-02 | 张德奎 | Extended release formulation for antibiotic replacement therapy |
| CN112675152A (en) * | 2020-12-25 | 2021-04-20 | 厦门金达威生物科技有限公司 | NMN slow-release enteric-coated microcapsule and preparation method thereof |
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2020
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| CN104862079A (en) * | 2015-05-27 | 2015-08-26 | 天水师范学院 | Method for extracting essential oil from trigonella foenum-graecum leaves |
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Application publication date: 20201106 |