CN101780232A - Coix seed oil proliposome and preparation method thereof - Google Patents
Coix seed oil proliposome and preparation method thereof Download PDFInfo
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Abstract
The invention relates to coix seed oil proliposome and a preparation method thereof. The method comprises the following steps: adding supporting agents, surface active agents and antioxidants in the preparation process of coix seed oil lipidosome turbid liquor; carrying out freeze drying or spray drying; and obtaining a coix seed oil proliposome powdery solid preparation. Adding a certain amount of water into the coix seed oil proliposome powdery solid preparation before use, the coix seed oil proliposome powdery solid preparation can be converted back into the liquid coix seed oil lipidosome through hydrating the coix seed oil proliposome via oscillation or ultrasonic sound treatment or agitation. The invention has simple operation, is suitable for industrial production, and can obviously improve the stability of the coix seed oil and liquid coix seed oil lipidosome. The obtained coix seed oil proliposome has the advantages of ordinary liquid lipidosome, also has the characteristics of easy package, convenient transportation, convenient storage, convenient use and the like, can be used as health care food or nutritional additives to be added to other food, and can also be used as medicine preparations.
Description
Technical field
The invention belongs to functional health-care food and field of pharmaceutical preparations, but be specifically related to contain the pro-liposome of Semen Coicis oil and the preparation method of industrial applications thereof.
Background technology
Semen Coicis (Coix lachryma-jobi Linn) is grass family (Gramineae) Coix (Coix L.) herbaceous plant, and the nutritive value of Semen Coicis is very high, is described as " king of world grass ".Its kernel is a Semen Coicis, but medicated diet is dual-purpose, has the effect of spleen invigorating, tonifying the lung, heat clearing away, dampness removing.Contain the Semen Coicis oil of having an appointment about 2-7% in the Semen Coicis, zoopery and the clinical Semen Coicis oil that all confirms have analgesic, calm, analgesia, enhancing immunity, auxiliary hyperglycemic, treatment cardiovascular system diseases and suppress effect of malignant tumors.But unsaturated fatty acid content surpasses 80% in the Semen Coicis oil, and is very easily oxidized, limited its extensive use greatly.
Adopt liposome embedded Semen Coicis oil, its effective ingredient is wrapped in the lipid bilayer, can strengthen the stability of Semen Coicis oil, prevent its oxidative degradation, and can improve its water solublity.Liposome can prevent effectively that as the oral lipoids carrier of Semen Coicis oil Semen Coicis oil from by enzyme hydrolysis or liver first-pass effect, strengthening its stability in gastrointestinal tract, is easy to be absorbed by intestinal mucosa, improves bioavailability.Chinese patent CN1440782A " a kind of preparation technology and prescription that contains Semen Coicis oil and Oleum Fructus Bruceae composite Nano Emulsion " discloses the preparation method of a kind of Semen Coicis oil and Oleum Fructus Bruceae complex liposome, that is: earlier with the cholesterol ultra-sonic dispersion in ethanol, 60 ℃ of heating in water bath, add phospholipid and stir into opaque viscous solution, under agitation splash into Semen Coicis oil and Oleum Fructus Bruceae, stirred 2-3 minute, add the low amounts of water dilution, under agitation slowly add water to full dose subsequently, ultrasonic 4 minutes promptly.Complex liposome consist of contain Semen Coicis oil 0.1～15.0g, Oleum Fructus Bruceae 0.1～15.0g, fabaceous lecithin 0.8～3.0g, cholesterol 1.0～5.0g in every 100mL liposome emulsion, all the other are water for injection.
The above-mentioned background technology exists the technological operation temperature higher, does not take to add measures such as antioxidant or oxygen barrier effective ingredient is protected, and makes active ingredient in the Semen Coicis oil be subjected to a certain degree destruction; Phenomenons such as gathering, fusion, sedimentation also appear in above-mentioned liquid complex liposome easily, and packing, transportation, condition of storage require also relatively harsher, are difficult to long term store.
Summary of the invention
The objective of the invention is problem, a kind of proliposome preparation and preparation method thereof is provided at Semen Coicis oil and ordinary liquid lipidosome existence.Pro-liposome is a kind of solid preparation, has stable in properties, packs characteristics such as easy, storage, convenient transportation.Add a certain amount of water before the use, through vibration or ultrasonic or stirring, hydration can revert back to liquid lipidosome.Semen Coicis oil is made pro-liposome, can improve preparation long term store process stability of drug, pack, preserve, transport and use more convenient, and can effectively solve the problem of oxidation of the gathering of liquid Semen Coicis oil liposome, sedimentation, fusion, seepage and sterilization phospholipid.
Coix seed oil proliposome of the present invention, contain following component and percetage by weight:
Semen Coicis oil 1～50%
Phosphatidase 13～75%
Cholesterol 0.1～20%
Surfactant 0.2～15%
Antioxidant 0.001～4%
Proppant 0.5～70%
Coix seed oil proliposome of the present invention is the pulverulent solids preparation that makes through lyophilization or spray drying, face with before adding a certain amount of water, through vibration or ultrasonic or stirring, make the coix seed oil proliposome hydration can revert back to liquid Semen Coicis oil liposome.
Multiple phospholipid of the present invention is one or more in Ovum Gallus domesticus Flavus lecithin, hydrolecithin, distearoyl phosphatidylcholine, Phosphatidylserine, phosphatidylinositols, PHOSPHATIDYL ETHANOLAMINE, phosphatidyl glycerol, phosphatidylcholine, dipalmitoyl phosphatidyl choline, two myristoyl phosphatidylcholines, the ceramide.
Surfactant of the present invention is one or more in polyoxyethylene castor oil, polyoxyethylene hydrogenated Oleum Ricini, monoglyceride, sodium lauryl sulphate, Tween 80, polysorbate60, Brij, Myrij, sorbester p17, sorbester p18, sodium cholate, the sodium deoxycholate.
Antioxidant of the present invention is V
E, V
CAmong cetylate, BHA (BHA), TBHQ (tertiarybutylhydroquinone) or the BHT (dibenzylatiooluene) one or more.
Proppant of the present invention is in mannitol, glucose, polyvinyl alcohol 6000, sucrose, lactose, trehalose, polyvinylpyrrolidone, Macrogol 4000, chitosan, carboxymethyl chitosan, the cyclodextrin a kind or multiple.
Coix seed oil proliposome of the present invention prepares by following method and step:
(1) press the component mass percent with Semen Coicis oil, phospholipid, cholesterol, antioxidant, surfactant with suitable organic solvent dissolution, make lipid soln;
(2) lipid soln that (1) is made is injected in the buffer solution that is dissolved with proppant, after this buffer solution placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove organic solvent, rapidly after the cooling, through supersound process (59KHz, power 95%, 10min) or extra high pressure homogenize handle (15000～20000psi, circulate 1～3 time), make the Semen Coicis oil liposome turbid liquor;
(3) the Semen Coicis oil liposome turbid liquor of (2) being made is removed moisture through lyophilization or spray drying, promptly gets coix seed oil proliposome.
Organic solvent of the present invention is a kind of in chloroform, ether, ethanol or the methanol.
Buffer solution of the present invention comprises phosphate buffer, acetic acid-ammonium acetate buffer or acetic acid-sodium-acetate buffer, and pH of buffer is 6.0～7.4.
Spray drying of the present invention is meant that 140～220 ℃ of inlet temperature, leaving air temp carries out spray drying for 70～110 ℃.
The invention has the beneficial effects as follows: Semen Coicis oil is prepared as pro-liposome except that having the advantage of conventional liposome, as increase medicine stability and percutaneous absorbability, also have the following advantages: 1, coix seed oil proliposome is a solid preparation, good stability, long shelf-life, convenient transportation, add water through vibration or ultrasonic or stirring with preceding need, make the coix seed oil proliposome hydration can revert back to liquid Semen Coicis oil liposome, thereby solved Semen Coicis oil liposome instability problem such as easily gathering, sedimentation, fusion under liquid state.2, because coix seed oil proliposome is a solid preparation, in storage and use, the Semen Coicis oil functional components is more stable, when making an addition to other food as nourishing additive agent, uses more convenient flexible.
The specific embodiment
Embodiment 1
Semen Coicis oil 12, hydrolecithin 7.5g, cholesterol 1.5g, V
E0.003g, TBHQ0.001g, polyoxyethylene castor oil 1g, trehalose 3g, lactose 1g, chloroform 40mL, pH6.8 phosphate buffer 500mL.
Accurately take by weighing Semen Coicis oil, hydrolecithin, cholesterol, V in the above-mentioned prescription
ETBHQ, polyoxyethylene castor oil, it is extremely molten in 50 ℃ of water-baths to add the 40mL chloroform, get lipid soln, be injected in the phosphate buffer that 500mL is dissolved with trehalose and lactose with constant flow pump while stirring, after this phosphate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (55 ℃ of chloroforms, vacuum 0.1MPa), cooling rapidly is through supersound process (59KHz, power 95%, 10min), get the Semen Coicis oil liposome turbid liquor, the Semen Coicis oil liposome turbid liquor is through (45 ℃ of lyophilizations, vacuum 0.1MPa), promptly get the coix seed oil proliposome that loosens.
Embodiment 2
Semen Coicis oil 2, Ovum Gallus domesticus Flavus lecithin 10g, cholesterol 1.5g, V
E0.003g, sodium lauryl sulphate 1g, sucrose 1.5g, mannitol 1g, ether 40mL, pH6.0 acetic acid-ammonium acetate buffer 300mL.
Accurately take by weighing Semen Coicis oil, Ovum Gallus domesticus Flavus lecithin, cholesterol, V in the above-mentioned prescription
ESodium lauryl sulphate, it is extremely molten in 45 ℃ of water-baths to add the 40mL ether, get lipid soln, be injected in acetic acid-ammonium acetate buffer that 300mL is dissolved with sucrose and mannitol with constant flow pump while stirring, after this acetic acid-ammonium acetate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (45 ℃ of ether, vacuum 0.1MPa), cooling rapidly is through supersound process (59KHz, power 95%, 10min), get the Semen Coicis oil liposome turbid liquor, the Semen Coicis oil liposome turbid liquor is through (45 ℃ of lyophilizations, vacuum 0.1MPa), promptly get the coix seed oil proliposome that loosens.
Embodiment 3
Semen Coicis oil 5g, phosphatidylcholine 20g, dipalmitoyl phosphatidyl choline 5g, cholesterol 10g, TBHQ 0.01g, Tween 80 4g, sorbester p17 0.75g, carboxymethyl chitosan 15g, chitosan 10g, ethanol 40mL, pH6.8 phosphate buffer 300mL.
Accurately take by weighing Semen Coicis oil in the above-mentioned prescription, phosphatidylcholine, dipalmitoyl phosphatidyl choline, cholesterol, TBHQ, Tween 80, sorbester p17, it is extremely molten in 40 ℃ of water-baths to add 40mL ethanol, get lipid soln, be injected in the phosphate buffer that 300mL is dissolved with carboxymethyl chitosan and chitosan with constant flow pump while stirring, after this phosphate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (45 ℃ of ethanol, vacuum 0.1MPa), cooling rapidly, through supersound process (59KHz, power 95%, 10min), get the Semen Coicis oil liposome turbid liquor, the Semen Coicis oil liposome turbid liquor is through (45 ℃ of lyophilizations, vacuum 0.1MPa), promptly get the coix seed oil proliposome that loosens.
Embodiment 4
Semen Coicis oil 2g, Phosphatidylserine 10g, phosphatidylinositols 10g, cholesterol 5g, BHT 0.01g, sodium cholate 3g, sodium deoxycholate 1.5g, polyvinyl alcohol 6000 10g, methanol 40mL, pH6.8 phosphate buffer 300mL.
Accurately take by weighing Semen Coicis oil in the above-mentioned prescription, Phosphatidylserine, phosphatidylinositols, cholesterol, BHT, sodium cholate, sodium deoxycholate, it is extremely molten in 45 ℃ of water-baths to add 40mL methanol, get lipid soln, be injected in the phosphate buffer that 300mL is dissolved with polyvinyl alcohol 6000 with constant flow pump while stirring, after this phosphate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (55 ℃ of methanol, vacuum 0.1MPa), cooling rapidly, handle (18000psi through extra high pressure homogenize, circulate 2 times), get the Semen Coicis oil liposome turbid liquor, the Semen Coicis oil liposome turbid liquor promptly gets the coix seed oil proliposome that loosens through lyophilization (45 ℃, vacuum 0.1MPa).
Embodiment 5
Semen Coicis oil 5g, PHOSPHATIDYL ETHANOLAMINE 10g, phosphatidyl glycerol 5g, cholesterol 1.5g, V
CCetylate 0.005g, monoglyceride 1.5g, Macrogol 4000 8.5g, ether 20mL, pH7.4 phosphate buffer 350mL.
Accurately take by weighing Semen Coicis oil, PHOSPHATIDYL ETHANOLAMINE, phosphatidyl glycerol, cholesterol, V in the above-mentioned prescription
CCetylate, monoglyceride, it is extremely molten in 45 ℃ of water-baths to add the 20mL ether, get lipid soln, be injected in the phosphate buffer that 350mL is dissolved with Macrogol 4000 with constant flow pump while stirring, after this phosphate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (45 ℃ of ether, vacuum 0.1MPa), cooling rapidly is through supersound process (59KHz, power 95%, 10min), get the Semen Coicis oil liposome turbid liquor, Semen Coicis oil liposome turbid liquor spray-dried (140 ℃ of inlet temperature, 70 ℃ of leaving air temps) promptly gets coix seed oil proliposome.
Embodiment 6
Semen Coicis oil 10g, Ovum Gallus domesticus Flavus lecithin 5g, ceramide 5g, cholesterol 0.5g, BHT0.003g, BHA0.002g, Myrij 0.5g, class of department 601.5g, cyclodextrin 15g, glucose 5g, ethanol 50mL, pH7.4 phosphate buffer 500mL.
Accurately take by weighing Semen Coicis oil in the above-mentioned prescription, Ovum Gallus domesticus Flavus lecithin, ceramide, cholesterol, BHT, BHA, Myrij, class of department 60, it is extremely molten in 40 ℃ of water-baths to add 50mL ethanol, get lipid soln, be injected in the phosphate buffer that 500mL is dissolved with cyclodextrin and glucose with constant flow pump while stirring, after this phosphate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (45 ℃ of ethanol, vacuum 0.1MPa), cooling rapidly, handle (16000psi through extra high pressure homogenize, circulate 3 times), get the Semen Coicis oil liposome turbid liquor, Semen Coicis oil liposome turbid liquor spray-dried (220 ℃ of inlet temperature, 110 ℃ of leaving air temps) promptly gets coix seed oil proliposome.
Embodiment 7
Semen Coicis oil 2g, Ovum Gallus domesticus Flavus lecithin 3g, cholesterol 1g, BHA0.001g, monoglyceride 0.5g, carboxymethyl chitosan 3g, ethanol 30mL, pH6.8 phosphate buffer 400mL.
Accurately take by weighing Semen Coicis oil in the above-mentioned prescription, Ovum Gallus domesticus Flavus lecithin, cholesterol, BHA, monoglyceride adds 150mL, it is extremely molten in 40 ℃ of water-baths to add 30mL ethanol, get lipid soln, be injected in the phosphate buffer that 400mL is dissolved with carboxymethyl chitosan with constant flow pump while stirring, after this phosphate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (45 ℃ of ethanol, vacuum 0.1MPa), cooling rapidly, through supersound process (59KHz, power 95%, 10min), get the Semen Coicis oil liposome turbid liquor, Semen Coicis oil liposome turbid liquor spray-dried (180 ℃ of inlet temperature, 80 ℃ of leaving air temps) promptly gets coix seed oil proliposome.
Embodiment 8
Semen Coicis oil 4g, distearoyl phosphatidylcholine 4g, two myristoyl phosphatidylcholine 14g, cholesterol 2g, V
CCetylate 0.001g, BHA0.001g, Brij 0.3g, polyvinylpyrrolidone 10g, chloroform 50mL, pH6.8 phosphate buffer 500mL.
Accurately take by weighing Semen Coicis oil in the above-mentioned prescription, distearoyl phosphatidylcholine, two myristoyl phosphatidylcholines, cholesterol, V
CCetylate, BHA, Brij, it is extremely molten in 50 ℃ of water-baths to add the 50mL chloroform, get lipid soln, be injected in the phosphate buffer that 500mL is dissolved with polyvinylpyrrolidone with constant flow pump while stirring, after this phosphate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (55 ℃ of chloroforms, vacuum 0.1MPa), cooling rapidly is through supersound process (59KHz, power 95%, 10min), get the Semen Coicis oil liposome turbid liquor, Semen Coicis oil liposome turbid liquor spray-dried (200 ℃ of inlet temperature, 90 ℃ of leaving air temps) promptly gets coix seed oil proliposome.
Embodiment 9
Semen Coicis oil 8g, hydrolecithin 4g, phosphatidylcholine 1g, phosphatidylinositols 1g, cholesterol 2g, BHT 0.01g, sodium cholate 3g, Macrogol 4000 2g, polyvinylpyrrolidone 1g, trehalose 1g, ether 50mL, pH7.0 phosphate buffer 300mL.
Accurately take by weighing Semen Coicis oil in the above-mentioned prescription, hydrolecithin, phosphatidylcholine, phosphatidylinositols, cholesterol, BHT, sodium cholate, it is extremely molten in 45 ℃ of water-baths to add ether 50mL, get lipid soln, be injected into 300mL with constant flow pump while stirring and be dissolved with Macrogol 4000, in the phosphate buffer of polyvinylpyrrolidone and trehalose, after this phosphate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (45 ℃ of ether, vacuum 0.1MPa), cooling rapidly, handle (15000psi through extra high pressure homogenize, circulate 2 times) handle, promptly get the Semen Coicis oil liposome turbid liquor, Semen Coicis oil liposome turbid liquor spray-dried (190 ℃ of inlet temperature, 85 ℃ of leaving air temps) promptly gets coix seed oil proliposome.
Embodiment 10
Semen Coicis oil 4g, hydrolecithin 25g, Ovum Gallus domesticus Flavus lecithin 10g, cholesterol 8g, TBHQ0.02g, polysorbate60 1g, polyoxyethylene hydrogenated Oleum Ricini 0.5g, chitosan 40g, ethanol 70mL, pH6.0 acetic acid-sodium-acetate buffer 400mL.
Accurately take by weighing Semen Coicis oil in the above-mentioned prescription, hydrolecithin, Ovum Gallus domesticus Flavus lecithin, cholesterol, TBHQ, polysorbate60, polyoxyethylene hydrogenated Oleum Ricini, it is extremely molten in 40 ℃ of water-baths to add ethanol 70mL, get lipid soln, be injected in acetic acid-sodium-acetate buffer that 400mL is dissolved with chitosan with constant flow pump while stirring, after this acetic acid-sodium-acetate buffer placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove (45 ℃ of ethanol, vacuum 0.1MPa), cooling rapidly, handle (20000psi through extra high pressure homogenize, circulate 1 time) handle, promptly get the Semen Coicis oil liposome turbid liquor, Semen Coicis oil liposome turbid liquor spray-dried (140 ℃ of inlet temperature, 70 ℃ of leaving air temps) promptly gets coix seed oil proliposome.
Claims (10)
1. a coix seed oil proliposome contains Semen Coicis oil, cholesterol, soybean lecithin component, it is characterized in that, the component of described pro-liposome also has surfactant, antioxidant, proppant, the multiple phospholipid except that soybean lecithin; The mass percent of each component is: Semen Coicis oil 1～50%, phosphatidase 13～75%, cholesterol 0.1～20%, surfactant 0.2～15%, antioxidant 0.001～4%, proppant 0.5～70%.
2. coix seed oil proliposome according to claim 1 is characterized in that: described pro-liposome is the pulverulent solids preparation.
3. coix seed oil proliposome according to claim 1 is characterized in that: described multiple phospholipid is one or more in Ovum Gallus domesticus Flavus lecithin, hydrolecithin, distearoyl phosphatidylcholine, Phosphatidylserine, phosphatidylinositols, PHOSPHATIDYL ETHANOLAMINE, phosphatidyl glycerol, phosphatidylcholine, dipalmitoyl phosphatidyl choline, two myristoyl phosphatidylcholines, the ceramide.
4. coix seed oil proliposome according to claim 1 is characterized in that: described surfactant is one or more in polyoxyethylene castor oil, polyoxyethylene hydrogenated Oleum Ricini, monoglyceride, sodium lauryl sulphate, Tween 80, polysorbate60, Brij, Myrij, sorbester p17, sorbester p18, sodium cholate, the sodium deoxycholate.
5. coix seed oil proliposome according to claim 1 is characterized in that: described antioxidant is V
E, V
CAmong cetylate, BHA (BHA), TBHQ (tertiarybutylhydroquinone), the BHT (dibenzylatiooluene) one or more.
6. coix seed oil proliposome according to claim 1 is characterized in that: described proppant is one or more in mannitol, glucose, polyvinyl alcohol 6000, sucrose, lactose, trehalose, polyvinylpyrrolidone, Macrogol 4000, chitosan, carboxymethyl chitosan, the cyclodextrin.
7. the preparation method of a coix seed oil proliposome is characterized in that preparation process is as follows:
(1) presses the component mass percent with Semen Coicis oil, phospholipid, cholesterol, antioxidant and surfactant organic solvent dissolution, make lipid soln;
(2) lipid soln that (1) is made is injected in the buffer solution that is dissolved with proppant, after this buffer solution placed on the shaking table vibration aquation 30min, be placed on the rotary evaporation in vacuo instrument rotary evaporation and remove organic solvent, rapidly after the cooling, through supersound process (59KHz, power 95%, 10min) or extra high pressure homogenize handle (15000～20000psi, circulate 1～3 time), make the Semen Coicis oil liposome turbid liquor;
(3) the Semen Coicis oil liposome turbid liquor of (2) being made is removed moisture through lyophilization or spray drying, promptly gets coix seed oil proliposome.
8. coix seed oil proliposome preparation method according to claim 7 is characterized in that: described organic solvent is a kind of in chloroform, ether, ethanol or the methanol.
9. coix seed oil proliposome preparation method according to claim 7 is characterized in that: described buffer comprises phosphate buffer, acetic acid-ammonium acetate buffer or acetic acid-sodium-acetate buffer, and pH of buffer is 6.0～7.4.
10. the preparation method of coix seed oil proliposome according to claim 7 is characterized in that: described spray drying is meant 140～220 ℃ of inlet temperature, carries out spray drying under 70～110 ℃ of the leaving air temps.
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