CN1965944A - Microsphere of dried tangerine peel oil and method for preparing same - Google Patents

Microsphere of dried tangerine peel oil and method for preparing same Download PDF

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Publication number
CN1965944A
CN1965944A CN 200610024327 CN200610024327A CN1965944A CN 1965944 A CN1965944 A CN 1965944A CN 200610024327 CN200610024327 CN 200610024327 CN 200610024327 A CN200610024327 A CN 200610024327A CN 1965944 A CN1965944 A CN 1965944A
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China
Prior art keywords
microcapsule
citri reticulatae
oleum citri
arabic gum
oleum
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CN 200610024327
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Chinese (zh)
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冯怡
徐德生
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Shanghai University of Traditional Chinese Medicine
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Shanghai University of Traditional Chinese Medicine
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Priority to CN 200610024327 priority Critical patent/CN1965944A/en
Publication of CN1965944A publication Critical patent/CN1965944A/en
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Abstract

The invention relates to a method for preparing tangerine peel oil capsule, wherein it comprises capsule material, strengthener, tangerine peel oil, emulsifier, and anti-adhesive agent at 0.5-1:0.05-0.1:0.2-1.2:0.025-0.05:0.01-0.05; atomizes and dries, to obtain the capsule at 7-30 mum. And the inventive capsule can reduce volatilization and improve stability. And it solidifies tangerine peel oil, to support storage and transmission.

Description

A kind of Oleum Citri Reticulatae microcapsule and preparation method thereof
Technical field
The present invention relates to the Chinese medicine preparation technical field, be specifically related to a kind of Oleum Citri Reticulatae microcapsule and preparation method thereof.
Background technology
Volatile oil be in the plant class can with steam distillation and with the general name of the not miscible multiple mixture that becomes to be grouped into of water.Volatile oil mainly is monoterpene and sesquiterpene and oxygenatedchemicals thereof, and is responsive to air, daylight and Temperature Influence, is easy to decompose rotten.Volatile oil is the oily liquids with special and strong abnormal smells from the patient under normal conditions, can wave diffusingly under the room temperature, contains a large amount of volatile oil in the Chinese crude drug and play the pharmacological action of outbalance in its prescription.Therefore volatile oil being reduced the loss, keep its stability, is the problem of paying close attention to during Chinese medicine preparation is produced.Among the preparation technology of dosage forms such as traditional solid preparation such as tablet, granule, capsule, after often volatile oil being dissolved in the dilution of small amount of ethanol equal solvent, be sprayed onto in the dried granule, after having 38 kinds of volatile oil to extract separately in one one of 05 year version pharmacopeia, according to above-mentioned production technology production, but this production process very easily makes the volatile oils loss, and is difficult to guarantee the stability of volatile oil in storage and application process.In recent years, it is a lot of that the application beta-schardinger dextrin-prepares the research of volatile oil clathrate compound, but this method is comparatively loaded down with trivial details, and drug loading is on the low side.
The Chinese medicine Pericarpium Citri Reticulatae is a conventional Chinese medicine, the main volatile oil that contains, and wherein principal component has limonene, γ-Song Youxi, β-moon to hang alkene, alpha-terpineol etc., and fragrant spleen invigorating, the wind dispelling therapeutic method to keep the adverse QI flowing downwards can be treated the weakness of the spleen and stomach stagnation of QI; And can eliminate the phlegm and regulate the flow of vital energy.How preserving the active ingredient in the Oleum Citri Reticulatae to greatest extent in the preparation process, and improve volatile oil stability in storage and application process, is the content that the present invention studies.
Summary of the invention
Technical problem to be solved by this invention, be to adopt microcapsule technology, reduce the loss of Oleum Citri Reticulatae volatile component in preparation is produced, but provide a kind of production technology of volatile oil microcapsule of feasible process industrialization, and make the volatile oil solid state, be convenient to transportation for follow-up preparation production provides a kind of, store stay-in-grade intermediate products Oleum Citri Reticulatae microcapsule.
Oleum Citri Reticulatae microcapsule disclosed by the invention is to be the capsule material by weight ratio: the emulsion that plasticizer: Oleum Citri Reticulatae: emulsifying agent: antiplastering aid=0.5-1: 0.05-0.1: 0.2-1.2: 0.025-0.05: 0.01-0.05 makes, the particle diameter that spray-dried back obtains is at the microcapsule of 7-30 μ m.
Oleum Citri Reticulatae of the present invention is the commercially available prod, mainly contains limonene, γ-Song Youxi, hangs compositions such as alkene, alpha-terpineol by β-moon.
Capsule material of the present invention is selected from water-soluble high-molecular materials such as arabic gum, chitosan, sodium alginate, ethyl cellulose, methylcellulose, hydroxypropyl emthylcellulose, phthalic acid diacetate fiber ester (CAP), cross-linked carboxymethyl cellulose (SCMC) and cyclodextrin, or is selected from mictocystis materials such as arabic gum-gelatin, arabic gum-maltodextrin, arabic gum-sodium alginate.
Described plasticizer is selected from glycerol, Polyethylene Glycol and propylene glycol.
Described emulsifying agent is selected from span, tween and Pa Luoshamu.
Described antiplastering aid is selected from magnesium stearate, micropowder silica gel and Pulvis Talci.
Oleum Citri Reticulatae microcapsule of the present invention is specifically made by following method:
Get the capsule material by said ratio and add the solution that water is mixed with 5%-25% (w/v) concentration, add plasticizer, Oleum Citri Reticulatae and emulsifying agent successively, make Emulsion through emulsifying, add the antiplastering aid mix homogeneously, by peristaltic pump emulsion solution is sucked and be spray dried to microcapsule in the spray dryer; Wherein the spray drying technology parameter is: injector temperature is 130-155 ℃, and atomisation pressure is 24-38m 2/ h, sample introduction speed is 5-20ml/min.
Emulsifying machinery the best that emulsifying is adopted is dispersing emulsification machine, colloid mill, also can adopt magnetic stirrer and tissue refiner.
In the microcapsule preparation process, add a certain amount of plasticizer and can reduce the microcapsule gathering, make it adhesion, good dispersion.The Oleum Citri Reticulatae microcapsule that makes with the inventive method is spherical in shape under electron-microscope scanning is observed, smooth surface or matrix slightly, and particle diameter 7-30 μ m, drug loading and envelop rate are better, discharge very fast.Through comparing with the technology of other preparation microcapsules, the Oleum Citri Reticulatae microcapsule that the present invention adopts spray drying method to make has the big characteristics of drug loading: Pericarpium Citri Reticulatae volatile oil is 7.8% through its drug loading of beta-cyclodextrin inclusion compound; The volatile oil microcapsule drug loading for preparing with complex coacervation is: 9-15%, and the drug loading of the microcapsule that the present invention prepares reaches 28.3%.
Oleum Citri Reticulatae microcapsule preparation method of the present invention is verified through pilot plant test, mature preparation process, steady quality.Through the preliminarily stabilised investigation, without under the Packing Condition, Pericarpium Citri Reticulatae volatile oil and see Table 1 in the microcapsule without encapsulation Pericarpium Citri Reticulatae volatile oil retention rate.
Table 1. Pericarpium Citri Reticulatae volatile oil retention rate (the 0-2 month)
0 month volatile oil retention rate (%) Volatile oil retention rate in January (%) Volatile oil retention rate in February (%)
Encapsulation not behind the microencapsulation 28.32±1.43 3.37±0.35 26.14 ± 1.56 do not detect 23.19 ± 1.11 do not detect
The present invention adopts the microencapsulation technology of spray drying method to prepare the Oleum Citri Reticulatae microcapsule, and is simple to operate, and process stabilizing is fit to big production.Because Oleum Citri Reticulatae is wrapped in the small spherical capsule, thereby reduced volatile oils, improved volatile oil stability, and make the Oleum Citri Reticulatae solid state, be convenient to store, transport, can be used as the intermediate of medicine and daily chemicals, be applied to pharmaceutical production, can further make various dosage forms such as tablet, capsule, granule, gel, suppository.
The specific embodiment
Embodiment 1
Get gum arabic powder 18g, with water dissolution and be made into 6% (w/v) concentration 300ml, add glycerol 3.6g, Oleum Citri Reticulatae 36g, tween 1.8g after the tissue refiner stirring and emulsifying, adds micropowder silica gel 1.8g again, stirs down, by 145 ℃ of inlet temperature, 85 ℃ of leaving air temps, atomisation pressure are 25m 2/ h, the process conditions of charging rate 20ml/min are carried out spray drying, promptly.Record drug loading 28.15%.
Embodiment 2
Getting sodium alginate is sprinkled on the liquid level in the container that 150ml water is housed swelling in right amount and becomes 5% (w/v) solution one night; Get the 7.5g gum arabic powder again with water dissolution and be made into 5% (w/v) concentration 150ml, and with above-mentioned sodium alginate soln mix homogeneously; At mixed liquor at middle adding glycerol 0.9g, Oleum Citri Reticulatae 14.5g, span 0.5g after colloid mill emulsifying evenly, adds micropowder silica gel 0.2g again, stirs down, by 145 ℃ of inlet temperature, 85 ℃ of leaving air temps, atomisation pressure are 38m 2/ h, the process conditions of charging rate 20ml/min are carried out spray drying, promptly.Record drug loading 25.92%.
Embodiment 3
Get methylcellulose 15g, with water dissolution and be made into 5% (w/v) concentration 300ml, in mixed liquor, add Polyethylene Glycol 1.5g, Oleum Citri Reticulatae 3g, span 0.4g, after the tissue refiner stirring and emulsifying, add Pulvis Talci 0.15g again, stir down, by 155 ℃ of inlet temperature, 90 ℃ of leaving air temps, atomisation pressure are 38m 2/ h, the process conditions of charging rate 10ml/min are carried out spray drying, promptly.Calculating drug loading is 27.82%.
Embodiment 4
Get cyclodextrin 15g, with water dissolution and be made into 15% (w/v) concentration 100ml, in mixed liquor, add Polyethylene Glycol 2g, Oleum Citri Reticulatae 18g, tween 0.75g, after the tissue refiner stirring and emulsifying, add magnesium stearate 0.3g again, stir down, by 130 ℃ of inlet temperature, 80 ℃ of leaving air temps, atomisation pressure are 30m 2/ h, the process conditions of charging rate 15ml/min are carried out spray drying, promptly.Calculating drug loading is 25.39%.
Embodiment 5
Get hydroxypropyl emthylcellulose-100 18g, with water dissolution and be made into 25% (w/v) concentration 60ml, in mixed liquor, add glycerol 1.5g, Oleum Citri Reticulatae 10g, Pa Luoshamu 0.5g, after the tissue refiner stirring and emulsifying, add magnesium stearate 0.18g again, stir down, by 155 ℃ of inlet temperature, 90 ℃ of leaving air temps, atomisation pressure are 30m 2/ h, the process conditions of charging rate 10ml/min are carried out spray drying, promptly.Calculating drug loading is 27.53%.
Embodiment 6
Get ethyl cellulose 15g, with water dissolution and be made into 10% (w/v) concentration 150ml, in mixed liquor, add Polyethylene Glycol 2g, Oleum Citri Reticulatae 18g, span 1.5g, after the tissue refiner stirring and emulsifying, add micropowder silica gel 0.3g again, stir down, by 155 ℃ of inlet temperature, 90 ℃ of leaving air temps, atomisation pressure are 30m 2/ h, the process conditions of charging rate 15ml/min are carried out spray drying, promptly.Calculating drug loading is 28.45%.

Claims (6)

1, a kind of Oleum Citri Reticulatae microcapsule, it is characterized in that this microcapsule is is the capsule material by weight ratio: the emulsion that plasticizer: Oleum Citri Reticulatae: emulsifying agent: antiplastering aid=0.5-1: 0.05-0.1: 0.2-1.2: 0.025-0.05: 0.01-0.05 makes, the particle diameter that spray-dried back obtains is at the microcapsule of 7-30 μ m.
2, Oleum Citri Reticulatae microcapsule according to claim 1 is characterized in that wherein said capsule material is selected from arabic gum, chitosan, sodium alginate, ethyl cellulose, methylcellulose, hydroxypropyl emthylcellulose, phthalic acid diacetate fiber ester, cross-linked carboxymethyl cellulose, cyclodextrin, arabic gum-gelatin, arabic gum-maltodextrin and arabic gum-sodium alginate.
3, Oleum Citri Reticulatae microcapsule according to claim 1 is characterized in that wherein said plasticizer is selected from glycerol, Polyethylene Glycol and propylene glycol.
4, Oleum Citri Reticulatae microcapsule according to claim 1 is characterized in that wherein said emulsifying agent is selected from span, tween and Pa Luoshamu.
5, the preparation method of Oleum Citri Reticulatae microcapsule according to claim 1 is characterized in that wherein said antiplastering aid is selected from magnesium stearate, micropowder silica gel and Pulvis Talci.
6, the preparation method of the described Oleum Citri Reticulatae microcapsule of a kind of claim 1 is characterized in that this microcapsule is made by following method:
Getting the capsule material by proportioning adds water and is mixed with the solution that bulking value concentration is 5%-25%, add plasticizer, Oleum Citri Reticulatae and emulsifying agent successively, make Emulsion through emulsifying, add the antiplastering aid mix homogeneously, by peristaltic pump emulsion solution is sucked and be spray dried to microcapsule in the spray dryer; Wherein the spray drying technology parameter is: injector temperature is 130-155 ℃, and atomisation pressure is 24-38m 2/ h, sample introduction speed is 5-20ml/min.
CN 200610024327 2006-03-03 2006-03-03 Microsphere of dried tangerine peel oil and method for preparing same Pending CN1965944A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102783617A (en) * 2012-07-30 2012-11-21 无限极(中国)有限公司 Dried orange peel extract micro-capsule powder as well as preparation method and application of dried orange peel extract micro-capsule powder
CN105076612A (en) * 2015-09-01 2015-11-25 广州蓓而泰生物科技有限公司 Preparation method of instant tangerine peel oil tea powder and product of instant tangerine peel oil tea powder
CN106967507A (en) * 2017-03-10 2017-07-21 佛山市禅香新材料有限公司 It is a kind of for lavender transparency liquid microcapsules of preserved flower and preparation method thereof
CN107569468A (en) * 2017-09-20 2018-01-12 辽宁上药好护士健康科技有限公司 Ginseng essential oil micro-capsule and preparation method thereof
CN111346162A (en) * 2020-03-20 2020-06-30 鲁南制药集团股份有限公司 Children's food retention removing and cough relieving micro-capsule preparation and preparation method thereof
CN112385839A (en) * 2019-10-16 2021-02-23 富诺健康股份有限公司 Lutein ester microcapsule and preparation method thereof
WO2021184636A1 (en) * 2020-03-20 2021-09-23 鲁南厚普制药有限公司 Shouhui tongbian microcapsule preparation and preparation method therefor

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102783617A (en) * 2012-07-30 2012-11-21 无限极(中国)有限公司 Dried orange peel extract micro-capsule powder as well as preparation method and application of dried orange peel extract micro-capsule powder
CN105076612A (en) * 2015-09-01 2015-11-25 广州蓓而泰生物科技有限公司 Preparation method of instant tangerine peel oil tea powder and product of instant tangerine peel oil tea powder
CN106967507A (en) * 2017-03-10 2017-07-21 佛山市禅香新材料有限公司 It is a kind of for lavender transparency liquid microcapsules of preserved flower and preparation method thereof
CN107569468A (en) * 2017-09-20 2018-01-12 辽宁上药好护士健康科技有限公司 Ginseng essential oil micro-capsule and preparation method thereof
CN107569468B (en) * 2017-09-20 2021-02-05 辽宁上药好护士健康科技有限公司 Ginseng volatile oil microcapsule and preparation method thereof
CN112385839A (en) * 2019-10-16 2021-02-23 富诺健康股份有限公司 Lutein ester microcapsule and preparation method thereof
CN112385839B (en) * 2019-10-16 2022-11-08 富诺健康股份有限公司 Lutein ester microcapsule and preparation method thereof
CN111346162A (en) * 2020-03-20 2020-06-30 鲁南制药集团股份有限公司 Children's food retention removing and cough relieving micro-capsule preparation and preparation method thereof
WO2021184636A1 (en) * 2020-03-20 2021-09-23 鲁南厚普制药有限公司 Shouhui tongbian microcapsule preparation and preparation method therefor
WO2021184639A1 (en) * 2020-03-20 2021-09-23 山东新时代药业有限公司 Microcapsule preparation for eliminating food stagnation and relieving coughs in children and preparation method therefor
CN111346162B (en) * 2020-03-20 2021-12-14 鲁南制药集团股份有限公司 Children's food retention removing and cough relieving micro-capsule preparation and preparation method thereof

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