CN1067548C

CN1067548C - Preparation and application of β-carotene or carotenoid microcapsules

Info

Publication number: CN1067548C
Application number: CN94112026A
Authority: CN
Inventors: 忻祥法; 王玉苓
Original assignee: Shanghai No6 Pharmaceutical Factory
Current assignee: Shanghai No6 Pharmaceutical Factory
Priority date: 1994-01-21
Filing date: 1994-01-21
Publication date: 2001-06-27
Anticipated expiration: 2014-01-21
Also published as: CN1109329A

Abstract

β-胡萝卜素或类胡萝卜素制成微型胶囊后能提高稳定性，从而扩大了它们的用途。本发明提供了β-胡萝卜素或类胡萝卜素微型胶囊的制备方法及其在水生生物或家畜、家禽饲养或装入胶壳中成为保健用硬胶囊等方面的应用。Microencapsulation of beta-carotene or carotenoids increases their stability and thus expands their usefulness. The invention provides a preparation method of beta-carotene or carotenoid microcapsules and its application in raising aquatic organisms or domestic animals or poultry or filling them into hard capsules for health care and the like.

Description

The preparation of beta-carotene or carotene micro capsule and application

Have 9 conjugated double bonds in the molecular structure of beta-carotene or carotenoid, thereby they are to light, heat, oxygen, wet etc. very responsive, in processing with use and very easily fall during storage

K.MunZel etc. are at Pharm, Acta, Helv, 1969,44, and 208 had reported once that the beta-carotene crystalline solid reduces easily in put procedure tires, and after tested, tiring after three months almost reduces to zero.See the following form:

Table one beta-carotene crystalline solid is tired and is tired 100% 66% 22.3% 10.6% 0% after original 8 days of the date over time after 1 month after 2 months after 3 months

The objective of the invention is to improve the stability of beta-carotene or carotenoid, and enlarge its range of application.

The present invention adopts complex coacervation that thereby beta-carotene or carotenoid are made microencapsulation raising stability.

Though the complex coacervation preparation technique has report, as Luzzi etc., J.Pharm-Sci.53,429 (1964), be applied to that the beta-carotene product is made beta-carotene or carotene micro capsule is that the present invention initiates.

The present invention at first provides β-Radix Dauci Sativae rope or class Radix Dauci Sativae rope microencapsulation.This capsule is to be active ingredient and medicinal (or edible) carrier by beta-carotene or class Radix Dauci Sativae rope, and containing beta-carotene or carotenoid by weight and be 0.01～99.9% is that 99.9%～0.01% arbitrary proportion is prepared from 100% composition with containing carrier.Carrier wherein is vegetable and animals oils, anion glue, two property ion glue, sucrose etc.

Another object of the present invention provides the preparation method of beta-carotene or carotene micro capsule.

Method of the present invention is that β-Radix Dauci Sativae rope is suspended in vegetable and animals oils or other oil, with anion glue is the capsule heart, coated with two property ion glue, at the following acidity encystation of isoelectric point, IP, adopt cryogenic temperature condensation and liquid-solid fixed again, filter, washing with aldehyde, soak the back granulating with sucrose solution again, dry and beta-carotene or carotenoid capsule.

The invention discloses the preparation method of beta-carotene or carotene micro capsule:

(1) preparation emulsion:

The animal and vegetable oil that beta-carotene or carotenoid is added 10～30 times of amounts grinds to form suspension, be heated to 30～60 ℃, with 50 ℃ of the bests, add 10～40% anion glue solutions then, wherein the weight ratio of vegetable and animals oils and anion glue is 1: 0.4～0.8, with 0.5 the best, be heated to 30～60 ℃, this mixed liquor is put into emulsator make emulsion;

(2) preparation β-Radix Dauci Sativae rope or carotene micro capsule:

In the encystation device, add earlier and be preheated to water 200～400ml of 30～60 ℃, the emulsion that adds above-mentioned (1) preparation again, add 10～40% two property glue solutions then, the weight ratio of this two property glue and above-mentioned anion glue is 1: 0.8～1.2, with 1: 1 the best, stir the clarification back and regulate PH to 3～5 with acid, add entry 200～400ml simultaneously, the consumption of water is 1.2～5 parts (weight) of anion glue herein, with 1.5 parts of the bests, be cooled to below 20 ℃, add 1～2 times to the aldehyde solution of anion glue amount with the amount of 1.2 times of the bests, the reuse sodium hydroxid is regulated PH to 8～9, continue to be cooled to below 5 ℃, stir after-filtration, be washed with water to neutrality, refilter, stir in the sucrose solution with filtrate immersion 50～80% then, after the filtration, add the magnesium stearate of 1～5% amount in the filter cake, granulating, oven dry promptly gets beta-carotene or carotene micro capsule.

Used anion glue is arabic gum, Resina persicae and other natural gum among the present invention; Used two property glue are gelatin, osseocolla and other animal skin glue; Used animal and vegetable oil is Oleum Arachidis hypogaeae semen, Oleum Glycines, fish oil or other is as the paraffin wax wet goods; Used acid is common acid such as acetic acid, hydrochloric acid; Used aldehydes is formaldehyde or other aldehydes etc.

The beta-carotene of the present invention's preparation or the stability of carotene micro capsule significantly increase, and for example with 1% beta-carotin microcapsule, reinstall one-tenth hard capsule for health care in the glue shell.Its stability sees the following form:

The microcapsule 100% 95% 90% 88% 85% duricrust microcapsule 100% 98% 95% 92% 90% of packing into of tiring after 1 year after 9 months after 6 months after original 3 months of the stable date of table two 1% beta-carotin microcapsule and hard capsule

It is bigger to this shows that stability improves, and can meet the requirement of guaranteeing the quality a year.

Another purpose of the present invention has provided the application of beta-carotene microencapsulation.

Improve by the stability of hands beta-carotene or carotene micro capsule, be applied to aquatile and domestic animal, poultry etc., can not only promote growth, resist disease, can also increase in body colour and the ovum egg colour generation etc. as feed additive.See Table three table three beta-carotene and other structural carotenoid and purposes

In addition, β-Radix Dauci Sativae rope or carotenoid are made microcapsule, and reinstalling to become hard capsule for health care (seeing Table two) in the glue shell.

Embodiment one to seven:

Embodiment one preparation beta-carotin microcapsule

Beta-carotene 1.5g is added the 30ml vegetable oil to grind to form suspension and is heated to 50 ℃.The clear and bright liquid that adds 14g arabic gum and 200ml water composition more also is heated to 50 ℃.Enter emulsator jointly and become emulsion (1).In the encystation device, add 5O ℃ of water 200ml of preheating earlier, add above-mentioned emulsion (1) again, the back adds the 14g gelatin and 200ml water is formed clear and bright liquid, adjust it with acetic acid and add thinned water 300ml simultaneously to subacidity (PH=4.1), add formaldehyde (37%) 18ml after being cooled to 15 ℃, reuse 20%NaOH regulator solution (PH=8) is to alkalescence, continue to be cooled to 5 ℃, stirred 1 hour.Filtration is washed with water to neutrality, refilters, and wet capsule immerses 210g sucrose and 90ml water is formed in the liquid glucose, and 25 ℃～30 ℃ were stirred 1 hour.Refilter, add magnesium stearate 6g granulating, oven dry, 60 ℃ of temperature controls, get beta-carotin microcapsule 130g, content 1%, moisture content＜3%, yield: 86.6% at 6～10 hours time.

Embodiment two preparation beta-carotin microcapsules

One operation change beta-carotene throwing amount result is as follows with example: (1) throws the 11g beta-carotene, after the processing: 120g80% microcapsule yield: 87.2%.(2) throw the 13g beta-carotene, after the processing: 115g, 100% microcapsule yield: 84.6%.(3) throw the 0.14g beta-carotene, after the processing: 125g, 0.1% microcapsule yield: 89.3%.

Embodiment three preparation carotenoid microcapsules change its initiation material (replacement beta-carotene) with example one operation, draw following product

	Initiation material	Feed intake	Title	Product
				Product			Quantity	Content	Yield
				1	α-carotene	1.5g	The alpha-carotene microcapsule	130g	1%	86.6%
2	Phylloxanthin	1.5g	Xanthin micro-capsule	125g	1%	83.3%
3	Cantharides xanthin	1.5g	The cantharides xanthin microcapsule	120g	1%	80.0%
4	Astaxanthin	1.5g	The astaxanthin microcapsule	128g	1%	85.3%
★ 5	Cryptoxanthin	1.5g	The cryptoxanthin microcapsule	120g	1%	80.0%

★ beta-cryptoxanthin, lycopene, batching and productive rate are with example 5.

Embodiment four beta-carotin microcapsules are as the application of feed additive

With 1% beta-carotin microcapsule 6g, mix the 1Kg prawn and raise with in the common dry feed, to press constant and fed preceding 60 days of harvest time, test group increases weight more than 30% than matched group.

With three mu of ponds is example:

The test pool: gross output 422.68Kg, per unit area yield 140.96Kg/ mu, specification 60 tails/Kg.

The contrast pool: gross output 306Kg, per unit area yield 102Kg/ mu, specification 76.8 tails/Kg.

Embodiment five beta-carotin microcapsules improve the test of egg yolk element

1% beta-carotin microcapsule 3g is mixed the 1Kg laying hen with in the common dry feed, feed more than 6 weeks, the egg yolk element that produces can improve 1.5 Luo Shi ColourIndex numbers.

The application of embodiment six beta-carotene in Carassius auratus is raised

1% beta-carotin microcapsule 2g is mixed in the 1Kg goldfish bait, and it is as follows that (common dried bait) raises after three months the result:

Test group 200 tails, complete red five tails of result; Half red 9 tails; Raising rate: 0.

Matched group 200 tails, complete red 20 tails of result; Half red 15 tails; Raising rate: 150%.

The application of embodiment seven beta-carotin microcapsules in the steamed bun fish is raised

With 1% beta-carotin microcapsule 6g, mix 1Kg, (common in bait) was through 60 days feeding trials in the Anguillar japonica bait.Test group increases weight more than 30% than matched group.

Test group: the former 123Kg that puts in a suitable place to breed, results 376.5Kg, survival rate: 96.4%

Matched group: the former 123Kg that puts in a suitable place to breed, results 298.4Kg, survival rate: 94.8%

Claims

1. A β-carotene or carotenoid microcapsule, characterized in that the microcapsule is composed of β-carotene or carotenoid as an active ingredient and a medicinal or edible carrier by weight to contain β-carotene or 0.01-99.9% of carotenoids and 99.9%-0.01% of carriers are prepared in arbitrary proportions through a complex coacervation method to form a 100% composition.

2. A method for preparing β-carotene or carotenoid microcapsules as claimed in claim 1, characterized in that it comprises the following steps: (1) preparing an emulsion:

Grind β-carotene or carotenoid with 10 to 30 times the amount of animal and vegetable oils to form a suspension, heat to 30 to 60°C, and then add 10 to 40% anionic gum aqueous solution, wherein the weight of animal and vegetable oils and anionic gum The ratio is 1:0.4~0.8, heated to 30~60°C, put the mixed solution into an emulsifier to make an emulsion; (2) Prepare β-carotene or carotenoid microcapsules:

First add 200-400ml of water preheated to 30-60°C into the capsule forming device, then add the emulsion prepared in (1) above, and then add 10-40% amphoteric gum aqueous solution, the amphoteric gum and the above-mentioned anion The weight ratio of glue is 1: 0.8～1.2, after stirring and clarification, adjust pH to 3～5 with acid, add water 200～400ml simultaneously, the consumption of water here is 1.2～5 parts (weight) of anionic glue solution, cool to Below 20°C, add aldehyde solution 1 to 2 times the amount of anionic glue, then adjust the pH to 8~9 with sodium hydroxide, continue cooling to below 5°C, filter after stirring, wash with water until neutral, and then filter. Then immerse the filtrate in 50-80% sucrose solution, stir and filter, add 1-5% magnesium stearate into the filter cake, chisel and dry to obtain beta-carotene or carotenoid microcapsules.

3. The β-carotene or carotenoid microcapsules according to claim 1, wherein said pharmaceutical or edible carrier is anionic gum, amphoteric gum, oil, sucrose.

4. The preparation method of β-carotene or carotenoid microcapsules according to claim 2, wherein said anionic gum is gum arabic or peach gum; amphoteric gum is gelatin or bone glue; oil is peanut oil, soybean oil or fish oil; acid is acetic acid or hydrochloric acid; aldehyde is formaldehyde.