专利摘要:
Capsules containing two phases and procedure for obtaining them. The present invention relates to capsules coated with a film of calcium alginate containing two phases immiscible or partially miscible with each other, such as for example an aqueous phase and a hydrophobic phase or a liquid phase and a solid phase. In addition, the present invention also relates to the process by which it is possible to encapsulate and maintain said two phases stable within the formed capsule. (Machine-translation by Google Translate, not legally binding)
公开号:ES2541504A1
申请号:ES201530738
申请日:2015-05-27
公开日:2015-07-20
发明作者:Ramón RAMÓN REAL;Ramón María RAMÓN FERRES
申请人:Caviaroli SL;
IPC主号:
专利说明:

DESCRIPTION

Capsules containing two phases and procedure for obtaining them.

The present invention relates to capsules coated with a calcium alginate film 5 containing two immiscible or partially miscible phases, such as for example an aqueous phase and a hydrophobic phase or a liquid phase and a solid phase. In addition, the present invention also relates to the method by which it is possible to encapsulate and keep said two phases within the formed capsule.
 10
The inventor of the present patent is not aware that there are capsules coated with calcium alginate in which two immiscible or partially miscible phases are present inside.

The biphasic capsules of the present invention can be obtained by a method commonly referred to as "spherification" either by direct spherification or by reverse spherification.

In direct spherification on an industrial scale, for example, the substance to be encapsulated and a non-calcium alginate solution are pumped through two concentric tubes with about 20 flow rates so that a drop of the substance to be encapsulated wrapped by a film of the non-calcium alginate solution, which acts as a gelling agent. It is also possible to mix the alginate with the substance to be encapsulated. This drop falls into a bath that contains a source of calcium ions, forming a gel layer that contains the material to be encapsulated. Said film is formed almost instantaneously on the outside, being semi-solid and gelatinous, and it keeps the encapsulated substance inside it, in solid form if it allows the migration of calcium ions and in liquid form if it does not allow the migration of calcium ions.

An industrial spherification process is disclosed, for example, in the application of PCT Patent WO 2009/109681 A1, in which food products, such as fruit pulp, are encapsulated, said food products being always encapsulated in aqueous base, is say, that the substance to be encapsulated is hydrophilic.

On the other hand, in reverse spherification the substance to be encapsulated is mixed with a source of calcium or magnesium ions, for example, calcium chloride or other calcium salt. Next, a drop or any other form is formed with said mixture of substance to be encapsulated and calcium or magnesium ions and introduced into a solution containing non-calcium alginate, for example, sodium alginate. Upon contacting the formed drop containing calcium ions with the solution containing alginate, a semi-solid and gelatinous outer film of calcium alginate is formed almost instantaneously, which keeps the substance to be encapsulated inside.

The inventor of the present patent, after exhaustive studies, has developed a spherification process by means of which it is possible to industrially obtain capsules containing two substances that form two immiscible or partially miscible phases, with a surprisingly spherical shape and, furthermore, it is possible to obtain a diameter of said capsules up to 50 mm in diameter without affecting the sphericity thereof, preferably in the range of 5 mm to 50 mm, more preferably 10 mm to 50 mm, even more preferably 15 mm at 50 mm, from 20 mm to 50 mm, from 25 mm to 50 mm and 50 more preferably from 30 mm to 50 mm.

The process of the present invention is based on the use of two concentric tubes that form the droplet of the two phases to be encapsulated and the gelling solution, being
It is necessary that the substance applied by the outer tube comprises a source of calcium or magnesium ions. The elaboration of the biphasic capsules is carried out by a procedure known as reverse spherification with some variations.

Therefore, the present invention discloses a process for preparing capsules 5 of biphasic substances, characterized in that it comprises the following steps:

a) preparation of the aqueous non-calcium alginate solution in which the alginate concentration is in the range of 0.05% to 5% by weight of the solution;
b) preparation of the substances that will form the two phases to be encapsulated in which one of said substances comprises a source of calcium or magnesium ions;
c) application of the substances that will form the two phases to be encapsulated through concentric tubes, it being necessary that through the outer tube the substance comprising the source of calcium or magnesium ions be applied;
d) introduction of the drop or drops formed in step (c) into the aqueous solution containing alginate, in which the outer layer of the drop reacts forming at least one sphere containing both phases;
e) wash, drain and pack the capsules formed in step (d).

The process of the present invention can be used both in the food industry, as well as in the cosmetic, intra-pharmaceutical, chemical, pharmaceutical and any other industry that requires these types of capsules.

In addition, the process of the present invention makes it possible to obtain two-phase spheres but, obviously, one skilled in the art could carry out said encapsulation of spheres with two phases by other known methods, such as direct spherification or other variants of reverse spherification.

In the present invention biphasic substances are understood as two substances that are immiscible or partially miscible with each other. They can be organic or inorganic substances as long as they comply with the above.

It is further understood that the term biphasic herein refers to two phases that are immiscible or partially miscible with each other, and can encompass both liquid, liquid-solid phases whose solid can be obtained with or without reaction, liquid- gas, even a person skilled in the art could use additives to emulsify the encapsulated solutions and obtain two-phase spheres that are more stable over time. Finally, it is also within the scope of the present invention two-phase spheres obtained by freezing one or both phases and subsequent direct or reverse spherification reaction, by a method known as freezing spherification. Also included in the scope of protection are two 40 phases that are separated by an alginate film, or even a previously formed alginate sphere incorporated into the sphere that will be subsequently formed by the process of the present invention. For example, an oil sphere obtained by direct spherification can be included in a vinegar solution with a calcium source, which after contact with alginate creates a sphere surrounded by an alginate film that includes said oil sphere inside . Likewise, a solid phase of a frozen or gelled product that is incorporated into said calcium-rich solution can be included for subsequent gelation.

In the case of the cosmetic industry, paraffins, petrolatum, 50 vegetable oils, waxes, fatty alcohols and their esters, lanolin and silicones, and mixtures thereof can be used as the oil phase.

In the case of the food industry, two-phase spheres can be obtained, for example vinegar-oil, soy sauce-sesame oil, mustard-olive oil, honey-olive oil, coffee-chocolate, among others. One skilled in the art will understand that any combination of substances that form two immiscible or partially miscible phases can be used to encapsulate according to the process of the present invention. 5

In addition, said immiscible or partially miscible substances can be mixed with dressings, aromas, flavors and other oil-soluble additives.

It is evident to one skilled in the art that the aqueous solution containing calcium ions 10 used in the process of the present invention can be any source of calcium ions, provided it is capable of forming a calcium alginate gel that forms the outer film of the capsule. Among such sources of calcium ions can be mentioned, for example, calcium chloride, calcium lactate, calcium gluconate, or a mixture thereof. Preferably, the source of calcium ions is calcium chloride. fifteen

In addition, said calcium ion solution can contain any type of additive or it can be mixed with any raw material that allows modifying the organoleptic characteristics of the capsule obtained.
 twenty
The alginate solution of the process of the present invention can be any non-calcium alginate salt, provided it reacts in the presence of calcium ions and forms the outer calcium alginate film of the capsules. Preferably, the alginate used is sodium alginate. The pH of the alginate solution is between 2 and 14.
 25
An additional advantage of the process of the present invention is that all steps are performed at room temperature. An increase or decrease of the temperature, in addition to the increase in the production costs of the capsules, can affect the viscosity, density and surface tension of the oily and aqueous phases present in the process, so it would also be necessary to modify various parameters of the process to obtain the same 30 results as at room temperature.

EXAMPLES

Example 1. Preparation of biphasic vinegar-olive oil capsules according to the method 35 of the present invention.

A commercial vinegar was taken and 1.2% by weight xanthan gum, 3% by weight calcium lactate was added. In addition, a 0.4% by weight sodium alginate solution was prepared. For the second phase extra virgin olive oil was used. 40

Drops containing olive oil inside and the prepared vinegar solution outside were generated through two concentric tubes and introduced into the sodium alginate solution in a room temperature bath. Said drops were collected and placed in a bath with water for washing them. They were drained and packaged. At least one 45 mm diameter capsule was obtained, containing two phases of olive oil and vinegar.

Example 2. Preparation of biphasic soybean-sesame oil capsules.
 fifty
A commercial soy sauce was taken and 1% xanthan gum was added, 1% calcium chloride by weight was added. In addition, a 0.5% by weight sodium alginate solution was prepared. Sesame oil was used for the second phase.

Drops containing sesame oil inside and the prepared soy sauce solution outside were generated through two concentric tubes and introduced into the sodium alginate solution in a room temperature bath. Said drops were collected and placed in a bath with water for washing them. They were drained and packed. 22 mm diameter capsules were obtained, containing two phases of sesame oil and soy sauce.

Example 3. Preparation of two-phase capsules of jojoba oil and caffeine.

A 0.2% by weight caffeine solution was taken and 0.8% calcium chloride by weight was added. In addition, a 0.9% by weight sodium alginate solution was prepared. For the second phase, jojoba oil containing Vitamin E 0.05% by weight was used.

Drops containing jojoba oil and Vitamin E inside and the prepared caffeine solution outside were generated through two concentric tubes, and sodium alginate solution was introduced into a room temperature bath. Said drops were collected and placed in a bath with water for washing them. They were drained and packed. At least one 16 mm diameter capsule was obtained, which contained two phases of jojoba oil with Vitamin E and caffeine.
 twenty
Example 4. Preparation of biphasic solid-liquid capsules

A solution containing coffee, 1% by weight xanthan gum was prepared and 0.2% by weight calcium chloride was added. In addition, liquid chocolate was prepared and 0.2% sodium alginate was added. 25

Drops containing the liquid chocolate solution inside and the prepared coffee solution outside were generated through two concentric tubes and introduced into the 0.3% sodium alginate solution in a room temperature bath. In said bath, the outer layer of the coffee solution reacts with the alginate forming a film of calcium alginate 30 on the outside. In turn, the calcium included inside the coffee reacts with the sodium alginate included in the chocolate forming a film outside the chocolate. This chocolate solidifies completely, obtaining at least one capsule containing two phases: a solid chocolate phase and a liquid coffee phase, which has a diameter of 10 mm. 35

Example 5. Preparation of two-phase capsules of vinegar-olive oil macerated with rosemary

Commercial vinegar was taken and xanthan gum 1% by weight, calcium lactate 0.4% by weight was added. In addition, it was taken for the second phase, olive oil macerated with rosemary was taken. 40

Drops containing rosemary macerated olive oil inside and the prepared vinegar solution outside were generated through two concentric tubes and placed in a 0.3% sodium alginate solution in a room temperature bath. Said drops were collected and placed in a bath with water for washing them. 45 were drained and packed. At least one 28 mm diameter capsule was obtained, which contained two phases of olive oil macerated with rosemary and vinegar.

While the invention has been described with respect to examples of preferred embodiments, these should not be considered as limiting the invention, which will be defined by the broader interpretation of the following claims.
权利要求:
Claims (15)
[1]

1. Spherical capsule formed in its outer part by a calcium alginate film characterized in that it comprises in its interior two substances that form two immiscible or partially miscible phases. 5

[2]
2. Spherical capsule according to claim 1, characterized in that the diameter of said capsule is up to 50 mm.

[3]
3. Spherical capsule according to claim 1, characterized in that the diameter of said capsule is in the range of 5 mm to 50 mm.

[4]
4. Spherical capsule according to claim 1, characterized in that the diameter of said capsule is in the range of 10 mm to 50 mm.
 fifteen
[5]
5. Spherical capsule according to claim 1, characterized in that the diameter of said capsule is in the range of 15 mm to 50 mm.

[6]
6. Spherical capsule according to claim 1, characterized in that the diameter of said capsule is in the range of 20 mm to 50 mm. twenty

[7]
7. Spherical capsule according to claim 1, characterized in that the diameter of said capsule is in the range of 25 mm to 50 mm.

[8]
8. Spherical capsule according to claim 1, characterized in that the diameter of said capsule is in the range of 30 mm to 50 mm.

[9]
9. Spherical capsule according to any of the preceding claims, characterized in that the substances that form two immiscible or partially miscible phases are vinegar-oil, soy sauce-sesame oil, mustard-olive oil and honey-olive oil , 30 coffee-chocolate.

[10]
10. Process for making spherical capsules according to claims 1-9, characterized in that it comprises the following steps:
 35
f) preparation of the aqueous non-calcium alginate solution in which the alginate concentration is in the range of 0.05% to 5% by weight of the solution;
g) preparation of the substances that will form the two phases to be encapsulated in which one of the substances comprises a source of calcium or magnesium ions;
h) application of the substances that will form the two phases to be encapsulated through concentric tubes 40, it being necessary that the substance comprising the source of calcium or magnesium ions be applied through the outer tube;
i) introduction of the drop or drops formed in step (c) into the aqueous solution containing alginate, in which the outer layer of the drop reacts forming at least one sphere containing both phases; Four. Five
j) wash, drain and pack the capsules formed in step (d).

[11]
Method according to claim 10, characterized in that the aqueous solution containing calcium ions is selected from solutions of calcium chloride, calcium lactate, calcium gluconate, or a mixture thereof. fifty

[12]
12. Method according to claim 11, characterized in that the source of calcium ions is calcium chloride.

[13]
13. Method according to claims 10-12, characterized in that the alginate used is sodium alginate.

[14]
14. Method according to claims 10-13, characterized in that the concentration of the non-calcium alginate salt is in the range of 0.05% to 5% by weight in relation to the alginate solution.

[15]
15. Method according to claims 10-14, characterized in that the pH of the alginate solution is between 2 and 14.
 10
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引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题
GB762700A|1954-05-17|1956-12-05|Alginate Ind Ltd|Improvements in or relating to encapsulation|
EP0116311A1|1983-01-17|1984-08-22|Morishita Jintan Co., Ltd.|Double soft capsules and production thereof|CN110200075A|2019-07-18|2019-09-06|江南大学|One grows tea double-deck quick-fried pearl of newborn flavor and preparation method thereof|JPH0116143B2|1984-07-11|1989-03-23|Q P Corp|
NO20021592D0|2002-04-04|2002-04-04|Fmc Biopolymer As|Polysaccharide Capsules and Method of Preparation thereof|
PL218009B1|2010-05-14|2014-09-30|Inst Chemii Fizycznej Polskiej Akademii Nauk|Capsules with hydrophilic core and polymer coating and process for the preparation thereof|DE202018000041U1|2018-01-05|2018-02-23|Ulrich Brunner|Spherical product|
US20190328019A1|2018-04-26|2019-10-31|Stephanie Ann Green|Olive Oil Pods or O2 Pods|
WO2019219766A1|2018-05-18|2019-11-21|Unilever N.V.|Emulsified food composition|
EP3849342A1|2018-09-12|2021-07-21|CDJ Partners, LLC|Edible alcohol-containing spheres|
US20220055007A1|2019-02-21|2022-02-24|Sushanta MITRA|Liquid encapsulation method and compositions and uses related thereto|
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ES201530738A|ES2541504B1|2015-05-27|2015-05-27|Capsules containing two phases and procedure for obtaining them|ES201530738A| ES2541504B1|2015-05-27|2015-05-27|Capsules containing two phases and procedure for obtaining them|
EP16713497.2A| EP3305084A1|2015-05-27|2016-03-14|Capsules containing two phases and method for their preparation|
US15/577,296| US20180146704A1|2015-05-27|2016-03-14|Capsules containing two phases and method for their preparation|
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JP2018513915A| JP6689963B2|2015-05-27|2016-03-14|Capsules containing two phases and methods for obtaining said capsules|
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