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Stable Fructooligosaccharides Compositions

Abstract: The present disclosure relates to a fructooligosaccharides composition that comprises 90-99.99% w/w fructooligosaccharides and 0.01 to 5.00 % w/w of an additive selected from the group consisting of locust bean gum, corn syrup, corn starch, polyvinylpyrrolidone, hydroxypropyl methylcellulose, pectin, carboxy methyl cellulose, guar gum, sodium alginate, and a combination thereof. The present disclosure also relates to a fructooligosaccharides composition that comprises 90-99.99% w/w fructooligosaccharides; 100-5000 ppm of a buffer; and 0.05-5.0% of a stabilizer selected from the group consisting of a saccharide, a polyol and a combination thereof.

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Notices, Deadlines & Correspondence

Patent Information

Application #
Filing Date
15 November 2021
Publication Number
20/2023
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
email@obhans.com
Parent Application

Applicants

TATA CHEMICALS LIMITED
BOMBAY HOUSE, 24 HOMI MODI STREET, MUMBAI – 400001, INDIA

Inventors

1. ROY, SAIKAT
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA
2. DUBEY, ASHOK
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA
3. SHAJAHAN, S
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA
4. SARAVANAN, R
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA
5. AKHTAR, ASIF
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA
6. NARAYANAN, S
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA
7. ROKADE, SUNIL
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA
8. KALLEPELLI, MAHESH
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA
9. TRIPATHI, ANU
TATA CHEMICALS LTD., INNOVATION CENTRE, SURVEY NO. 315, HISSA NO. 1-14, AMBEDVETH (V), PAUD ROAD, MULSHI, PUNE-412111, MAHARASHTRA, INDIA

Specification

DESC:FIELD OF INVENTION
The present disclosure relates to fructooligosaccharides (FOS) compositions and processes for preparing such compositions. More specifically, it relates to stable FOS compositions and processes for preparing such compositions.

BACKGROUND
FOS are non-digestible oligosaccharides that occur naturally in a wide variety of foods such as banana, tomato, wheat, and onion. FOS are commercially available as a food ingredient or a nutritional supplement and have Generally Recognized as Safe (GRAS) status.

According to a growing body of research, FOS may provide several health benefits, for example, improvements in plasma lipids and lipoproteins, reduction in serum insulin and glucose concentrations, and inhibition of harmful bacteria in gut. Further, FOS have sweetening profile, and water retention properties similar to those of sucrose and sorbitol. They are also known to improve moisture retention, texture, and shelf life of food products. Due to these properties, FOS are widely used as alternative sweetener, and prebiotic or functional food.

FOS in the powder form exhibits high deliquescent properties when exposed to the air. The powder becomes sticky when applied to food, feed, and other industrial processes especially during the hot and humid summer season. It also tends to solidify even after mixing.

The problems associated with the powder form of FOS can be avoided by using a liquid composition of FOS. Although, the liquid composition is easy to use and has certain advantages, its application is restricted due to the crystal precipitation in the composition during long term storage.

SUMMARY

The present disclosure relates to a fructooligosaccharides composition, which comprises 90-99.99% w/w fructooligosaccharides; and 0.01 to 5.00 % w/w of an additive selected from the group consisting of locust bean gum, corn syrup, corn starch, polyvinylpyrrolidone, hydroxypropyl methylcellulose, pectin, carboxy methyl cellulose, guar gum, sodium alginate, and a combination thereof.

The present disclosure also relates to a fructooligosaccharides composition, which comprises 90-99.99% w/w fructooligosaccharides; 100-5000 ppm of a buffer; and 0.05-5.0% of a stabilizer selected from the group consisting of a saccharide, a polyol and a combination thereof.

DETAILED DESCRIPTION
For the purpose of promoting an understanding of the principles of the disclosure, reference will now be made to embodiments and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the disclosure is thereby intended, such alterations and further modifications in the disclosed composition and method, and such further applications of the principles of the disclosure therein being contemplated as would normally occur to one skilled in the art to which the disclosure relates.

It will be understood by those skilled in the art that the foregoing general description and the following detailed description are exemplary and explanatory of the disclosure and are not intended to be restrictive thereof.

Reference throughout this specification to “one embodiment”, “an embodiment” or similar language means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the present disclosure. Thus, appearances of the phrase “in one embodiment”, “in an embodiment” and similar language throughout this specification may, but do not necessarily, all refer to the same embodiment

The terms “a,” “an,”, and “the” are used to refer to “one or more” (i.e. to at least one) of the grammatical object of the article.

The terms "comprises", "comprising", or any other variations thereof, are intended to cover a non-exclusive inclusion and are not intended to be construed as “consists of only”, such that a process or method that comprises a list of steps does not include only those steps but may include other steps not expressly listed or inherent to such process or method.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the disclosure, the preferred methods, and materials are now described.

Fructooligosaccharides (FOS) compositions and methods of preparing said composition are disclosed. The FOS are oligosaccharides comprising 2–10 fructose units with the terminal fructose linked to a glucose residue by ß-(1?2) glycosidic bonds. The disclosed compositions are in a liquid form. The disclosed FOS compositions exhibit are stable and exhibit improved shelf life.

In an aspect, the present disclosure relates to an FOS composition, which comprises 90-99.99% w/w FOS and 0.01 to 5.00% w/w of an additive selected from the group consisting of locust bean gum, corn syrup, corn starch, polyvinylpyrrolidone, hydroxypropyl methylcellulose, pectin, carboxy methyl cellulose, guar gum, sodium alginate, and a combination thereof.

In an embodiment, the additive includes one additive. In another embodiment, the additive is a combination of two or more additives.

In an embodiment, the composition comprises locust bean gum in the range of 0.005-2% w/w.

In an embodiment, the composition comprises corn syrup or corn starch in the range of 0.1-5% w/w.

In an embodiment, the composition comprises polyvinylpyrrolidone in the range of 0.1-5% w/w.

In an embodiment, the composition comprises hydroxypropyl methylcellulose in the range of 0.05-2% w/w.

In an embodiment, the composition comprises pectin in the range of 0.002-2% w/w.

In an embodiment, the composition comprises carboxy methyl cellulose in the range of 0.002-2% w/w.

In an embodiment, the composition comprises guar gum in the range of 0.002-2% w/w.

In an embodiment, the composition comprises sodium alginate in the range of 0.005-2% w/w.

In an embodiment, the additive is a combination of corn syrup and corn starch. In an embodiment, the composition comprises 0.1-5% w/w of the combination of corn syrup and corn starch.

In an embodiment, the additive is a combination of polyvinylpyrrolidone and hydroxypropyl methylcellulose. In an embodiment, the composition comprises 0.1-0.5% w/w each of polyvinylpyrrolidone and hydroxypropyl methylcellulose.

In an embodiment, the additive is a combination of locust bean gum, pectin, carboxy methyl cellulose, and guar gum. In an embodiment, the composition comprises 0.005-0.125% w/w locust bean gum, 0.005-0.125% w/w pectin, 0.005-0.125% w/w carboxy methyl cellulose, and 0.005-0.125% w/w guar gum.

In accordance with an embodiment, the composition further comprises a buffer selected from the group consisting of disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium citrate citric acid, magnesium chloride, calcium ascorbate, potassium ascorbate, potassium malate, calcium gluconate, and a combination thereof.

In accordance with an embodiment, the buffer is in the range of 100-5000 ppm. In accordance with an embodiment, the buffer is in the range of 100-3000 ppm. In accordance with a specific embodiment, the buffer comprises disodium hydrogen phosphate, and sodium dihydrogen phosphate in a ratio in the range of 1:0.5-1:2.

In accordance with an embodiment, the composition further comprises an additional ingredient. In accordance with an embodiment, the additional ingredient is selected from the group consisting of an emulsifier, a stabilizer, an antioxidant, and a combination thereof. Specific examples of the additional ingredient include but are not limited to stearic acid ester such as glycerol monostearate, propylene glycol monostearate, and a combination thereof.

In accordance with an embodiment, the composition has a sugar content in a range of 60-85 brix. In an embodiment, the sugar content is in the range of 65-80 brix.

The present disclosure also relates to a process for preparing the above disclosed composition. The process comprises adding and mixing the additive in a FOS liquid. In accordance with an embodiment, the FOS liquid has a sugar content in a range of 73-77 brix. The mixing is done at a temperature in the range of 20 to 80°C. In an embodiment, the additive is dissolved in water before the mixing. In another embodiment, the additive is dissolved in water and the solution so obtained is heated before the mixing.

In another aspect, the present disclosure relates to an FOS composition, which comprises 90-99.99% w/w fructooligosaccharides; 100-5000 ppm of a buffer; and 0.05-5.0% of a stabilizer selected from the group consisting of a saccharide, a polyol and a combination thereof.

In an embodiment, the stabilizer includes one stabilizer. In another embodiment, the stabilizer includes a combination of two or more stabilizers.

In accordance with an embodiment, the saccharide is a monosaccharide, a disaccharide or a trisaccharide. In accordance with an embodiment, the saccharide is selected from the group consisting of maltose, raffinose, fructose, and a combination thereof. In accordance with an embodiment, the composition comprises the saccharide in the range of 0.05-2.0% w/w.

In accordance with an embodiment, the polyol is selected from the group consisting of glycerol, sorbitol, arabitol, erythritol, maltitol, isomalt, and a combination thereof. In accordance with a specific embodiment, the polyol is glycerol and/or sorbitol. In accordance with an embodiment, the composition comprises the polyol in the range of 0.5-3.0% w/w.

In accordance with an embodiment, the buffer is in the range of 100-3000 ppm. In accordance with an embodiment, the buffer is selected from the group consisting of disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium citrate, citric acid, magnesium chloride, calcium ascorbate, potassium ascorbate, potassium malate, calcium gluconate and a combination thereof. In a specific embodiment, the buffer comprises disodium hydrogen phosphate and sodium dihydrogen phosphate in a ratio in the range of 1:05-1:2.

In accordance with an embodiment, the composition comprises one or more suitable additional ingredients. In accordance with an embodiment, the additional ingredient is selected from the group consisting of an emulsifier, a stabilizer, an antioxidant, and a combination thereof. Examples of additional ingredient without limitation include stearic acid ester(s) such as glycerol monostearate and/or propylene glycol monostearate.
In accordance with an embodiment, the composition has a sugar content in the range of 60-85 brix. In accordance with an embodiment, the sugar content is in the range of 65-80 brix.

The present disclosure also relates to a process for preparing the above disclosed composition. The process comprises adding and mixing the stabilizer and the buffer in a FOS liquid. In accordance with an embodiment, the FOS liquid has a sugar content in a range of 73-77 brix. The mixing is done at a temperature in the range of 20 to 80°C. In an embodiment, the stabilizer is dissolved in water before the mixing. In another embodiment, the stabilizer is dissolved in water and the solution so obtained is heated before the mixing.

The compositions and processes according to the present disclosure are further illustrated by the following examples. The examples illustrate various embodiments of the inventive compositions, the method of making them, and the advantages achieved. The present disclosure is not intended to be limited by the examples, and it is to be appreciated that one skilled in the art would understand that a variety of compositions can be prepared, by following the teachings herein, which would achieve the same or similar results.

EXAMPLES

Example 1: Preparation of FOS Composition A
0.3 gm of locust bean gum was added to 2-3 ml of water and heated to make a solution or a gel. The solution was added to 99.7 gm of 73-77 brix FOS liquid to make a ~75-76 brix mixture. The mixture was stirred for some time to obtain FOS composition A.
Example 2: Preparation of FOS Composition B
0.1 gm each of locust bean gum, pectin, carboxy methyl cellulose and guar gum were added to 2 ml of water and heated to make a solution or gel. This solution was added to 99.9 gm of 76 brix FOS liquid to make a ~75 brix mixture. The mixture was heated at 65-70°C and stirred for some time to obtain FOS composition B.
Example 3: Preparation of FOS Composition C
0.5 gm each of polyvinylpyrrolidone was added to 2 ml of water and heated to make a solution. This solution was added to 99.5 gm of 76 brix FOS liquid to make a ~75 brix mixture. The mixture was heated at 65-70 °C and stirred for some time to obtain FOS composition C.

Example 4: Preparation of FOS Composition D

0.25 gm of hydroxypropyl methyl cellulose was added to 2 ml of water and heated to make a solution. This solution was added to 99.75 gm of 76 brix FOS liquid to make a ~75 brix mixture. The mixture was heated at 65-70°C and stirred for some time to obtain FOS composition D.
Example 5: Preparation of FOS Composition E
0.25 gm of sodium alginate was added to 2 ml of water and heated to make a solution. This solution was added to 99.75 gm of 76 brix FOS liquid to make a ~75 brix mixture. The mixture was heated at 65-70°C and stirred for some time to obtain FOS composition E.
Example 6: Preparation of FOS Composition F
0.0125 gm each of locust bean gum, pectin, carboxy methyl cellulose and guar gum were added to 2ml water and heated to make a solution or gel. This solution was added to 99.9 gm of 63 brix FOS liquid. The mixture was heated at 65-70 °C for some time under vacuum to obtain a ~72 brix mixture to form FOS composition F.
Example 7: Comparison of FOS compositions A-F with a Control
75 brix FOS liquid was used as a control. The FOS compositions A-F and the control were kept in the same type of smooth surface plastic containers at 25 +/- 2 °C and 7±2 °C for visual and microscopic observation of nucleation and crystallization. The results are provided in Table 1.
Table 1: Comparison of FOS Compositions A-F with the Control
Control/
FOS Composition After 1 month After 3 months After 6 months After 9 months
Control Crystallization Crystallization Crystallization Crystallization

A No Crystallization No Crystallization Crystallization Crystallization
B No Crystallization No Crystallization No Crystallization No Crystallization
C No Crystallization No Crystallization Crystallization Crystallization
D No Crystallization No Crystallization Crystallization Crystallization
E No Crystallization No Crystallization Crystallization Crystallization
F No Crystallization No Crystallization No Crystallization No Crystallization

Example 8: Preparation of FOS Compositions G-I

To prepare compositions G-I, corn syrup or locust bean gum and 1:1 composition of disodium hydrogen phosphate and sodium dihydrogen phosphate were added in the amounts specified below to 95.0 to 99.7 gm of 75 brix FOS liquid to prepare ~75-76 brix mixtures.

For preparing the composition containing locust bean gum, locust bean gum was first added to water, and heated to make a gel or a solution. The gel or the solution so obtained was then added to the FOS liquid. The details of the compositions are provided in Table 2 below.
Table 2: Details of Compositions G-I

FOS composition Corn syrup Locust bean gum Disodium hydrogen phosphate and
sodium dihydrogen phosphate (1:1)
G 2% - 1400 ppm
H 5% - 1400 ppm
I - 0.3% 1400 ppm

Example 9: Comparison of FOS compositions G-I with a Control
75 brix FOS liquid was used as a control. FOS compositions G-I and the control were kept in the same type of plastic containers at 25 +/- 2 °C for visual and microscopic observation of nucleation and crystallization. The results are provided in Table 3.
Table 3: Comparison of FOS Compositions G-I with the Control
Control/FOS Composition After 1 month After 3 months After 6 months
Control Crystallization Crystallization Crystallization
G No Crystallization Crystallization Crystallization
H No Crystallization Crystallization Crystallization
I No Crystallization No Crystallization No Crystallization

Example 10: Preparation of FOS Compositions 1-5
To prepare compositions 1-5, disodium hydrogen phosphate, and sodium dihydrogen phosphate along with glycerol, or sorbitol were added to 75 brix FOS liquid to prepare ~75-76 brix mixtures. The mixtures were stirred to obtain compositions 1-5. The details of the compositions are provided in Table 1 below.
Table 4: Details of the FOS Compositions 1-5

FOS Composition Glycerol Sorbitol Di sodium hydrogen phosphate and
Sodium dihydrogen phosphate (1:1)
1 1% 0 1400 ppm
2 2% 0 1400 ppm
3 3% 0 1400 ppm
4 0 0.5% 1400 ppm
5 0 0 1400 ppm

Example 11: Comparison of FOS compositions 1-5 with Control
75 brix FOS liquid was used as a Control. FOS compositions 1-5 and the Control were kept in the same type of plastic containers at 25 +/- 2 °C for visual and microscopic observation of nucleation and crystallization. The results are provided in Table 2.

Table 5: Results of the Comparison

Control/FOS Composition Crystallization Observed

After 1 week After 2 weeks After 1 month After 3 months
Control Yes Yes Yes Yes
1 No No No Yes
2 No No No No
3 No No No No
4 No No No No
5 No No No No

INDUSTRIAL APPLICABILITY
The present disclosure provides stabilized liquid FOS compositions that exhibit a good shelf life. The disclosed compositions do not suffer from crystallization even after being stored for a long period of time. Thus, the disclosed compositions do not develop a cloudy or turbid appearance and remain clear over a long period of time. The process for obtaining the disclosed composition is simple, economical, and efficient.
,CLAIMS:We Claim:

1. A fructooligosaccharides composition comprising:
90-99.99% w/w fructooligosaccharides; and
0.01 to 5.00 % w/w of an additive selected from the group consisting of locust bean gum, corn syrup, corn starch, polyvinylpyrrolidone, hydroxypropyl methylcellulose, pectin, carboxy methyl cellulose, guar gum, sodium alginate, and a combination thereof.

2. The composition as claimed in claim 1, comprising 0.005-2% w/w locust bean gum.

3. The composition as claimed in claim 1, comprising 0.1-5% w/w corn syrup and/or corn starch.

4. The composition as claimed in claim 1, comprising 0.1-5% w/w polyvinylpyrrolidone.

5. The composition as claimed in claim 1, comprising 0.05-2% w/w hydroxypropyl methylcellulose.

6. The composition as claimed in claim 1, comprising 0.1-0.5% w/w each of polyvinylpyrrolidone and hydroxypropyl methylcellulose.

7. The composition as claimed in claim 1, comprising 0.002-2% w/w pectin.

8. The composition as claimed in claim 1, comprising 0.002-2% w/w carboxy methyl cellulose.

9. The composition as claimed in claim 1, comprising 0.002-2% w/w guar gum.

10. The composition as claimed in claim 1, comprising 0.005-2% w/w sodium alginate.

11. The composition as claimed in claim 1, comprising 0.005-0.125% w/w locust bean gum, 0.005-0.125% w/w pectin, 0.005-0.125% w/w carboxy methyl cellulose, and 0.005-0.125% w/w guar gum.

12. The composition as claimed in any of the preceding claims, further comprising a buffer selected from the group consisting of disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium citrate citric acid, magnesium chloride, calcium ascorbate, potassium ascorbate, potassium malate, calcium gluconate, and a combination thereof.

13. The composition as claimed in claim 12, wherein the buffer is in the range of 100-5000 ppm.

14. The composition as claimed in any of claims 12 or 13, wherein the buffer comprises disodium hydrogen phosphate and sodium dihydrogen phosphate in a ratio in the range of 1:0.5-1:2.

15. The composition as claimed in any of the preceding claims further comprising an additional ingredient selected from the group consisting of an emulsifier, a stabilizer, an antioxidant, and a combination thereof.

16. The composition as claimed in any of the preceding claims, wherein the composition has a sugar content in the range of 60-85 brix.

17. A fructooligosaccharides composition comprising:
a) 90-99.99% w/w fructooligosaccharides;
b) 100-5000 ppm of a buffer; and
c) 0.05-5.0% of a stabilizer selected from the group consisting of a saccharide, a polyol, and a combination thereof.

18. The composition as claimed in claim 17, comprising the saccharide in the range of 0.05-2.0% w/w.

19. The composition as claimed in any of claims 17 or 18, wherein the saccharide is selected from the group consisting of maltose, raffinose, fructose, and a combination thereof.

20. The composition as claimed in claim 17, comprising the polyol in the range of 0.5-3.0% w/w.

21. The composition as claimed in any of claims 17 or 20, wherein the polyol is selected from the group consisting of glycerol, sorbitol, arabitol, erythritol, maltitol, isomalt, and a combination thereof.

22. The composition as claimed in any of claims 17, 20 or 21, wherein the polyol is glycerol and/or sorbitol.

23. The composition as claimed in any of claims 17-22, wherein the buffer is in the range of 100-3000 ppm.

24. The composition as claimed in any of claims 17-23, wherein the buffer is selected from the group consisting of disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium citrate, citric acid, magnesium chloride, calcium ascorbate, potassium ascorbate, potassium malate, calcium gluconate and a combination thereof.

25. The composition as claimed in any of claims 17-24, wherein the buffer comprises disodium hydrogen phosphate and sodium dihydrogen phosphate in a ratio in the range of 1:05-1:2.

26. The composition as claimed in any of claims 17-25, further comprising an additional ingredient selected from the group consisting of an emulsifier, a stabilizer, an antioxidant, and a combination thereof.

27. The composition as claimed in any of claims 17-26, wherein the composition has a sugar content in the range of 60-85 brix.

Documents

Application Documents

# Name Date
1 202121052351-PROVISIONAL SPECIFICATION [15-11-2021(online)].pdf 2021-11-15
2 202121052351-FORM 1 [15-11-2021(online)].pdf 2021-11-15
3 202121052351-FORM-26 [09-02-2022(online)].pdf 2022-02-09
4 202121052351-Proof of Right [20-04-2022(online)].pdf 2022-04-20
5 202121052351-FORM 3 [15-11-2022(online)].pdf 2022-11-15
6 202121052351-ENDORSEMENT BY INVENTORS [15-11-2022(online)].pdf 2022-11-15
7 202121052351-COMPLETE SPECIFICATION [15-11-2022(online)].pdf 2022-11-15
8 202121052351-FORM 3 [19-01-2023(online)].pdf 2023-01-19
9 202121052351-FORM 18 [04-09-2024(online)].pdf 2024-09-04