SURFACE-REACTED CALCIUM CARBONATE IN FOOD
20220104525 · 2022-04-07
Inventors
- Tanja Budde (Brittnau, CH)
- Anaïs Hecker (Lyss, CH)
- Lalit SHARMA (Zofingen, CH)
- Laura De Miguel (Oftringen, CH)
Cpc classification
A23V2002/00
HUMAN NECESSITIES
C01P2004/61
CHEMISTRY; METALLURGY
A23L5/42
HUMAN NECESSITIES
A23V2002/00
HUMAN NECESSITIES
A23P20/15
HUMAN NECESSITIES
A23P20/25
HUMAN NECESSITIES
A23P20/10
HUMAN NECESSITIES
A23L33/115
HUMAN NECESSITIES
A23K20/24
HUMAN NECESSITIES
A61K9/0056
HUMAN NECESSITIES
C01P2004/51
CHEMISTRY; METALLURGY
International classification
A23L29/00
HUMAN NECESSITIES
A23L33/115
HUMAN NECESSITIES
A23L5/42
HUMAN NECESSITIES
A23P20/15
HUMAN NECESSITIES
A23P20/25
HUMAN NECESSITIES
A61K9/00
HUMAN NECESSITIES
Abstract
The present invention refers to an edible composition comprising water and/or at least one edible oil and a surface-reacted calcium carbonate having a volume median particle size d.sub.50 from 0.1 to 90 μm, an edible coating and/or filling comprising the surface-reacted calcium carbonate, a food product or pharmaceutical product or neutraceutical product at least partially coated and/or filled with the edible composition, a method for producing a food product or pharmaceutical product or neutraceutical product at least partially coated and/or filled with the edible composition and the uses of the surface-reacted calcium carbonate as whitening agent or opacifier and/or sweetness reduction agent and/or calorie reduction agent in an edible coating and/or filling of a food product or pharmaceutical product or neutraceutical product, as a replacement agent for titanium dioxide in an edible coating and/or filling of a food product or pharmaceutical product or neutraceutical product as well as for reducing the dry time of an edible composition being at least partially applied on the surface of and/or filled into a food product or pharmaceutical product or neutraceutical product.
Claims
1. Method for producing a food product or pharmaceutical product or nutraceutical product at least partially coated a) mixing water and/or at least one edible oil with a surface-reacted calcium carbonate having a volume median particle size d.sub.50 from 0.1 to 90 μm, wherein the surface-reacted calcium carbonate is a reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more H.sub.3O.sup.+ ion donors, wherein the carbon dioxide is formed in situ by the H.sub.3O.sup.+ ion donors treatment and/or is supplied from an external source, for obtaining an edible composition, and b) applying the edible composition obtained in step a), one or more times, at least partially on the surface of a food product or pharmaceutical product or nutraceutical product, or filling the edible composition obtained in step a) into a food product or pharmaceutical product or nutraceutical product.
2. The method according to claim 1, wherein applying the edible composition obtained in step a) at least partially on the surface of a food product or pharmaceutical product or nutraceutical product in step b) is carried out by brushing or pouring, pan coating, curtain or dip coating, fluidized bed coating, hot melt coating and/or compression coating or the filling of the edible composition obtained in step a) into a food product or pharmaceutical product or nutraceutical product in step b) is carried out by injecting the edible composition into the food product or pharmaceutical product or nutraceutical product.
3. The method of claim 1, wherein the surface-reacted calcium carbonate has a volume median particle size d.sub.50 from 0.1 to 75 μm.
4. The method of claim 1, wherein the surface-reacted calcium carbonate has a volume median particle size d.sub.50 from 0.5 to 50 μm.
5. The method of claim 1, wherein the surface-reacted calcium carbonate has a volume median particle size d.sub.50 from 1 to 40 μm.
6. The method of claim 1, wherein the surface-reacted calcium carbonate has a volume median particle size d.sub.50 from 1.2 to 30 μm.
7. The method of claim 1, wherein the surface-reacted calcium carbonate has a volume median particle size d.sub.50 from 1.5 to 15 μm.
8. The method of claim 1, wherein the surface-reacted calcium carbonate has a specific surface area of from 15 m.sup.2/g to 200 m.sup.2/g, measured using nitrogen and the BET method.
9. The method of claim 1, wherein the surface-reacted calcium carbonate has a specific surface area of from 20 m.sup.2/g to 180 m.sup.2/g, measured using nitrogen and the BET method.
10. The method of claim 1, wherein the surface-reacted calcium carbonate has a specific surface area of from 25 m.sup.2/g to 160 m.sup.2/g, measured using nitrogen and the BET method.
11. The method of claim 1, wherein the surface-reacted calcium carbonate has a specific surface area of from 27 m.sup.2/g to 150 m.sup.2/g, measured using nitrogen and the BET method.
12. The method of claim 1, wherein the surface-reacted calcium carbonate has a specific surface area of from 30 m.sup.2/g to 140 m.sup.2/g, measured using nitrogen and the BET method.
13. The method of claim 1, wherein the surface-reacted calcium carbonate is a whitening agent or opacifier and/or sweetness reduction agent and/or calorie reduction agent.
14. The method of claim 1, wherein the surface-reacted calcium carbonate is a replacement agent for titanium dioxide in the food product or pharmaceutical product.
Description
SHORT DESCRIPTION OF THE FIGURES
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[0233]
[0234]
[0235]
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[0240]
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[0242]
[0243]
[0244]
EXAMPLES
1. MEASUREMENT METHODS
[0245] In the following, measurement methods implemented in the examples are described.
[0246] Particle Size Distribution
[0247] Volume determined median particle size d.sub.50(vol) and the volume determined top cut particle size d.sub.98(vol) was evaluated using a Malvern Mastersizer 2000 Laser Diffraction System Malvern Instruments Plc., Great Britain). The d.sub.50(vol) or d.sub.98(vol) value indicates a diameter value such that 50% or 98% by volume, respectively, of the particles have a diameter of less than this value. The raw data obtained by the measurement was analyzed using the Mie theory, with a particle refractive index of 1.57 and an absorption index of 0.005. The methods and instruments are known to the skilled person and are commonly used to determine particle size distributions of fillers and pigments.
[0248] The weight determined median particle size d.sub.50(wt) was measured by the sedimentation method, which is an analysis of sedimentation behaviour in a gravimetric field. The measurement was made with a Sedigraph™ 5120 of Micromeritics Instrument Corporation, USA. The method and the instrument are known to the skilled person and are commonly used to determine particle size distributions of fillers and pigments. The measurement was carried out in an aqueous solution of 0.1 wt.-% Na.sub.4P.sub.2O.sub.7. The samples were dispersed using a high speed stirrer and supersonicated.
[0249] Specific Surface Area (SSA)
[0250] The specific surface area was measured via the BET method according to ISO 9277 using nitrogen, following conditioning of the sample by heating at 250° C. for a period of 30 minutes. Prior to such measurements, the sample was filtered within a Büchner funnel, rinsed with deionised water and dried overnight at 90 to 100° C. in an oven. Subsequently, the dry cake was ground thoroughly in a mortar and the resulting powder was placed in a moisture balance at 130° C. until a constant weight was reached.
[0251] Intra-Particle Intruded Specific Pore Volume (in cm.sup.3/g)
[0252] The specific pore volume was measured using a mercury intrusion porosimetry measurement using a Micromeritics Autopore V 9620 mercury porosimeter having a maximum applied pressure of mercury 414 MPa (60 000 psi), equivalent to a Laplace throat diameter of 0.004 μm m(˜nm). The equilibration time used at each pressure step was 20 seconds. The sample material was sealed in a 5 cm.sup.3 chamber powder penetrometer for analysis. The data were corrected for mercury compression, penetrometer expansion and sample material compression using the software Pore-Comp (Gane, P. A. C., Kettle, J. P., Matthews, G. P. and Ridgway, C. J., “Void Space Structure of Compressible Polymer Spheres and Consolidated Calcium Carbonate Paper-Coating Formulations”, Industrial and Engineering Chemistry Research, 35(5), 1996, p 1753-1764.).
[0253] The total pore volume seen in the cumulative intrusion data can be separated into two regions with the intrusion data from 214 μm down to about 1-4 μm showing the coarse packing of the sample between any agglomerate structures contributing strongly. Below these diameters lies the fine inter-particle packing of the particles themselves. If they also have intra-particle pores, then this region appears bi-modal, and by taking the specific pore volume intruded by mercury into pores finer than the modal turning point, i.e. finer than the bi-modal point of inflection, the specific intra-particle pore volume is defined. The sum of these three regions gives the total overall pore volume of the powder, but depends strongly on the original sample compaction/settling of the powder at the coarse pore end of the distribution.
[0254] By taking the first derivative of the cumulative intrusion curve the pore size distributions based on equivalent Laplace diameter, inevitably including pore-shielding, are revealed. The differential curves clearly show the coarse agglomerate pore structure region, the inter-particle pore region and the intra-particle pore region, if present. Knowing the intra-particle pore diameter range it is possible to subtract the remainder inter-particle and inter-agglomerate pore volume from the total pore volume to deliver the desired pore volume of the internal pores alone in terms of the pore volume per unit mass (specific pore volume). The same principle of subtraction, of course, applies for isolating any of the other pore size regions of interest.
[0255] Preparation of a Coated Surface
[0256] Coated surfaces were prepared by using the respective coating formulations and applying them with a box scarper having a coater gap of 300 μm on contrast cards. The contrast cards used are Leneta contrast cards, form 3-B-H, size 7⅝×11⅜ (194×289 mm), sold by the company Leneta, and distributed by Novamart, Stäfa, Switzerland.
[0257] Determination of Colour Values (Rx, Ry, Rz)
[0258] The colour values Rx, Ry, Rz were determined over the white and black fields of the Leneta contrast card, and are measured with a spectraflas SF 450 X spectrophotomer of the company Datacol or, Montreuil, France.
[0259] Contrast Ratio (Opacity) of a Coated Surface/Film
[0260] Contrast ratio (covering power) values were determined according to ISO 2814 at a spreading rate of 7.5 m.sup.2/l with the ELREPHO SF 450X.
[0261] The contrast ratio was calculated as described by the equation below:
[0262] with Ry.sub.black and Ry.sub.white being obtained by the measurement of the color values.
[0263] Yellowness Value
[0264] The yellowness value was determined according to ISO 2814 at a spreading rate of 7.5 m.sup.2/l with the ELREPHO SF 450X.
[0265] Dry Film Thickness
[0266] The film was allowed to dry and then the thickness of the film was measured with a L&W micrometer, Lorentzen & Wettre.
2. MATERIALS
[0267] Pigment Materials
[0268] Titanium Dioxide
[0269] Tioxide® Purity 73 was obtained from Huntsman.
[0270] Calcium Carbonate [0271] GCC 1: a high purity natural calcium carbonate having a d.sub.50 (wt.-%) of 2 μm that is commercially available from Omya [0272] GCC 2: a high purity natural calcium carbonate having a d.sub.50 (wt.-%) of 3 μm that is commercially available from Omya [0273] GCC 3: a high purity natural calcium carbonate having a d.sub.50 (wt.-%) of 5.5 μm that is commercially available from Omya
[0274] Surface-Reacted Calcium Carbonate
[0275] SRCC 1
[0276] SRCC1 has a d.sub.50=6.6 μm, a d.sub.98=13.7 μm, a SSA=59.9 m.sup.2g.sup.−1 and an intra-particle intruded specific pore volume of 0.939 cm.sup.3/g (for the pore diameter range of 0.004 to 0.51 μm).
[0277] The SRCC 1 has been prepared as follows:
[0278] SRCC 1 was obtained by preparing 350 litres of an aqueous suspension of ground calcium carbonate in a mixing vessel by adjusting the solids content of a ground limestone calcium carbonate from Omya SAS, Orgon having a mass based median particle size of 1.3 μm, as determined by sedimentation, such that a solids content of 10 wt.-%, based on the total weight of the aqueous suspension, is obtained.
[0279] Whilst mixing the slurry at a speed of 6.2 m/s, 11.2 kg phosphoric acid was added in form of an aqueous solution containing 30 wt.-% phosphoric acid to said suspension over a period of 20 minutes at a temperature of 70° C. After the addition of the acid, the slurry was stirred for additional 5 minutes, before removing it from the vessel and drying using a jet-dryer.
[0280] SRCC 2
[0281] SRCC 2 had a d.sub.50(vol)=6.2 μm, d.sub.98(vol)=9.7 μm, SSA=88.0 m.sup.2/g with an intra-particle intruded specific pore volume of 1.550 cm.sup.3/g (for the pore diameter range of 0.004 to 0.6 μm).
[0282] The SRCC 2 has been prepared as follows:
[0283] In a mixing vessel, 10 liters of an aqueous suspension of ground marble calcium carbonate was prepared by adjusting the solids of a ground marble calcium carbonate having a particle size distribution of 90 wt.-% below 2 μm, based on the total weight of the ground calcium carbonate, such that a solids content of 15 wt.-%, based on the total weight of the aqueous suspension, is obtained.
[0284] Whilst mixing the slurry, 2.8 kg phosphoric acid was added in form of an aqueous solution containing 30 wt.-% phosphoric acid to said suspension over a period of 10 minutes. Throughout the whole experiment the temperature of the suspension was maintained at 70° C. After the addition of the acid, the suspension was stirred for additional 5 minutes before removing it from the vessel and drying.
[0285] SRCC 3
[0286] SRCC 3 had d.sub.50(vol)=4.5 μm, d.sub.98(vol.)=8.6 μm, SSA=96.1 m.sup.2/g with an intra-particle intruded specific pore volume of 1.588 cm.sup.3/g (for the pore diameter range of 0.004 to 0.4 μm).
[0287] The SRCC 3 has been prepared as follows:
[0288] In a mixing vessel, 10 liters of an aqueous suspension of ground limestone calcium carbonate was prepared by adjusting the solids of a ground limestone calcium carbonate having a particle size distribution of 90 wt.-% below 2 μm, based on the total weight of the ground calcium carbonate, such that a solids content of 15 wt.-%, based on the total weight of the aqueous suspension, is obtained.
[0289] Whilst mixing the slurry, 2.8 kg phosphoric acid was added in form of an aqueous solution containing 30 wt.-% phosphoric acid to said suspension over a period of 10 minutes. Throughout the whole experiment the temperature of the suspension was maintained at 70° C. After the addition of the acid, the suspension was stirred for additional 5 minutes before removing it from the vessel and drying.
[0290] Other Materials
[0291] Tween 60V Pharma (emulsifier): is a Polysorbate 60: polyoxyethylene (20) sorbitan monostearate; an emulsifier used in pharma and food preparations. The supplier was Croda.
[0292] Icing sugar: powdered sugar; obtained from Migros, Switzerland under the name “poudre”.
[0293] Chewing gum cores: supplied by asCom Confection GmbH, Walldorf, Germany; sugar-free and containing sorbitol, maltitol syrup and mannitol. The average weight of each gum core was 1.5 grams.
[0294] Crystal sugar: supplied by Suedzucker, Germany.
[0295] Sugar alcohol maltitol: supplied by Roquette under the name “Maltisorb P200”.
[0296] PEG 6005 (plasticizers: supplied by BASF AG, Germany, is a polyethylene glycol) having a molecular weight from 570 to 630 g/mol
[0297] Pharmacoat 606 (film-forming agent): supplied by Shirt-Etsu Chemical Co., Ltd., Japan, and is a hydroxypropyl methylcellulose (HPMC) grade 606, substitution type 2910, i.e. the first two digits indicate the percentage of methoxy groups; last two digits indicate the percentage of hydroxypropyl groups, having a viscosity of 6 mPas/s.
[0298] Dimethicone grade: defoaming agent): supplied by Solvias AG, Switzerland.
[0299] Sodium lauryl sulphate (SLS: surfactant): supplied by Sigma-Aldrich, USA.
3. EXAMPLES
[0300] A. Preparation of Sugar Coating Formulations
[0301] The coating formulations were produced according to the following protocol.
[0302] 1. Preparation of Tween 60V Pharma Solution and Pigment Material Pastes Used
[0303] Before preparing the final coating formulations, a paste containing only the pigment material, water and emulsifier (polyoxyethylene (20) sorbitan monostearate; Tween 60 V Pharma) has been produced in order to disperse the pigment material particles and to avoid the formation of agglomerates.
[0304] The below Table 1 shows an overview over the emulsifier solution and pigment material pastes produced:
TABLE-US-00001 TABLE 1 Emulsifier solution and pigment material pastes Ingredient % w/w Formula 0 1 2 3 4 5 6 7 A) Aqua dem. 75.0 32.0 23.0 23.0 21.0 58.6 67.3 69.4 Emulsifier 25.0 6.0 4.5 4.5 4.5 11.0 11.5 11.8 TiO.sub.2 — 55.0 — — — — — — GCC 1 — — 71.4 — — — — — GCC 2 — — — 71.4 — — — — GCC 3 — — — — 74.1 — — — SRCC 1 — — — — — 30.4 — — SRCC 2 — — — — — — 21.2 — SRCC 3 — — — — — — — 18.8 B) Aqua dem. — 7.0 1.1 1.1 3.1 — — — 100 100 100 100 100 100 100 100 Emulsifier TiO.sub.2 GCC 1 GCC 2 GCC 3 SRCC 1 SRCC 2 SRCC 3 solution paste paste paste paste paste paste paste
[0305] Phase A [0306] In a container water and emulsifier were blended with a Dispermat™ (from Getzmann, Reichshof, Germany) using the dissolver impeller with a diameter of 40 mm. [0307] Then, the pigment material was slowly added, and the resulting mixture was mixed using the Dispermat™ (4 000 rpm; appr. 5 minutes, dissolver impeller diameter: 40 mm) until a homogenous mixture was obtained.
[0308] Phase B [0309] Then, the water (phase B) was added at, the end to phase A and mixed by hand.
[0310] The quantity of produced paste was 500 g for each case.
[0311] Remark: The emulsifier was added in order to improve the wetting and the homogeneity of the pigment material used.
[0312] 2. Preparation of Final Coating Formulations
[0313] Phase C [0314] In a container water and emulsifier or emulsifier solution prepared according to Formula 0 listed in Table 1 were blended with a Dispermat™ (from Getzmann, Reichshof, Germany) using the dissolver impeller with a diameter of 40 mm. [0315] Then, the pigment material paste (listed in Formulas 1 to 7 of Table 1) was slowly added, and the resulting mixture was mixed using the Dispermat™ (4 000 rpm; appr. 5 minutes, dissolver impeller diameter: 40 mm) until a homogenous mixture was obtained.
[0316] Phase D [0317] The components of phase D were added after the homogenization of phase C in the following order: [0318] The icing sugar was slowly added to phase C and mixed under high/medium speed using the Dispermat™ (4 000 rpm, 5-10 minutes, dissolver impeller diameter: 40 mm) [0319] Then, the water was added at the end and mix by hand.
[0320] The quantity of produced final coating formulation was 100 g for each case.
[0321] After mixing and before spreading on the Leneta contrast cards, the final icing sugar coating formulation has been mixed for 2 minutes at 3 000 rpm using a SpeedMixer™ DAC 150.1 FVZ (from Hauschild, Hamm, Germany).
[0322] The below Table 2 shows an overview over the produced final coating formulations and lists all of the components used as well as their quantities.
TABLE-US-00002 TABLE 2 Quantities of components used in the final coating formulations Ingredients % w/w Formula 8 9 10 11 12 13 14 15 16 17 18 C) Aqua dem. 7.2 1.0 4.0 4.0 2.5 2.5 2.0 1.4 0.9 2.0 — Emulsifier — — 2.5 1.9 1.0 1.0 0.6 0.3 0.5 0.7 — Emulsifier 12.8 12.4 — — — — — — — — — solution (Formula 0) TiO.sub.2 Paste — 0.9 — — — — — — — — — (Formula 1) GCC 1 Paste — — 14.0 28.0 49.0 — — — — — — (Formula 2) GCC 2 Paste — — — — — 49.0 — — — — 31.0 (Formula 3) GCC 3 Paste — — — — — — 56.0 — — — — (Formula 4) SRCC 1 Paste — — — — — — — 26.3 — — 16.4 (Formula 5) SRCC 2 Paste — — — — — — — — 23.60 — — (Formula 6) SRCC 3 Paste — — — — — — — — — 21.30 — (Formula 7) D) Icing sugar 80.0 79.5 70.0 60.0 45.0 45.0 40.0 72.0 75.0 76.0 52.6 Aqua dem. — 6.2 9.5 6.1 2.5 2.5 1.4 — — — — 100 100 100 100 100 100 100 100 100 100 100
[0323] The following Table 3 gives an overview over the amount of pigment material that was present in the final coating formulations shown in Table 2.
TABLE-US-00003 TABLE 3 amount of pigment material present in the final coating formulations Formula 9 10 11 12 13 14 15 16 17 18 TiO.sub.2 (%) 0.5 — — — — — — — — — GCC 1 (%) — 10.0 20.0 35.0 — — — — — — GCC 2 (%) — — — — 35.0 — — — — 22.2 GCC 3 (%) — — — — — 40.0 — — — — SRCC 1 (%) — — — — — — 8.0 — — 5.0 SRCC 2 (%) — — — — — — — 5.0 — — SRCC 3 (%) — — — — — — — — 4.0 —
[0324] Finally, Table 4 shows the R(y) white part and R(y) black part as well as the covering power (in %) that was measured for the final coating formulations listed in Table 2.
TABLE-US-00004 TABLE 4 Covering power (in %) and R(y) white part and R(y) black part for the produced final coating formulations Covering power Formula R(y) white part R(y) black part (%) 8 85.5 28.6 33.4 9 85.6 41.2 48.2 10 84.9 28.3 33.3 11 85.0 33.6 39.5 12 85.0 41.2 48.5 13 85.3 39.5 48.7 14 85.6 41.3 48.2 15 84.3 40.1 47.6 16 84.9 36.2 42.6 17 84.5 36.5 43.1 18 85.0 46.1 54.2
[0325] From the above results it is apparent that surface-reacted calcium carbonates provide a similar coverage to sugar coatings containing 20 to 40 wt.-% of ground calcium carbonates (Formulation Nos. 11 to 13) but at lower concentrations (8 wt.-%, 5 wt.-% and 4 wt.-% for Formulation Nos. 14 to 16, respectively).
[0326] Also, the surface-reacted calcium carbonates provide a similar coverage to a sugar coating containing titanium dioxide. The best covering was obtained with a mixture of a ground calcium carbonate and a surface-reacted calcium carbonate, and this covering was even better than the one provided by titanium dioxide.
[0327] The results are also shown in
[0328] B. Coating of Chewing Gum Cores with a Coating Formulation
[0329] The present example exemplifies the coating of chewing gum cores with different sugar/polyol and mineral material formulations.
[0330] Also, the coating strength and the coating thickness of the obtained coated chewing gums was determined.
[0331] Coating of Chewing Gum Cores with Coating Formulations
[0332] The coating of the gum cores was carried out in a standard coating pan with a batch size of 10 kg.
[0333] The formulations used for coating of the gum cores are listed in following Table 5.
TABLE-US-00005 TABLE 5 Composition of formulations used for coating of chewing gum cores Ingredients % w/w Formula 19 20 21 22 23 24 25 26 TiO.sub.2 7.5 — — — 7.5 — — — GCC 1 — 525.0 — — — 525.0 — — GCC 2 — — — 330.0 — — — 330.0 SRCC 1 — — 120.0 75.0 — — 120.0 75.0 Crystal sugar 1492.5 975.0 1380.0 1095.0 — — — — Malitol — — — — 1492.5 975.0 1380.0 1095.0 Aqua dem. 500.0 500.0 500.0 500.0 642.5 642.5 642.5 642.5 2000 2000 2000 2000 2142.5 2142.5 2142.5 2142.5 Solids (%) 75 75 75 75 70 70 70 70 Percentage of 0.5 35.0 8.0 5.0 SRCC 0.5 35.0 8.0 5.0 SRCC pigment material 1 + 22.0 1 + 22.0 in formulation GCC 2 GCC 2 based on solids (%)
[0334] The coating formulations containing the crystal sugar were prepared with a solids content of 75 wt.-%, based on the total weight of the coating formulation, i.e. 1 part water and 3 parts of a mix of crystal sugar and pigment material(s). The sugar-free coating formulations containing the sugar alcohol malitol were prepared with a solids content of 70 wt.-%, based on the total weight of the coating formulation, i.e. 1 part of water and 2.33 parts of a mix the sugar alcohol malitol and pigment material(s). The coating formulations were prepared at a temperature between 70 and 80° C. under stiffing.
[0335] The coating formulations were applied on the gum cores by pouring the coating formulation onto the gum core mass followed by drying with hot air. The drying air had a temperature of 55° C. The application of coating formulation followed by a drying cycle was carried out until a desired coating amount of around 20 to 35% w/w was achieved.
[0336]
[0337] Measurement of the Coating Strength and the Coating Thickness
[0338] The coating strength was measured using an Anton Paar MCR 301 rheometer instrument. The geometry plate was moved with a constant speed of 0.1 mm/sec and the force was measured while pressing the chewing gum dragee (
[0339] The thickness of the chewing gum coating was calculated by difference between height of coated chewing gum core and uncoated chewing gum cores. The strength of coating was determined by the point in measurement graph where there was sudden dip into the force, this was due to the breakage of chewing gum coating (
[0340] As seen clearly in
[0341] As can be seen in
[0342] C. Measurement of the Drying Time
[0343] Method for preparing the coating composition:
[0344] All compositions were prepared on the basis of the W/W total solids (TS) in the composition, i.e. 50% TS composition means 50 grams of solids in 100 gram of final composition.
[0345] The compositions tested had 27.27% TS; 10% TS and 5% TS.
[0346] Despite of changes in TS percentage of composition, the ratio of sugar, water and other components were constant. The SRCC coating composition had 92% sugar and 8% SRCC 1 of solids. The TiO.sub.2 composition had 99.5% sugar and 0.5% TiO.sub.2 of solids. The reference sugar composition had 100% solids sugars.
[0347] Equipment used: [0348] Weighing scale—Mettler Toledo XS603S [0349] Oven for drying the films—Hera Therm oven OMH180-S [0350] Magnetic Stirrer—Variomag Multipoint [0351] Beaker for Mixing—Duran 150 mL
[0352] The compositions were prepared in the steps given below: [0353] The required water was weighed in a glass beaker [0354] The sugar was put in water under constant stirring at 600 rpm for 10 min [0355] The SRCC 1 or TiO.sub.2 was added in a next step into the sugar composition at constant stirring rate of 600 rpm [0356] The composition was mixed under constant stirring of 600 rpm for 20 min
[0357] The drying of the compositions for film formation was performed in the steps given below: [0358] 3 gram of composition were poured on an aluminium plate (Rotilabo Probenschalen 28 mL) [0359] The aluminum plate was gently moved to make a constant film on the plate [0360] The plate was transferred in the oven and dried at 90° C. and the weight of the plate was measured after 30, 60 and 120 minutes (T30, T60 and T120) [0361] The moisture left in the films was calculated by initial weight and weight after drying
TABLE-US-00006 TABLE 6 Samples used for the drying experiments Amount of Amount of fine Amount of SRCC 1 Sample water [g] powdered sugar [g] or TiO.sub.2 [g] 27% TS-SRCC 1 73 2.16 24.84 27% TS-TiO.sub.2 73 0.135 26.865 27% TS-Sugar 73 27 0 10% TS-SRCC 1 90 9.2 0.8 10% TS-TiO.sub.2 90 9.95 0.05 10% TS-Sugar 90 90 0 5% TS-SRCC 1 95 4.6 0.4 5% TS-TiO.sub.2 95 4.975 0.025 5% TS-Sugar 95 5 0
TABLE-US-00007 TABLE 7 Drying performance at 27% TS Moisture content in film (W/W %) Sample T0 T30 T60 T120 27% TS-SRCC 1 73.00% 5.13% 4.14% 3.92% 27% TS-TiO.sub.2 73.00% 5.75% 4.65% 4.33% 27% TS-Sugar 73.00% 5.89% 4.58% 4.14%
TABLE-US-00008 TABLE 8 Drying performance at 10% TS Moisture content in film (W/W %) Sample T0 T30 T60 T120 10% TS-SRCC 1 90.00% 0.95% 0.51% 0.51% 10% TS-TiO.sub.2 90.00% 1.18% 0.75% 0.53% 10% TS-Sugar 90.00% 1.30% 0.87% 0.87%
TABLE-US-00009 TABLE 9 Drying performance at 5% TS Moisture content in Film (W/W %) Sample T0 T30 T60 T120 5% TS-SRCC 1 95.00% 0.14% 0.03% 0.03% 5% TS-TiO.sub.2 95.00% 0.25% 0.14% 0.14% 27% TS-Sugar 95.00% 0.75% 0.54% 0.32%
[0362] It is clearly demonstrated by the data set out in tables 7 to 9 that a surface-reacted calcium carbonate reduces the moisture content in the prepared films faster than TiO.sub.2 and only sugar films and also reduces the drying time. Due to the increased drying performance of the edible composition of the present invention, this composition is suitable as an edible coating and/or filling for a food, pharmaceutical and neutraceutical product.
[0363] D. Opacifying Efficiency of Films Prepared from the Edible Compositions
[0364] The present example exemplifies the opacifying efficiency of the inventive edible compositions for coatings and/or fillings for food, pharmaceutical and neutraceutical products.
[0365] Especially, the opacifying efficiency of surface-reacted calcium carbonate compared to titanium dioxide in films was determined on a weight replacement basis (I g of titanium dioxide replaced by 1 g of surface-reacted calcium carbonate).
[0366] A basecoat as described in table 10 below was prepared by using a dispersing mixer (Dispermat) at approx. 1 000 to 2 000 rpm.
TABLE-US-00010 TABLE 10 composition of the basecoat parts g PEG 600S (plasticizer) 4.0 20 Water 85.2 426 Pharmacoat 606 (HPMC) 10.0 50 Dimethicone (defoaming agent) 0.5 2.5 SLS (surfactant) 0.3 1.5 Sum 100.0 500
[0367] This basecoat was used for the preparation of a film with different pigments according to the formulations listed in Table 11 below.
TABLE-US-00011 TABLE 11 Films with different pigments Ratio HPMC + Basecoat plasticizer/ Film (g) Pigment Addition pigment 1 50 13 g TiO.sub.2 2% Tween 60V 7/13 Pharma 2 50 13 g SRCC 1 2% Tween 60V 7/13 Pharma
[0368] The films were prepared as follows:
[0369] The Tween 60V Pharma was added into the basecoat under mixing with the dispermat. The pigment was then added to the basecoat. First, the obtained mixture was mixed by hand, then, mixed in a high-speed mixer at 3 000 rpm for 1 min, then mixed by hand again and finally homogenised in a high-speed mixer at 3 000 rpm for 1 min.
[0370] Subsequently, films were applied on Leneta contrast cards in accordance with the preparation of a coated surface set out under the measurement methods above. The films were then allowed to dry at ambient temperature until dryness. The characteristics of the films are shown in
[0371] From
[0372] The basecoat set out in table 10 was also used for the preparation of color films with different pigments according to the formulations listed in Table 12 below as follows:
TABLE-US-00012 TABLE 12 Colour films with different pigments Ratio HPMC + Basecoat plasticiser/ Film (g) Pigment Addition pigment/lake SRCC 1 50 13 g SRCC1 2% Tween 60V 13/7/4 Pharma TiO.sub.2 50 13 g TiO2 2% Tween 60V 13/7/4 Pharma
[0373] The Tween 60V Pharma was added into the basecoat under mixing with the dispermat. The pigment was then added to the basecoat. First, the obtained mixture was mixed by hand, then, mixed in a high-speed mixer at 3 000 rpm for 1 min, then mixed by hand again and finally homogenised in a high-speed mixer at 3 000 rpm for 1 min. Al-carmine lake pigment (Al-Carmine Lake 50%, FCCII, E120) was then added to the mixture and mixed by hand and then in a high-speed mixer for 15 minutes.
[0374] Subsequently, films were applied on Leneta contrast cards in accordance with the preparation of a coated surface set out under the measurement methods above. The films were then allowed to div at ambient temperature until dryness. The characteristics of the films are shown in
[0375] The color characteristics of the films set out in table 12 were determined. The test was carried out with an Al-Carmine Lake 50%, FCCII, E120 water insoluble powder. The color characteristics of the films are set out in table 13 below and
TABLE-US-00013 TABLE 13 Color characteristics of the films Yellowness Film L* a* b* value TiO.sub.2 54.77 42.86 −1.64 55.42 SRCC 1 40.37 52.99 9.79 135.35
[0376] From the color characteristics of the films, it can be gathered that a film comprising the surface-reacted calcium carbonate has a brighter color than a film comprising the same amount of titanium dioxide.
[0377] Summarizing the above, the edible composition of the present invention, i.e. wherein titanium dioxide is replaced by surface-reacted calcium carbonate, is suitable as an edible coating and/or filling for food, pharmaceutical and neutraceutical products, and especially an edible coating for pharmaceutical and neutraceutical products, as it provides a similar opacifying efficiency but a brighter color than a corresponding titanium dioxide containing composition.