CA2431856A1 - Method of controlling release of caffeine in chewing gum and gum produced thereby - Google Patents
Method of controlling release of caffeine in chewing gum and gum produced thereby Download PDFInfo
- Publication number
- CA2431856A1 CA2431856A1 CA002431856A CA2431856A CA2431856A1 CA 2431856 A1 CA2431856 A1 CA 2431856A1 CA 002431856 A CA002431856 A CA 002431856A CA 2431856 A CA2431856 A CA 2431856A CA 2431856 A1 CA2431856 A1 CA 2431856A1
- Authority
- CA
- Canada
- Prior art keywords
- caffeine
- chewing gum
- gum
- release
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
Links
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 title claims abstract description 389
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 title claims abstract description 206
- 229960001948 caffeine Drugs 0.000 title claims abstract description 192
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 title claims abstract description 192
- 235000015218 chewing gum Nutrition 0.000 title claims abstract description 42
- 229940112822 chewing gum Drugs 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims description 64
- 239000011248 coating agent Substances 0.000 claims abstract description 33
- 238000000576 coating method Methods 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 60
- 239000000843 powder Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000007921 spray Substances 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
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- 239000004208 shellac Substances 0.000 claims description 13
- 229940113147 shellac Drugs 0.000 claims description 13
- ZLGIYFNHBLSMPS-ATJNOEHPSA-N shellac Chemical compound OCCCCCC(O)C(O)CCCCCCCC(O)=O.C1C23[C@H](C(O)=O)CCC2[C@](C)(CO)[C@@H]1C(C(O)=O)=C[C@@H]3O ZLGIYFNHBLSMPS-ATJNOEHPSA-N 0.000 claims description 13
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- 235000003599 food sweetener Nutrition 0.000 claims description 12
- -1 physically-modified caffeine salt compound Chemical class 0.000 claims description 12
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- IAOZJIPTCAWIRG-QWRGUYRKSA-N aspartame Chemical compound OC(=O)C[C@H](N)C(=O)N[C@H](C(=O)OC)CC1=CC=CC=C1 IAOZJIPTCAWIRG-QWRGUYRKSA-N 0.000 claims description 9
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- NUFKRGBSZPCGQB-FLBSXDLDSA-N (3s)-3-amino-4-oxo-4-[[(2r)-1-oxo-1-[(2,2,4,4-tetramethylthietan-3-yl)amino]propan-2-yl]amino]butanoic acid;pentahydrate Chemical compound O.O.O.O.O.OC(=O)C[C@H](N)C(=O)N[C@H](C)C(=O)NC1C(C)(C)SC1(C)C.OC(=O)C[C@H](N)C(=O)N[C@H](C)C(=O)NC1C(C)(C)SC1(C)C NUFKRGBSZPCGQB-FLBSXDLDSA-N 0.000 claims description 4
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 5
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- 229920002367 Polyisobutene Polymers 0.000 description 1
- 241001237728 Precis Species 0.000 description 1
- ISRUGXGCCGIOQO-UHFFFAOYSA-N Rhoden Chemical compound CNC(=O)OC1=CC=CC=C1OC(C)C ISRUGXGCCGIOQO-UHFFFAOYSA-N 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 102100021782 SH3 domain-containing protein 19 Human genes 0.000 description 1
- 101150091821 SLC3A1 gene Proteins 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- UEDUENGHJMELGK-HYDKPPNVSA-N Stevioside Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O UEDUENGHJMELGK-HYDKPPNVSA-N 0.000 description 1
- 241001415849 Strigiformes Species 0.000 description 1
- 244000299461 Theobroma cacao Species 0.000 description 1
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- YGCFIWIQZPHFLU-UHFFFAOYSA-N acesulfame Chemical compound CC1=CC(=O)NS(=O)(=O)O1 YGCFIWIQZPHFLU-UHFFFAOYSA-N 0.000 description 1
- 229960005164 acesulfame Drugs 0.000 description 1
- GAMPNQJDUFQVQO-UHFFFAOYSA-N acetic acid;phthalic acid Chemical compound CC(O)=O.OC(=O)C1=CC=CC=C1C(O)=O GAMPNQJDUFQVQO-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
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- 235000010443 alginic acid Nutrition 0.000 description 1
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
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- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
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- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 244000309466 calf Species 0.000 description 1
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- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 235000010418 carrageenan Nutrition 0.000 description 1
- 239000000679 carrageenan Substances 0.000 description 1
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- 229940113118 carrageenan Drugs 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000015111 chews Nutrition 0.000 description 1
- 239000010634 clove oil Substances 0.000 description 1
- 229940110456 cocoa butter Drugs 0.000 description 1
- 235000019868 cocoa butter Nutrition 0.000 description 1
- 229940125846 compound 25 Drugs 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000000625 cyclamic acid and its Na and Ca salt Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- JXSJBGJIGXNWCI-UHFFFAOYSA-N diethyl 2-[(dimethoxyphosphorothioyl)thio]succinate Chemical compound CCOC(=O)CC(SP(=S)(OC)OC)C(=O)OCC JXSJBGJIGXNWCI-UHFFFAOYSA-N 0.000 description 1
- QGGZBXOADPVUPN-UHFFFAOYSA-N dihydrochalcone Chemical compound C=1C=CC=CC=1C(=O)CCC1=CC=CC=C1 QGGZBXOADPVUPN-UHFFFAOYSA-N 0.000 description 1
- PXLWOFBAEVGBOA-UHFFFAOYSA-N dihydrochalcone Natural products OC1C(O)C(O)C(CO)OC1C1=C(O)C=CC(C(=O)CC(O)C=2C=CC(O)=CC=2)=C1O PXLWOFBAEVGBOA-UHFFFAOYSA-N 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
- 230000009429 distress Effects 0.000 description 1
- 230000009189 diving Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- KXGVIPZFMKMPFU-OATXVPTESA-N fad-001 Chemical compound O([C@H]1C[C@@](O)(CC=2C(O)=C3C(=O)C=4C=CC=C(C=4C(=O)C3=C(O)C=21)OC)C(=O)CO)[C@@H]1O[C@@H](C)[C@@H](O)[C@@H](O)[C@H]1F KXGVIPZFMKMPFU-OATXVPTESA-N 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- 235000010417 guar gum Nutrition 0.000 description 1
- 239000000665 guar gum Substances 0.000 description 1
- 229960002154 guar gum Drugs 0.000 description 1
- 239000008123 high-intensity sweetener Substances 0.000 description 1
- 239000008172 hydrogenated vegetable oil Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000010420 locust bean gum Nutrition 0.000 description 1
- 239000000711 locust bean gum Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 235000010449 maltitol Nutrition 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- HYIMSNHJOBLJNT-UHFFFAOYSA-N nifedipine Chemical compound COC(=O)C1=C(C)NC(C)=C(C(=O)OC)C1C1=CC=CC=C1[N+]([O-])=O HYIMSNHJOBLJNT-UHFFFAOYSA-N 0.000 description 1
- 235000013615 non-nutritive sweetener Nutrition 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229940061319 ovide Drugs 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- 229960001462 sodium cyclamate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- HJHVQCXHVMGZNC-JCJNLNMISA-M sodium;(2z)-2-[(3r,4s,5s,8s,9s,10s,11r,13r,14s,16s)-16-acetyloxy-3,11-dihydroxy-4,8,10,14-tetramethyl-2,3,4,5,6,7,9,11,12,13,15,16-dodecahydro-1h-cyclopenta[a]phenanthren-17-ylidene]-6-methylhept-5-enoate Chemical compound [Na+].O[C@@H]([C@@H]12)C[C@H]3\C(=C(/CCC=C(C)C)C([O-])=O)[C@@H](OC(C)=O)C[C@]3(C)[C@@]2(C)CC[C@@H]2[C@]1(C)CC[C@@H](O)[C@H]2C HJHVQCXHVMGZNC-JCJNLNMISA-M 0.000 description 1
- MJZVAJZDKMFTBN-UHFFFAOYSA-M sodium;2-hydroxybenzoate;1,3,7-trimethylpurine-2,6-dione Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O.CN1C(=O)N(C)C(=O)C2=C1N=CN2C MJZVAJZDKMFTBN-UHFFFAOYSA-M 0.000 description 1
- CAKRAHQRJGUPIG-UHFFFAOYSA-M sodium;[4-azaniumyl-1-hydroxy-1-[hydroxy(oxido)phosphoryl]butyl]-hydroxyphosphinate Chemical compound [Na+].NCCCC(O)(P(O)(O)=O)P(O)([O-])=O CAKRAHQRJGUPIG-UHFFFAOYSA-M 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229940013618 stevioside Drugs 0.000 description 1
- OHHNJQXIOPOJSC-UHFFFAOYSA-N stevioside Natural products CC1(CCCC2(C)C3(C)CCC4(CC3(CCC12C)CC4=C)OC5OC(CO)C(O)C(O)C5OC6OC(CO)C(O)C(O)C6O)C(=O)OC7OC(CO)C(O)C(O)C7O OHHNJQXIOPOJSC-UHFFFAOYSA-N 0.000 description 1
- 235000019202 steviosides Nutrition 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000009495 sugar coating Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229920003176 water-insoluble polymer Polymers 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G4/00—Chewing gum
- A23G4/06—Chewing gum characterised by the composition containing organic or inorganic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G4/00—Chewing gum
- A23G4/02—Apparatus specially adapted for manufacture or treatment of chewing gum
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G4/00—Chewing gum
- A23G4/02—Apparatus specially adapted for manufacture or treatment of chewing gum
- A23G4/025—Apparatus specially adapted for manufacture or treatment of chewing gum for coating or surface-finishing
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G4/00—Chewing gum
- A23G4/06—Chewing gum characterised by the composition containing organic or inorganic compounds
- A23G4/068—Chewing gum characterised by the composition containing organic or inorganic compounds containing plants or parts thereof, e.g. fruits, seeds, extracts
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G4/00—Chewing gum
- A23G4/06—Chewing gum characterised by the composition containing organic or inorganic compounds
- A23G4/12—Chewing gum characterised by the composition containing organic or inorganic compounds containing microorganisms or enzymes; containing paramedical or dietetical agents, e.g. vitamins
- A23G4/126—Chewing gum characterised by the composition containing organic or inorganic compounds containing microorganisms or enzymes; containing paramedical or dietetical agents, e.g. vitamins containing vitamins, antibiotics
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G4/00—Chewing gum
- A23G4/18—Chewing gum characterised by shape, structure or physical form, e.g. aerated products
- A23G4/20—Composite products, e.g. centre-filled, multi-layer, laminated
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Botany (AREA)
- Health & Medical Sciences (AREA)
- Microbiology (AREA)
- Nutrition Science (AREA)
- Confectionery (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
A method for producing a chewing gum with a controlled release of caffeine, as well as the chewing gum so produced, is obtained by physically modifying caffeine's properties by coating and drying. Caffeine is coated by encapsulation, partially coated by agglomeration, entrapped by absorption, or treated by multiple steps of encapsulation, agglomeration, and absorption. The coated caffeine is then preferably co-dried and particle sized to produce a release-modified caffeine for use in chewing gum. When incorporated into the chewing gum, these particles are adapted to produce a fast release or a delayed release when the gum is chewed.
Description
~'~;~:b~~~ ~..~~ CaFI~'~~'~~.~rG ~I3~~ ."~
~~~e~ ~C?~f~~~..'F°~3 - 5 ~X'9.~_"~C7R;JI71VT'3 C:~r' ''~'r~~ ~i:?~~~~J'~"1'~''~ L~
'~~ae p:~esexw~ ~.~.~e~~~.caxa ~e~! a~.es tic? me~.~~ods fc~r ~~:o~.uo~.ng olze~a~..g g~~~~ ~~~b'e ~Sa~°~~.~~~.~.~:~.yr ~:~.e ~.z-a~re~aL~.o~a ~ela~.c~s ' ~.~a:r'oc~~c:°~ x~g oi?e~ir~g g~c~
con~aa.~.ir~g a ~.igl~ agr~o°~.n~. of s~.izn~.~.an~ ~~°~o~vz3 as ~.0 caffe~~ea The s~af:ce~.~ae ~~a~ is added ~.o ?:~e ei~.e~r~~g gtxm ra.as hegira. ~.~ea~ec~ ~.~.o ~~o~~~o~ ~ ~.s ~a~e of ~e~.e~.se ~~x ol~e$~r~ng gxzma xx ~ eo.er~.~. ~rea~°s ~ ef f ~P~°~s- ~a~ ~4 hee~~. ~.e~rc~~e~
~o corx~~olli~.g ~~elee.se cl~a~ao~~r~.s~~~s o°f ~a~a..o~.s ~5 ~..~gyec~.~.era~s ~~ ~.~e~.~~?~.g g'u~c~s ~~c~s~ ~xo~a~~i.~~°;
a~~e:mp~,s ~ya~re heed made ~o ~.e:~.a~ c~-!~ ~e~~.ease of so~ee'~e~e:~s a?2tY f~..a~'oY',.~"~ 1. Ti ~Ycs.~ ~ G12~ ~:ile'6tp~'~7C~° g~I'~'t fo~'121~:~'d<c"i i_3 C?'1~ L.o ~.~ereh~r I-eng~he~ ~a~e sa~~_~f~ao.~ocb~s.e~r:a.~~g Sr~.me c~f ~.a~e game Dela~~_~g she ~~elease of s~~ee~~ey~ers a.x~~~
~~3 flavors oar also a~ci~. a,-1 z~°~c3esa~ah~ a i~~e~~o~~e:c~.rxg ~o~rs~ of swee~x~.ess r~_r f~a~o~° r~x~r.~ng tYle a~.~z~.~~.ai.
C1'3eS~77 Tlg ~e ~'~.~5~ m ~~'a ~~.e '.~lt.!'~e~'_" 11a~2C.9 ~O%i~~ .'L I$-aF'r'- ~'eC~.:~_e~.c..s'°u~
~'I~'Ve heel ~~°a~E'.Q. ~C% a~' s. C~ ? ~C°~,°'_'ea~e ~~"tQ~'~ a.: ~'a~~
~°e~ease in ohe~r~1_rlg g°o ___ ~es~.de~ ~=~.~ee~e~.xe:~s, o~~.e~° ~~g~e~.ie~l~s mad z~e~:ire ~ co~.~~ol~ e;~. release f~°o~rc c:~?e~.~:i.~°ag gwm ~~.~.m.'ala~.~s soon as oaffe:~~e r~a~~° he added ~:o g~~~~
ilo=~re~re~s s~im~.~a~'ts ~..~e xxov ge~ae~°a~~.y .c~e s eased ~Je ~ead~.~ ~°~ C'affe~.x-7e mad he e~.car~s~.ia~e~ ~~ a wads=r ~0 so:L~.~blc ma~~°:~~ s~o'~ ~.he.~.~~.~~g ~.~ae e:~~e~a~x~g pe.~~od, ~.~°xe oaffea.l~e ~na~ Ire ~°e~easec~ qzxi~.kl~~
~°fwsxg,~ ~~.~.g o~.rx a fast ~elea:~e of s~.~.~~~ axl~w a~ abl a he~e:c-age m ~'h:~.s i~o~xld al.~o~- o~e~ring gym ~o he a ~ax~~~e~~° ~o~°
r°af'_Fe~~:w ~'_t1~9 ~t~"~.~~1 1GS fa ~~ :L.~~.a~.~"~-a ~ i:_o La a°31'd E'f:.~~'~:~°i.'EPe ~ C~.II1LL~~TI~:. m ~:r~. ~~e. c~.'~~a~° ~xa~.daw se~~oxxs ~a,~~e °;~~°ol~:~ems ma~~ a~~se heca~ase of ~:~le h~.~,~.ex: ~.a~~re ef o~.ffe_i_rxeo J a prc?2orlged o°~ debarred ~-el~ase c~f ~af~.=e~~le ~ro~xlc~ a~.Lc~z-r fo~° ~~e :~~e of oaffe~x~e ~.rx g$ h~~ ~.he ~L~ ~o~~ le~°e~ of ~°e~.ease mad Yep '~r~e ~.e~e~~ he~:~~r ~,~~s l taste th5reshol d ax~~. not give Chewing g~u~ a bitter taste quality. ~.'1 so, s:~o~:~ release may ~~.leaw some - individuals to mere ea.s~.ly tolerate Caffe~.~xe a nd not cause ~:astro-intestinal distress.
Thus, there ate specific ad~Yante.ges ?~.o adding caffe~.ne to chet~=vng g m by c.ontro:Lled rn~.ease me ChanlSITiS .
Caffeine use vn crre~ring gum was disclosed in t7. S . ~~atent ~To. ~., X98, ~~0 .
~ 0 Chewid~g gum cor°~r'aining caffeir~e as a stimulant and to cc:nbat fatigue: and rraigts.ane lleadaCheS lS d7.SCiGSe~ .I~ I"'T'"enC~'1 ~'atel3t ~o. 2, 845, 988 and in ~fest ~e:cr~~any Patent i'~o. 4, 34~, 568. ' ,also, c~~C ~apar~ese latent. ~ub~~.zcat~ ons, NoS . a ~ 91-? I245tJ and J~~ :~~.-25.533, C~:1.,.-r'ZG°~..oSe Ll~e~ Gf caffeine in che~,q~.ng gum t<o rerr~..uce dro~~siness.
n Ja.parese Patent ~ub~.icatiGre ~~o. J'P 96-01.93 e0, caffeine is added to ohe~xing gum as ara after meal chewing gum to replace tooth brushing.
Caf>=sine is a We~.l ~Cnown stimu i.ant from ccffee and tea, anfd. sevex'a~. patents dzsclc~se use of coffee or tea in g~~.mf such as ~°~apanese ~~atent .
Publication Pro. Jr 94-30391, South TCorea Patent 28 zubl icatiorl IV'o" 94-00868, and PCT Patent.
hubiication Ikon ~~~G 9-G=OG088.
SLJMMr~.R'~'~F TI~p; ~.r~:l~Tr~'i~~' The present inv,:niion is a r~re~~oci of producing cne~,ving bum with --8 0 physically modified caffeine to control its reiease rate, trte ;nethod cotnprisirzg draining a quantity of caffeizAw v~~ith a r:~odifyi~xg ~ger~t to ~:orrt:a a ph.ysicaZly-n~odii"~cd caffeine, and teen wdding a r.;uantity ofthe physiealiy-modified caffeine to a chewing guru ~~u~~uls.tion to p~'ovide a caffeine ievel it the guna 38 of fz-orr~ about 0.~% to about ~°/~.
The present inver~~tio~~ also relates to the chewing gum so procauced.
~affeir~e rnay be added to sucrose type gam oa~~ula~ior~s, rcislr~,cing a smali quantity of sucrose. ~'he forrn;~iatson nay Ire a iorv or nigh c~~cisture forn~uiation containing tow or higi~ a4nounts of moisture containing syr~zp.
~affeir~e nay also he used i~-~ Iow or z~oa~-s~ gar gam fort~~a~latic;ns, ~-e,hlaei~~g a small ciuantity of sorbitoi, n-,ar~~itc~~, ctz~er palyols ar carbatlydrates.. hora--sugar f~r;rmulations gray include low or high ~moiswure sugar free cheeaing gums.
Caffeine may be corrbir_ed or cadrid with bulk scaeeteners typical,.~y used in chewing c,urr~, such as sucrose, dextrose, fructose arid maltodewktrins, as well as sugar alcohols such as sorbitcl, manv~itol, r:yiitol, rraltitol, lactitol, hydrogenated iscmalt7~lose and hydrogenated starch hydrol~.~zates .
IC The modified :gel ease rate noted above may be a fast release or a delayed release. The mod~_fied release of caffeine is obta=_ne.d by encapsulation, partial encapsulation or p~zvtial coating, entrapzr~ervt oz: absorption caith high or low water soluble materia~Ls or wager insolub~_e materials . The procedures for modifyi_rlg the c~:ffeino incaude spray drying, spray ch.Llling, fluwd bed coating, coacervation, extrusion arid other agglomerating and standard encapsulating techniquess Caffeine may also be absorbed onto an inert or water-insoluble material.
~~~e~ ~C?~f~~~..'F°~3 - 5 ~X'9.~_"~C7R;JI71VT'3 C:~r' ''~'r~~ ~i:?~~~~J'~"1'~''~ L~
'~~ae p:~esexw~ ~.~.~e~~~.caxa ~e~! a~.es tic? me~.~~ods fc~r ~~:o~.uo~.ng olze~a~..g g~~~~ ~~~b'e ~Sa~°~~.~~~.~.~:~.yr ~:~.e ~.z-a~re~aL~.o~a ~ela~.c~s ' ~.~a:r'oc~~c:°~ x~g oi?e~ir~g g~c~
con~aa.~.ir~g a ~.igl~ agr~o°~.n~. of s~.izn~.~.an~ ~~°~o~vz3 as ~.0 caffe~~ea The s~af:ce~.~ae ~~a~ is added ~.o ?:~e ei~.e~r~~g gtxm ra.as hegira. ~.~ea~ec~ ~.~.o ~~o~~~o~ ~ ~.s ~a~e of ~e~.e~.se ~~x ol~e$~r~ng gxzma xx ~ eo.er~.~. ~rea~°s ~ ef f ~P~°~s- ~a~ ~4 hee~~. ~.e~rc~~e~
~o corx~~olli~.g ~~elee.se cl~a~ao~~r~.s~~~s o°f ~a~a..o~.s ~5 ~..~gyec~.~.era~s ~~ ~.~e~.~~?~.g g'u~c~s ~~c~s~ ~xo~a~~i.~~°;
a~~e:mp~,s ~ya~re heed made ~o ~.e:~.a~ c~-!~ ~e~~.ease of so~ee'~e~e:~s a?2tY f~..a~'oY',.~"~ 1. Ti ~Ycs.~ ~ G12~ ~:ile'6tp~'~7C~° g~I'~'t fo~'121~:~'d<c"i i_3 C?'1~ L.o ~.~ereh~r I-eng~he~ ~a~e sa~~_~f~ao.~ocb~s.e~r:a.~~g Sr~.me c~f ~.a~e game Dela~~_~g she ~~elease of s~~ee~~ey~ers a.x~~~
~~3 flavors oar also a~ci~. a,-1 z~°~c3esa~ah~ a i~~e~~o~~e:c~.rxg ~o~rs~ of swee~x~.ess r~_r f~a~o~° r~x~r.~ng tYle a~.~z~.~~.ai.
C1'3eS~77 Tlg ~e ~'~.~5~ m ~~'a ~~.e '.~lt.!'~e~'_" 11a~2C.9 ~O%i~~ .'L I$-aF'r'- ~'eC~.:~_e~.c..s'°u~
~'I~'Ve heel ~~°a~E'.Q. ~C% a~' s. C~ ? ~C°~,°'_'ea~e ~~"tQ~'~ a.: ~'a~~
~°e~ease in ohe~r~1_rlg g°o ___ ~es~.de~ ~=~.~ee~e~.xe:~s, o~~.e~° ~~g~e~.ie~l~s mad z~e~:ire ~ co~.~~ol~ e;~. release f~°o~rc c:~?e~.~:i.~°ag gwm ~~.~.m.'ala~.~s soon as oaffe:~~e r~a~~° he added ~:o g~~~~
ilo=~re~re~s s~im~.~a~'ts ~..~e xxov ge~ae~°a~~.y .c~e s eased ~Je ~ead~.~ ~°~ C'affe~.x-7e mad he e~.car~s~.ia~e~ ~~ a wads=r ~0 so:L~.~blc ma~~°:~~ s~o'~ ~.he.~.~~.~~g ~.~ae e:~~e~a~x~g pe.~~od, ~.~°xe oaffea.l~e ~na~ Ire ~°e~easec~ qzxi~.kl~~
~°fwsxg,~ ~~.~.g o~.rx a fast ~elea:~e of s~.~.~~~ axl~w a~ abl a he~e:c-age m ~'h:~.s i~o~xld al.~o~- o~e~ring gym ~o he a ~ax~~~e~~° ~o~°
r°af'_Fe~~:w ~'_t1~9 ~t~"~.~~1 1GS fa ~~ :L.~~.a~.~"~-a ~ i:_o La a°31'd E'f:.~~'~:~°i.'EPe ~ C~.II1LL~~TI~:. m ~:r~. ~~e. c~.'~~a~° ~xa~.daw se~~oxxs ~a,~~e °;~~°ol~:~ems ma~~ a~~se heca~ase of ~:~le h~.~,~.ex: ~.a~~re ef o~.ffe_i_rxeo J a prc?2orlged o°~ debarred ~-el~ase c~f ~af~.=e~~le ~ro~xlc~ a~.Lc~z-r fo~° ~~e :~~e of oaffe~x~e ~.rx g$ h~~ ~.he ~L~ ~o~~ le~°e~ of ~°e~.ease mad Yep '~r~e ~.e~e~~ he~:~~r ~,~~s l taste th5reshol d ax~~. not give Chewing g~u~ a bitter taste quality. ~.'1 so, s:~o~:~ release may ~~.leaw some - individuals to mere ea.s~.ly tolerate Caffe~.~xe a nd not cause ~:astro-intestinal distress.
Thus, there ate specific ad~Yante.ges ?~.o adding caffe~.ne to chet~=vng g m by c.ontro:Lled rn~.ease me ChanlSITiS .
Caffeine use vn crre~ring gum was disclosed in t7. S . ~~atent ~To. ~., X98, ~~0 .
~ 0 Chewid~g gum cor°~r'aining caffeir~e as a stimulant and to cc:nbat fatigue: and rraigts.ane lleadaCheS lS d7.SCiGSe~ .I~ I"'T'"enC~'1 ~'atel3t ~o. 2, 845, 988 and in ~fest ~e:cr~~any Patent i'~o. 4, 34~, 568. ' ,also, c~~C ~apar~ese latent. ~ub~~.zcat~ ons, NoS . a ~ 91-? I245tJ and J~~ :~~.-25.533, C~:1.,.-r'ZG°~..oSe Ll~e~ Gf caffeine in che~,q~.ng gum t<o rerr~..uce dro~~siness.
n Ja.parese Patent ~ub~.icatiGre ~~o. J'P 96-01.93 e0, caffeine is added to ohe~xing gum as ara after meal chewing gum to replace tooth brushing.
Caf>=sine is a We~.l ~Cnown stimu i.ant from ccffee and tea, anfd. sevex'a~. patents dzsclc~se use of coffee or tea in g~~.mf such as ~°~apanese ~~atent .
Publication Pro. Jr 94-30391, South TCorea Patent 28 zubl icatiorl IV'o" 94-00868, and PCT Patent.
hubiication Ikon ~~~G 9-G=OG088.
SLJMMr~.R'~'~F TI~p; ~.r~:l~Tr~'i~~' The present inv,:niion is a r~re~~oci of producing cne~,ving bum with --8 0 physically modified caffeine to control its reiease rate, trte ;nethod cotnprisirzg draining a quantity of caffeizAw v~~ith a r:~odifyi~xg ~ger~t to ~:orrt:a a ph.ysicaZly-n~odii"~cd caffeine, and teen wdding a r.;uantity ofthe physiealiy-modified caffeine to a chewing guru ~~u~~uls.tion to p~'ovide a caffeine ievel it the guna 38 of fz-orr~ about 0.~% to about ~°/~.
The present inver~~tio~~ also relates to the chewing gum so procauced.
~affeir~e rnay be added to sucrose type gam oa~~ula~ior~s, rcislr~,cing a smali quantity of sucrose. ~'he forrn;~iatson nay Ire a iorv or nigh c~~cisture forn~uiation containing tow or higi~ a4nounts of moisture containing syr~zp.
~affeir~e nay also he used i~-~ Iow or z~oa~-s~ gar gam fort~~a~latic;ns, ~-e,hlaei~~g a small ciuantity of sorbitoi, n-,ar~~itc~~, ctz~er palyols ar carbatlydrates.. hora--sugar f~r;rmulations gray include low or high ~moiswure sugar free cheeaing gums.
Caffeine may be corrbir_ed or cadrid with bulk scaeeteners typical,.~y used in chewing c,urr~, such as sucrose, dextrose, fructose arid maltodewktrins, as well as sugar alcohols such as sorbitcl, manv~itol, r:yiitol, rraltitol, lactitol, hydrogenated iscmalt7~lose and hydrogenated starch hydrol~.~zates .
IC The modified :gel ease rate noted above may be a fast release or a delayed release. The mod~_fied release of caffeine is obta=_ne.d by encapsulation, partial encapsulation or p~zvtial coating, entrapzr~ervt oz: absorption caith high or low water soluble materia~Ls or wager insolub~_e materials . The procedures for modifyi_rlg the c~:ffeino incaude spray drying, spray ch.Llling, fluwd bed coating, coacervation, extrusion arid other agglomerating and standard encapsulating techniquess Caffeine may also be absorbed onto an inert or water-insoluble material.
2;~ Caffeine rnay be :::nodi.f~ie~ :in a multiple step process oomp~~ising any of tine processe:~, or a covnbination of the processes noted. Prior to er~oap,~ulat~_oi~, caffeine mU.y also be combined crith balk s~,~eet~ners including sucrose;
dextrose, fructose, maitod~o~xtrin or other built sweeteners, as wel 1 as sugar a ~ cohols suet: as sorbitol, rn~~amitol, xylitol, maititol, lactitol, hydrogenated iscrnaltulose and hydrogenated star e: hydrolyzates.
Lricr to encapsulation, caffeine may be combined with high-intensity SweP4e'':er_s,. including b~.r not limited to thaumatin, aSpartalTte, aiI_taIPe, aCesul°ame ~~, .SaCCi:aryn aCld and its salts, glycyr_Nhizin, cyclamate. and its salts, stevioside and dihydrochalcone:s . Co-cncap:~ulaL~_on of caffeine along U;it.~ a high-:int:.ensity swe_=etener may reduce the bitterness or caffe__ne and cor~.tro:L the sweetener rel ease with caffeine. Tr:is can improcre the quality of the gum product and increa se consumer aocept.abiW~_ity.
In addition to use of high-intensity sweetenersr S bitterness inhibitors such as sodium gluccnate, sodium ascorbate c.r other soc gum salts may be combineca wi. ~h caffeine prior to encapsu?atien to reduce the cverall bitterness caused b~T caffeine 2nd-resul~~ in a gum product having s_ncreased co:~sume.~ acceptability.
DFTA:CI~ED D~'SCR1PTI0'~t OF T~aE PREFFRRrD ;_,M30DIVE~:~TS
Caffeine :~ s a natural chemic~;1 fcund i.n a variety of food prcdwcts such as coffee, tea; cocoa, c1-~_ocolate, and various other beveraf.ges .. Caffeia~e is known as an effective.
I5 stimulant to increas~ energy and reduce drowsi=ness.
Caffeine has a naturally bitter taste. The bitterness, however, a~.:tually ir;~proves the flavor percepticn o~- some beverages such as coffee and carbonated be~,.eraces~
G~hen caffeine is added to chewing gum at a level cf about 0.2% to about ~o, caffeine imparts an int~snse bitterness to the chewing gum that lasts t~nroucrhout the chewing peri od. "'he higher the level used the: stronger the bitterness. At about 0.2~, which is about 5 mg per 2.7 gram stick, the bi tterness is below the =~.lmeshold lir:?~_t and 2~ is not readily di.s c;~,~.rn.~bl~~ . Taste lim°.~ts u_n chewing gum.
are generally about C.4~ (?0 mg) to about ~o (200 mg) of caffeine in a stick of gum. 'r~~e o0-80 mg lezTel of caffeine is about the level of cafLeine found in a comrent~_onal cup ey coffee. The ta_r_get level cf caffev.ne in stv_ck gum is about ~0 mg per sticky with a _r_ange of about 25-60 mg, so that a five stick package of gum would contair< about 200 mg of caffeine, or the equivalent of cafl:o ine i.r_ two strong cups of coffee. However, at this levE;1 caffei~~e bitterness cver~,Thelms the f~.a~ror in. itial 1y and lasts throughout the chewing period.
~~~~ 9b1231bS - S _ ~'~~J'd~~9b11~~77 ~$it.h t~Ae caffeine release x~~od~.f:i.e~. ~.o ~'esust in a fast release of caffeine '~~a~.t~.'2 t~~.e chewing gum solu~? es ar.,d sweeter~ers, the bitterness can be effeci~.ive:l~' reducec.._ vief high.-~~~tex2s~.t~P
sweeteners car ~e ~:lended with caffeine to release a t~~"re ~allle ~~.TTlea ir~:!ws ~c;3C3 Carl redL7.C~v-: 4~.,~'lE' hi~~;E.'~'%"~eS~
effecv. Ot:~e~' che:~~~~.ca:Ls that irrxhibi~° i~it.teLn~as r~tx~%
be b1 ended with caffeine Lo al so ~°ed.uce ~aitterness.
Caffeine is r~~s~ a h~.gh~.y waFaer so~.~~~~le '~ 0 substance and, therefore9 has a znoderate~.y slow re~.ease froze ch.ewia~.g gum. Caffeine iv 2 . L°s soluk~le 1Y1 ~ w c'~'d~.e?" at room ~~..'TL1'',r7era~4.T;Iane r ~S~ So~g l~b:~~~ : 3.n 'W'a.te~
at 80°C and 40o sol~le in boiling water. this gives caffei_le a r~.c~de~ate~ y s.l.o~~ r~e~.eG:.se as sa~own 1S ~elowm Chewing ~:~.z°c:e ~' Cafye~.ne 12f_~ easy 0 min --S xztixx S 6 my~ Ad.
20 miry 88 4 J m~ ~'i ~'7 Gezaeral~y,4 higl~:~ ~r water soLn~o~.e .rxgredier~ts are ahca~.~. 80-~Oa reieaseci aster oxz:3.y 20 five minutes of chewingt For caffeirer c~n.~y about S0~ is rn~_eased, ~rh~.le tie other S0o a.=.~a-~aix-xs i.aa tae gum after f~.ve ~.n~;4es c~f chewing. Afver 20 ~.:aru~.es almost 90~ of Gaffe-one :~s releasedm ~~~erz if c~.ffe:~.xze ~.s dissolved in hot wat.-e:~°
2S and mixed in the g°~-~e ~rhen the gam. iscool°d or ~c~~t o.t rooz'~a temperatures ca~:fe~.ne z~ay ret'u:~°r~. to it>~
~.~oxma~. cx~rstalline Mate End release a~. the san'ze rate as shorn abo~re.
Caffeine ~~alt ccazn~ou:~~.~.s suc~~ ~.s r~aff~:ine SO citrate, caffeine soa.iuxr~. ~enzoatei caffeine sodium salicylate, °~~laich ~.a.y ~rc~ rs~ors a~rater sc~~~.'~~a~.e anal less hitte~° than caffe~n~:g xnay° ~.3,so he encs.°y~scxlated or __.
entrapped for cont~=oiled relea.,ae in accordance with the present inventions Caffeine can be added to the°v~r;_ng gum as a poc,Tder, as an aqueous di::,pe_°s~.om~., ar dispersed ;~n glycer~in, propylene giyCOl, corn sy~vup, hydrogenated starch hydrol yzate, or any other compatible aqueous d_LSpersiorm For aqueous di.spersi.on°s, an emulsifier can also be m:i:~ed in the so~~.z~t~_or, -~;~.th the caff~~iv~e and the m~i.xture Iii added to a chewing gume ?1 flavor can also be added to the caff_eyne/emulsifier mixtuw:e. The emu~_sion formed can be added to chewing gum. fovlrdered caffes_ne may ~~_Lso he mixed into a molten ;nh=,~~_.ng gum base during base manufacture or prior to manufactur-.~~ of the gL.mm Caff~a_r~e may also be 15 mixed with base ingredients during base manufacture o ~S Sta'ed pre'vlOLl~i~i ~ ~:a~fel:'lE: r~"leaSeS slowly from c'zewing gum d.~aring l.~~e ear 1 y stags of mastication of the gum because o °~ it s lo~~= solubility in wa ter.. Physical modifications of v he caffeir_e by encapsulation wlv~h a 2~ highly water solu~~7_e substrate will irlcrea:7e ~_ts release in chewsng gum by increasing the solubility or ds.ssolution rate ef caffeine. w~ny =tandard technique Cahicln gi~res partial or full encapsulation of the caffeine can be usedo These techniques ;_rl~:lude, but are nct limited v~o, spray 2~ drying, spray ch i~_,~lngr f~~.uid-bed coati ng and coacerzration o These encapsulation tecrna_aues. may be used ind:~vidual_ly ~_n a single s tep process or _~.n a~:.y combinat~_o.n ?.n a multiple step processes The preferred technique for fasv~ release of caffeine is spray dryi_n.g a 3G Caffeine :nay also be encapsul ate~:l or entra:oped to give a delayed release from chewing gun. A slow, even release of caffeine car: give a reduced bit~._.~ernc~ss ovei=
long period of t_imc~ and blo-_n_d taore eas_l y ~.aith ~_onger lasting flavors and. sw~et~=ncrsa craffeen-~: nay be encapsulated wi th s;°=reetenersg speci.fical-1 y hicJh-intensity sweeteners such as ...
thaumatin, dihydreChalc<>ness acesulfame F~, aspartame:
sucralcse, alitame, saccharin and cyclamatese These can al so A.ave the effect of reducing bitterness o ~ddit.ior.a~_ S bitterness inhibitors can also be combined with cai~feine and sweeteners to give << reduced bitterness with delayed release caffeineo The encapsulation techniques described herein are standard coating tee'<:nic°2ues and generazll y give varying I~ degrees of coating ~yrom partial tc full coating, depending on the ccating composition used in tre process Generally, compositions that '_nave high organic solubility, good film-forming properties and low water solubility give better delayed re lease of caffoir~e, ~r'~~ile com;~osi bona ttzat have IS high water solub:ilv'~y give better fast r_olease a Such low ;water-solubility compositions include :acrylic ~~olyrt.ers and copolymers, carbc~ny~~inyl polymer, polyaAn.ides, polys t~rrene, polyvinyl acetate, pclyvinyl acetate phthalate, polyv_,_nylpyrrolidcr~:~ and waxes n Althou,h al 1 cf the~,e 2Q materials are possible for encapsulation of caffeine, or_ly food-grade materials shawl d be considc.r_ed. T~r~« standarc!
good-grade coatiZG materi.=~1 s that are -gcod f_lrn forrners but not water soluble are shellac and Zei_n_ Others which are more water soluh:'.ea, but good. film .forriers, are materials 25 like agar, al ginates, a rrride range of cellulosr~ derivatives like ethyl cellulos~:o rnethyi cei:LuloscF soc.~ium hydroxymethyl cellulose, and h°~droxypiopylmethyl cellulose, dextrin, gelatin, and modified starche:se These ingredients, which ~~re generality approved :~~or ~:ood use, may 3G give a fast release when used as an encapsulant for caffeine. Other enoapsulan'~s ~~.ike aca~~ia or maltodextrin can also encapsulate caffeine arid give a :East release rate of calfeine in gum The amount:. of coatinc; or encapsulating material 3~ on the caf:Eeine may also c:ontro 1 the lr=ngth of time for its release from chewier gun4.
- g -Generally, tile higher th,: le~fel of coating and 'the lo~rer the amount of acti;re ca ffeine, the slocaer the release during mastication with i_o~t yrat's== soluble corlpo.sitions.
S The release rate is generally not instantaneousr but.
gradual over an extended period of tune. To obtain tile delayed release to blend with a gum's flavor release; the erscapsulant should be a rui°nimur.~. of abom~:, 20 ~ of the coated caffeine. Preferably, the encapsul_ant should be a minimum of about 300 of the coated caffeine, and most preferably should be a minimum of about 40~ o.f. th~~ coated caf.f_eine.
Depending on the coating m~:ter:ial, a hz.gher or lower amount of coming material rnay be needed to give the desired release.
IS another :~:ethod oz. giving a modified release of caffeine is agglomerat~_on with an. agglomerating agent which partially coats the caffeine. This method includes tile step of mia:ing cafio_ne and an agglomerating agent with a small amount of irate,r or solve:'at. °~he mixture is ~>repar_ed in sue:: a h:ay as tG :aJe lndlV'ldual wc~t. particles :ii:
contact with each other so that a partLal coating can be applied. After tire ~.,rater or other solsrent is removed, the mixture is ground and used as ~ 'powdered, coated caffci_ne.
I~latGric~iS triut can be: ushd a:~ the aC(C'iOITIt-':Cdi~:l_nCx ~S agent arc the same as those used in. encapsL:lata.on mentioned previousl y. I-iowever, since the coa',~ing is onl y a partial encapsulat icn and ~°4~ffeine is not very water soluble, some agglomerating agents are more effective in increasing the caffeine's release than others. Some of the batter agglomerating agents for delayed release a:~e the organic polymers mike acrylic poll.-°mers and COpolyr(lers, poiy'Vi.nvl acetate, polyvinylp~,.=rrolidone, waxes,. ahellac ar..d ?ein.
Other agglomerating agents are not as c~WFecti_ve in g:i_ving a delayed release as are the polymers, coaxes;. shellac and ~5 Zein, but calf_ be used to give some delayed release. Gther agglomerating agents that give a fast :rel~ease include, but are not limited to, agar, a;~_gi~nate:~, a wide range oT caater soluble cellulose derivatives li?~e ethyl cellu7_ose, methyl cellulose, sodium hydroxymethyl cellulose, hydroxypropyl:~.ethyl cellulose, dextrin, gelatin, modified starches, and vegetable gums like guar gum, locust bean gum and carrageenan ~ Eve~a though. the agglomerated caffeine is only partial~~.y coated, when the quantity of coati:~g is increased compared to t=ae quantity of caffoine, IO the re' ease of caffeine can al.5o be modified f or mastication. mho level of coating used In the agglomerated product is a minimum of about 5~e Preferab:ly, the coating level is a minimum of_ about 1_5~ and more preferably about 2Go. Depending on the, agglomerating ageni:, a higher or 1S lower amount of agent marl be needed to give the desired .release of the caffeine.
Caffeir_e rnay be coated ir~ a two-v~tep process or a mu7_tiple step process. Caffei=-a may be encapsulated with any of the material's as descrix~ed previously anal then the 2U encapsulated caffeine can be a-gglo~.erated as pareviouv~ly described to obtain an encapsulated/agglomerated/caffeine product that could be used in chewing gun to give a delayed release of the caffeine.
~Cn a:~other_ embodiment of th:i.s ins; ention, caffeine 25 may be absorbed onto another component wsich is porous and become er_tr-apped in the ma,..rix of the porous Componento Coxrmon materials used for absorbing caffeine ir<cl ude, but are not limited to, silicas, sil_Lcatesr pharmasorb clay, sponge'_ike beads or microbeads, amorphous carbonates ana 3(3 hydroxides, including aluminum and calcium lakes, all of wrhich result in a delayed release of caffeine. Other water soluble mat erials including amorphous ~uga~rs such as spray-dried dextrose, sucrosef alditols and Tregetable gums and ether spray-dried materials result in ~ faster release of .~5 caffeine _ ~~'~ 98123~~5 .- ~~ ° ~'~'/~T59f11$977 Depending on the type of absorbent materials and hom it is prepared, t~.ze ~.~rno~xnt of ca.fie~ne t'_~at can be loaded on°~.o the e.:bsorbent ~ril.l vary. Generally raa~~er~.a~.s lice ~o'a.yme:rs o~°
spongel~.ke beads o~- microbeads, amorphoc~s s~zgars aa~s~
alditols arid amorphous carbonaires and h~ydrcxides absorb about 10~ to about ~CJ~ of the ~reic~rzt of th_e absorbent . Othea: materials 1~.;~e sxlic;as ar~c~
pharmasorb clays ~.~ay be able tr-,~ absorb about ,~c~~s to ~.0 about 80~ of the ~~,e~.g~ht of the. absorbe:r~t.
The genera's. proced~zre for absorbing caffeine onto the absorbent is as follovas. ~n absorbent like gur~ec.°~' sil ica po~,~der can bL zr:i xed in a po°~rder blender and ~.n aa-ueous ;solut~.on of caffe9_ne can be sprayed onto 4he~ powder as z~~.aca.:c~ag contir~:~aes .
The aaueous solution can be about '~ to ~a solids, and higher solid le~rels to ~.~-30~ may be used if -te:mperatures up to ~~aL are ~~sed. generally grater is the eoh,rent, but other so~.~rents like a~.cohol 20 could also be used :~a~ appro~red for use ix-~. foodm .~s the powder mixes, the ~.~.gt~i d is sprayed onto the potader . ~prayzrtg is stopped before the ~.~ix bec~ornes damp. Tne still free-f.lo~~i ng po~rder is renoved frozr~
the mincer and. dried to remove the ~:ater oi~ other 2~ so~.vert, end is t~yer~ ground to a specz~:i~ part:zcle size.
After_ t?~e caffeine is absorbed or fixed onto an absorbent, the fix..ative/caffe~.z'~e ca.n be coated by encapsulation. wither f~xll or part~.a~.
3~- encaps~alatic>n may be used, depe.nc3arag on gv~e ~oat~x~g coz~npos~.tion used i~a the process. ~~a.l~. encapsul~at~.or~.
rnay be obtained by coat.~.ng w~ai t~:~ a poly~:~e~r as ~.n spray drying, spray chi~..li~r.g~ fltaid-beck coating~
coace~ation, or any -other star..dard technique. A
35 partial. er~capsu~.ation or coating can be obtained by agglomeration o~r t~~e fixative ;caffeine mixture usi~ag.
any of the materia~.disco sed above.
~'~raother ~'o~rcz eu encapsuLatic~7:~ i s by .
entrapment of an i~g~°ed~.ert by fiber ext-rus~.on or °
- ! ~. _' fiber spinr~i_ng into a ~o~.ymera Polymers that can be used for extrusion are P~J~~, rydrcxypropyl cellulose polyet:nylene, arid other types of plastics polymers. T
process of erlcapsu~-alien by fiber oxtrv.:~sion is disclosed in U.S. PatenL ~~oa ~,~73,537, which is he:rcby incorporated by reference. The water insoluble polymer may be preblended with caffeine prior to fiber extrusion, or may be added avter the polymer ~..s melted. ~~s the e:rtrudate is extruded, IO it results in smalt_ fibers than are cooled arid ground.
This type of encapsulationlentrapmer~t generally gives a very long, delayed release of an active ingredient.
The four primary methods to obtain a modified release of caffeine are: (~ ) ez~.capsulation by spray drying, IS fluid-bed coating, spray chilling and coacervation to give full or partial en~.apsulation, (2~ agglomeration to give partial encaps~alat pony (:~) fixation or absorption ~~rhich also gives partial e~ncapsulati;~n, and (~; entrapment into an extruded compound. 'Pl:ese four methods, combined in any 20 usab:ie manner whicx= physically isolates caffeine and modifies its dissol;rability or modiTies the releas4~ of caffeine, <ire included in this invention, A method of isolating caffeine from ether chewing gum ingredients is to add caffeine to uhe dusting compound 25 of a chewing gum. ~-; rol.:Li ng or dusting compound rray be applied to the surface of chewing chum a;~s it is formed.
"'his rolling or dust.ir~g compound serves to reduce sticking of the chewing gum product to vvachinery° as it is formed and as it is wrapped, and sticking of the product to its 30 wrapper after it is carapped and is being stored.. The rolling compound comprises caffeine powder in comb~_nation with mannitol, sorbf_t~oif sacroso, starch, calcium carbonate, talr_~, otr_e-= orally ~icceptab ~_e substa.nce.s or a combination thereof. The rolling compound constitwces from 3~ about 0.250 to about 10°, but preferably about to to about 1 s) ~.
~° by daeight of the chewing gum compositeon. ~rhe amount of J O
caffeine powder ~.dded to the rolling compound is about O.OS~ to about 200 of the rolling compound or about 5 ppzn ~.o about 2000 ppm of the the>ai~g c~~m c:omposition . Th~_s method o~ using cap ~ei~-~e powder in the che~,Ping guzn allows for a lower usage level of caffeine, gives the caffeine a fast release rate, ~~educ.:as caffeine bitterness when used with sweeteners ar_d redLzces or eliminates any possibV.e I0 reaction of t_ne caffeine caith gum base,, flavor components, or other components, yielding improved shelf stability.
Another method of isolating caffeine is to use it in the coating/pann~ng of a pellet chewing gum. Pellet or ball gum is prepared as conventional chewing gum, brt I5 formed into pellets that are pillow shaped or into balls.
~'he p~llet:s/balls c~-~n 'hen be sucxar Coa~od or panned by conventional panniuct techniques to malce ~ unique sugar coated pellet gum. Cafi~elne is very st~ab~~_e bute not I_ighly >aater soluble and can be easily dispersed in a sugar 20 sol uti.on prepared ~lor sugar parming. Ca~:feiz~e can also ,be added as a powder blended with other po~hrders often used in some types of conve:~ teorlal pannirdg procedures . Using caffeine in a coating isolates it from other gum ingreds_ents and moc~dies its rel ease rate in chewing gum.
25 Levels of caffeine may bve abou'L 100 pprn (0 . 0.L° ; to about 25, 0C0 ppm (2.5° ) iz~ the coating ar_d about 50 ppm (0. 005° ) to about 10, 000 pp.n (1 ~; of the w~,~i.ght: of the c~~.ewin,~ gum product . fhe ~-aeig~t of the coating may be about 20 o to about 50 0 of the wewgha o=: the finishE;d gram product .
30 Conventional pae~ning procedures generally coat ~,.,rith suc.~~~ose, but ~~:ecent advances in parzrzing have allowed the use of other ca=bohydrate material's to be used ir_ the place Of silCrOSe. SOme C7~~: tllC:Se COmponen-ts in:~lude, but are not limited to; dextrose, maltose, palatinose, xylitol, 35 lacti tol , hydrogena:ed ~.somaltulose and other new aldito 1 s or a combination thereof. These materials may be blended with panning modifiers including, :out not l~_mited toq gum arabic, maltodextrins, corn syrup, gelatin, cellulose type materials like carboxymethyl cellulose ac hydro~;ymethyl cellulose, starch and modified starches vegetable gums like alginates, loC~~.~>- bean. gum., guar c~umF and gum tragacanth, insolub~.e carbonates like calcium ca.rbo:nate or magnesium carbonate and ta~~c. Antitack: agents rnay a7_so be added as panning modifiers which allow for 'the use of a variety of carbohydrates arid sugar alco~iols in i::he development of new pa~~ned or coated gum products. Ilavors may also be added. with tie sugar coating and wit: c~~ffeine to yield unique product characteristics.
IS Another type of pan coating would also isolate caffeine frorn the cn~wing gum ~_ngredieats. This technique is referred to as film coat~_ng and is more corr~rnon in pharmaceuticals than in chewing gum, but procedures are similar. A film like shellac, Zero, or cellulose-type material is applied onto a pellet-type product form~_ng a.
thin film on the surface of the product. The film is applied by mi.x.i_n.g t°ne polymer, a p1 ast:Lciz~~_ and a solvent (pigments are o~..wional ) and spraying t:~ve mixture onto the pellet surface. ihi s i.s done :in conver~~tion.al type panning 2S equipment, or in more ad.wanced side-ver~.t~d coating pans .
Tv~'hen a solvent 1 ike al cool is usod, eVt:ra precautions are needed to prevent fires and explosions, and spec~saJ_ized equipment must be u;.;ed.
Some film polyi~ners can use water as the solvent in film coating. he cent ad~rances ~.r~ polymer researcrs and in film coating technology eliminates the problem aJsoc_i.<_;t~ed ;.with LIi~L u:;e of flammable solvents in coaLinc_ These adz-ances crake it possibJ_e to apply aqueous films to a pellet or chewing gum product. Although. caffeine is not 3~ nighi.y water soluble, it may be added ~!o this aqueous film - l4 -solution and applied with the filrn to tie pellet or chewing gum product. The agueous film, or ever the alcohol solvent fl lm, in which caffe~:~ne ~.'~s dispersed mail also cc;ntain a flavor along ~frit~~. th~~ po~~~ymer and piast.=~ci zc~r.
The prey=;.o~.~sly desCr_.bed er~ca.~~su ~_ated, agglomerated or absorbed caffeine may readily bF
incorporated into a chewing gum composition. 'a"~~e remainder of, the chewing gum ingredients are none:ritical to the l0 present invention. What is, the <.oatec~i particles of caffei ne can be inco~:~crated into convents_ona~'~ chews ng gum for:mul~{tior~s in a conventional manner. Coated r_affoine may be used in a sugar c~ieGaing gum or a sugarless Chewing gum.
The coated r_affeine may be- used. in ei than regular checaing ~S gum or bubble gum.
Tn general; a chewing garn con:auos_it:ion typically comprises a water-so:Luble bulk ~~.,o:rtion, a water-insoluble chewable gum base port=on and typically water-insoluble flavoring agents. T~:e water-soluble portion dissipates 20 with a portion of the flavoring agent over a period of time during chewing. T.~e gum base i~o.rtion is retairaed in the mouth throughout t'.de crew.
The insolu~~le gum base general l y comprises elastomers, resins, fats and o~.lsr waxes, softeners and 2S inorganic fillers. ~lastorners may include polyisobutylene, isobutylene-isoprene copolymer and styrene butadiene rubber; as well as natural latexes such as chlc.le. Resins include polyvinylaceva~e armd te.rpene resins. Fats ar_r.~ owls may also be included in the gum baser including tal~_ow, 30 hydrogenated and partial7_y hydrogenated vegetable oils, and cocoa butter. Commonly employed waxes include paraffin, mlc.rocrystalli:.e and natural waxes such as -beeswax and carnauba. According to the preferred e:mbodimenwt of tho present invention, the insoluble gum base constitutes 3S betiaeex about 5 o and about 95 o by weight of tk~e gu,°rao r3ore p-~eferabaly the insoluble gum base comprises bet~reen about 1o% and about ~t~ o by Freight o.~ the gum, and ?~osv preferably h~:~_~teen about COs and a:~ou~. 3~~ by a~e~.ghv o.f the guru.
The guru b~.se ~.yp~~.ca~~.y a'1 so :~nc~.x~des a filler component. ".~."he ~=i:~~.er coznp~ner~t umay be ~~alcium carbonate, ~~~a.g~.es~.~.~m carbonate, talc, dicalcii:m phosphate or the like. The filler may cons t ~ tote be t~ree~~. about 5 %' and about 6 ~ ~s by ~reaght 20 of the gum base.. ~:~~efe~~ab~.y, the filler compra..ses about 5 o to about. 5~~~ by ~?eigh~: of the guru bass:.
Gum bases typ~ca.l~.y G0.lso oo~.ta~.n softeners, includa.ng glyceYal monostearate and glycerol triacetaveo further, guru bases rc~ay also conta~.n optional °ing~°e~°~ze:a~a such as ant~o~cidar~ta, celor;~, and ezn~zlsi.fm~~ers v ~'he present ~7..n~Yer:~tior;~
contemplates employ:{ng any comn-cerc~ally ac~;epta.ble gum base.
The taater--soluble portion of the chewing 20 gum may further co~rz~orise softeners, s~reeteners, flavoring agents and combinations heweof.
Sof te~:ers are added to ~:,he c'her~ing gum :gin c;rder to optima~ze the cheV~ab~.l~.ty and rlo~zth feel ~f the gum.
Softeners, also ~~~o..~jn ~::~. ~.:.he art as pl<~.s~..zc:izex~s or ?5 plasticmzx~~g agents; generally constitF"te ?~et~aeen about 0 a ~~ and abouw 1~ a by Freight of tl~e che~airig gum. Softeners con~emr~lated by the present ~.n~rention include g'myce~y~.r:i, a.eci.th~.xa a.nd corc~i~.atzons thereo:~~ . 'w'u~~°ther y ac~u.eon.:~ wweeter~.er 30 solution) such as t~~.ose ccant~~.ming sorb~.to_a, hydrogenated starch hydrolyxates, corn. syrup and combinations thereof may be used as softeners and binding agents in g-'~n.
~s mentio..eaed ~,bo~re, the coat.e.d caffeine of 3~ ~.he present invention zn~.y be used ~n s~~.ge.r or sugarless gum fo~°su~wations . Sugar s~reeteners generally include sacoharlde-containing components corrcmo:~ly ~noin t~~e chewing gum art ~h~.c~.
comer ~ se, but are nr~,t limy te_d to, :sucrose, dextrose, ° a'~'~ )8/r3~~ej ._ ~.~ - g'~'~''/"sW ~u13.~'~ iT
~.ai~ose8 dextrinF d°wied invert s~xgare f:r-~.~tose, levulose, galactoseco:~a~ syrup solids and the like, alone or in aa~y comination. sugarless sv~eeterae~°
~? nclude componenvs Y~9i~.h sweetening ch;~.xact~~ris~,ics but which are de~roa.d of the cor~only kTZO~n sugars alld CoILl~~l.s~,, bud a=?T'u. nC.e~. ~ .7~yTt~.ted to, cal.5.gi~~.' c~~.~:o~'1C'_i.
such as soxbitolg ~nannitoE., <~'~a~to~., h.~:drogenated starch h~-dxol~rzatesg ma~~.~.~to~ and the l..~fce~ ~.~one ox . ; n a:~~ oombination . , - 1~ ~ Depending on the particular o.affe~.ne .
release pa~o~W~.e and s:~ze:Lf~-s~.ab~.~.~.c~r nf~.~a~aded, ~.he coated caffeine of the pxesent ~.n~rent~.on ca:a also be used in combination w~.tS. ~ncoated h~.g~A-~potenc~
sweeteners or wi~~~ ~-~igh-potency s~,reec~:~~ews coat"ed .3.5 with other materials and by other techniquesa Z-1 v.~a~o~°~.xzg age~~t ~na~r a~.so :gym present. ~r~
the chewing gwm in an axraourat ~a.~.hin tzve range ~sf prom abo~:c~. a m ~.~ ~.o ~bou~ ~_~% , prefe~°a~~~.~r f:~or~ a~bo~.~:~.
. 5 o to s.bout~ 3 0 : b ~y k~re~.gi~t o ~ the gu.:°r~. ~'lae lav-oy°ing ae~ents ~ria.~ corr!!pr.~.se essent~.a~. oi~.s, synthetic flavors,, ox :m~.~.~urew thereof: i~acaudi~.ag, but not limited ~.o oils deri°~ed from plants and ~xuyts s~xcr~ as c~~.x~~.s oils, -~:~~a.it essences, peppex~znnan~, oil, speermint oil; clove oil, oil of 25 sadintergreen, anis;_:, and ta~.e like. Art:if ~ cabals .~la°~orinc-~ components are ~.~.so cont2a~tp~..ated for use in gt::~s of the present in~.ren;:ion. Those spilled in she art ~:~1~. recogn:~~.ze that n~aura~. a:~.~d arti~.a.~.ia~.
flavc.xing agents z~.a~r be combined i?~ and ser~sorall~ .
30 acceptable blend. ~~.1. ;such flavors and, flavor blends are cos~templa°ced b;~~ the: present: ~.n.°~ent~.on.
Optional ingredients such as colorsp emuls~.fa.exs arid pha:~aceuta.ca 1 agents mad be acLded to t:he chewing gums. .
3~ rn genex°a:;t, cheRFring gum is ~~mn~fact~.~°ed bar sequentza~,l~T adding t-~.e ~z-ar~c~u.:~ chewz:~-~g gu:ca~
ingrec3ierWs to a coarcmexciall~ a~,rai°! ab~.e ~W:.~cer knock.
in the art. ~lfte~~° ~~.he ingredien°~s ha~~e peen tho~-oughl~r mixed, the g°~a mass ~.s~ discharged from .~ s.::~ ~,yn.au.y I l ci~le mixer and shaped ~r~~:o the ~.es~red. ~or~r such as ~~r rolling in~.c~ she~~.s :=zand cu~.'~.ing a~n~.~ s~.,:~..c:~s,, extx-uding in~r~ ch~,~s~s or c°as~~.~.~.g in tca ~:~e~'~lets m ~e~.e~°al l~ ~ the :~ngr ~:d'l e~.~s ~~ ~°e ~axe~. hy~
first melting t:ne gbase and ~.d.d~.ng ~.~. ~~ ~.~°~g~
rur~nir~g mixer. '~'~.e l~~s~: 5~ay c~ls~ ~e ~.e7 ced ~n the mixer itself. ~o:~cr or er~ulsa.fiers m~~~ ~.~.;~o be added ac this ~~.r~.e . ?~. ss~~ ~ener such as g~.y~cer:~n ~~n~~
c11 sO l'3e added ~.~ i:.?"s:l..s ~m._II''~e,~ ~.~.~Tl~' '4d'~~~"i u~'r~.a~
czIld c'~.
~0 portion o~ t:.he bu°? king :~gen ~ o _~'~.r~her pcart.ion<a o~
~~e a~ulkix~~g agent as?~y L:he~~ be ~.c~ded tc: ~~te Ix~ixer. Z~
fla~ror~.ng ~.ge~.t is ti~.~.lw~ bedded vri~mh ~.he ~ilaal portion o~ the bulking ~.ge~tm ~°he ccawec~ r~a~~c~a:ne of the present inc~enta.ol~ :~.s ~~°e~erabl~r added a..°rter ~ 5 the ~in~..1 portzc~n o~ bu~_ltil~zg ~ge~t. and ~l a~ror h~.~re been added.
'I'he entire ~rri:~4ir~g procedure t~,~y~ica'? l~~
cakes from ~i~re to z_i~tee~? rnirs~:.tes,. bc~;~ ~l.ol~?ger anixing cirnes rr~y sc~~ecz~.es be ~°e~.irec~.. ~.~:'~~se 20 skilled ice. the art ~7ii.l :~'eoagxli~e tha~~ r.n~
~rariations of the a~c~~re c~.es~r~_:~ed proGed~.re ar~~~ be cal 1 c'~ed a '~'xa~~~es ~'he ~ca~? lr~~r~.I7.g e~ar~p~.es of t~~e. in~ence~.on and comg~arac.i~e e:~~:~ple,s :ire ~~rc~~i.dec~. ~'~y ~~~ c~
expls.r~ation and a.11 ~sL.rs.t:~.c~.. _ she ~.c~°~~z:~as ~.~~.ated in ~'~.bl~~ :~ comprise ~rara.ows sugar ~or~~n.p~las ° ;~ ~rhich c~.ze~e_-~~~e can be added co gum ~.~ter t a..s d.issc~l~red ih -~arius ~.c~~a.ec~as cape scyl~e.n is .
_ ~8 _ ~rs~E z ~xaxay~.e Bxp~. Bxamgle Bx~nttp~_ q~xample ;~~.xainple J L
Sugar G3..9 ~~ ~ 9 G0. 3 G0. E3 G0.,,3 53 .3 Gun Bale 19 . 2 19 a 3 19 2 w9 . ~$ ~9 A :2 ~.9 . 2 Gl~~ex~.r~ 3_ . ~ ~ . a~. 0 m J 0 . 0 0 . C 1. .
Corn ~,5 ..~ 1.5 . 9 ~.2 ., 9 ~.2 0 =3 ~.~ . a SYp ~ec~_~P~ira 0 . 2 d ~ 0 .2 0 . ~ ~ 0 . ~, 0 . 7 Feppera~An t 0.9 0.9 C.9 0.9 0.9 0.9 Flavor Lic~.lid/
Cageine $ blind O.S C.0 G.0 G.tJ G.Cv 20.0 Example y . and 2 -~ Caffeine por,~rder can be added directly to the gum.
Example ~ w A " 0 . 0 gram portion of caffeine car.
be dissolved in 90.0 grams of hot water, -r,aking a 10.0 2~3 solution, and added to gum.
Example 4 -- A 5.0 gram portion of caffeine can be dissol;red in 95.0 grams of hot propylene glycol, making a S.Oo solu tion, and added to guru.
Example 5 ~- ~1 ~ . Cl gra.m portion of caf:Ceine can be 25 dissol,~ed in 95.0 gr:~m of llOt glycerin, making <~ 5.0 solution, and added to g~~,~m.
Example 6 - t~ %.5 gram portion of caffeine can be dissolved in hot earn syrup, making a 2.5~ solution, and added to gum.
3G Tn the next examples of a sugar gum formulation, caffeine can be di.solved ~.~n hc>t water and emulsifiers can be added tc the aqueous soa_ution. Example sclucions can be prepared by dlSSO~'~T.lng 10 crams of caf_~eine in 90 grams hot water and adding 5 grams o:L emulsifiers o:~ ~ra.rious 35 hydrop~z,il ~.c-lipophi.lic balance ~~iL~} val.ues to tie $~~' ~'~5'i~:iia1"3 _ ~ ~ _ d't~~IW~~Uiiio:l l l solution. The mixtures can then be used in the fol~.a~lxng forrz;uls.s a ~:~~~ 2 ;:ar~. ~~
~~ampl ~xamp~. ~~~:e ~mpl ~xar~;pl ~~carxpl a a ~ ~: ~: a 7 $ 9 10 11 12 St.~gar 50.7 50.7 50.~ 5tJ.7 50.7' Sfl >
gage 19.2 x.3.2 19.2 ' 19.2 29.2 19.2 Cozxa Syrup 12 . 9 1 ~ . 9 12 . 12 . 9 - 12 . 12 ~) 9 .
g G? ycerir_ 1. ~ ~ . ~ 1. ~ _ 1. ~ 1. 4 1.
~
Dextrose ~Sonohydrate 9.9 S.9 9.9 9.9 9.9 9.9 Peppermint 0.9 0.9 0.9 0.9 0.9 0.9 F? avor Caffaine/
emulsifier =hater 5.0 5.0 5.fl 5.0 5.0 5.0 2diacture Hone ~L~=2 a~=~ HZ~a6 HLB=9 H~-12 ~YaTri~J~.eS ~ - a'~3.e saIT:eta'le ~rJr!1t1~atltJl7.s 1~ ~ aS
made in examples - L~ , res~aect~.vely, except that the '?
flavor c ap b~ m~xec:~ togevher ts~e ~~.queoyas ~r:Ltlz caffeine soiutian a_~~d err~uls~.~zedbefore:.> ng r~he a~.da.
mixture to the batcbz. .
gum Catfea.~aecarp a:Lso be ersdec intovarious bl base ing red1ea~ts A ty ~.'1 cal formula as . base ?s f ollo~:s 'tft .
Polyv~.r~~%e~. acetate ~'7 ~ynthetlc rubber Paraffin ~~ax 13 2 t~ ~'a~. ~
~lyceral ~ianos=rearate Terpene ~Zes~.r C:alciu:~ ~arbo~.;~te ~ a.~t_ler ~:~a,~;~ ~s;~~~~s ~ ~~ w ~3~~r~~~~n~~~rr sof toned ~r~or to ~.I~eir s~d~.~.~:~on in ~.~~e base ~nt~fac~~ring pr,:,~cess ~ To ~h.~~ preso~~a:.ened ba0.~e corr~ponen~~ caffe~..ne ca~~ be added ar~.d mixed.g a~~d ~~Ler~
the presoftened base/c~.fiei no .b_Lend can be adcLed to r:vake the finished base o 1~~ the folio=~~i~~g exa~~p3.es a caffeine can be ~n~~ed fvrst v~y~.~h one ~~:~ the base ingredients o and 'r_r~.e mixed ~.zz~~redient~ can ~~~.e~:~ ~be used in ~aka.ng a b:~se. '~~ze i~~.grediej~.z..s b:-~e~.de:d ~~a.ti~
caffeine car 'chef. ~e used at vhe le°~re:ls i~°sdxcatLd :gin the typical base vcu~.a above ~xa:aple ~.9 - Tire te°~°pene re:,:~~.m;.sec~ to make the base is ~3°~ pc;l~r~erpene resin a~.~. ~m z5 caffeine.
example :2C - ~'he pc~.y~y°i~?~~. :~_ce~.a.te ~ESecs~o make the base is X80 1~.;~a~ ~.Y~q poly~ri~.~°1 acweta~:e and 2~s caffeineo ~xarn.ple ~~ _ Tne paraffin ~,~r~.x used ~:o ~~a~~e ~0 the base is 96% paraff~.n z~ax arid ~o c:affe~.n.em ~affe~.a~e zt~ay aa.so be added ~_o are ot~:~er~aV~_se complete c~L~Tn base.
~°xamp? a '%~ ~ U ~, 5 o caffei?7.e can be xnx.xed Sri th 99 > ~ o of a ~;a~.~ base ha-~ina t~.e ~.:~.~o~re listed ~5 typical foranula. °~he ~.a~:feir~.e can be: added ~~~ar L~'e end of t~se process after al ~. ~~he other ingreda_ents aLa addedm _.
The sara~p:Les of finwshed -base jade ~:a.t~a caffeine added t~o ,~~ fferent k~ase co~r~.~onents cG.n tl~er~
be e~raluated in =.W ;~uga~ -r.ype che~ir:g ~~;c &worm~:~late;~
as fr~l~o~s m ~~'~ 98?23Io~ _ ~~ _ ~/v~iS961~~~~i :~~LJ' 3 ~, s:
~; ~~, m For e~~.~ri~'~e~ ~~3 ~L~. ~~. ai:~
Stx~ar ~ ~ a 2 ba:~~ 1~ o ~ a ~c~r~~ ~~x4a~
~~~r~~.ex:i.r3 3. m 67 ea~~ ros ~
_ 15 ~ir.~~cal2~rd~ate ~ ~ ~
~ep~ermi~.~.
~'~wa~Or. ~9 ~ ~
2G ~.~3~a ~'~7.~ ~~c~,~O."_'er~..Cc?J.
~.e~.r~. O~ Cc'~.w~'~T'de La? ~1'1G
f 1.Y"11S'I1~C gL2I:1 1.S ~
m ~' n a ~Sl.Tlg a:.~'1~ fo~.~.~~93.T1~$ff~~2"11Lt1.c'~.'s,:.~..C3~7 of a i~..~C~cr 25 or sugar-free gu:-n, a ~rari~~t~c~f er~ca~~u~.ai.eci C a ~ f a 3.32 ~ S aFt1''~7 cl'C Er' ~ ~:
~ 2.~-~ C ~:? T3 ~ E? ~'t.~"a ~ 'L7 22. -''F,.FLE
~
yWt.
a) ~.uc~arFree Su a=w Sorbitol X8.8 --Sugar - 54 a -' viannitol 8 r -G;.am Base ~ 25 ~ 20 3 ~
~:~
Glyceri?: 8 . I .
5 . ~
I0 Corn Syrup - 12..0 Lycasin brand. 6.~
riydrogenated Starch Hydr olyzates Dextrcse - 10.0 Mono:~ydra to Peppermint ~. . ~ 0 . 9 ~0 T'1 a V~Or Active Caffeine 1.00 1.C)u for spray dryings the solids :'.evel of an aaueous or alcoholic solution can be about 5-30~, but preferred levels are indicated in the examples 1_sted.
Example 23 - An 80o s:~ellac, 20o active caffeine 3C~ pcwder mixture is ob~~ainecl by spray drying an alcoho~w~/sheilac/caffeine solution at to~.a:~ solids of i0~a Example 2C - A 50~ s~ellacp 50o active caffevne powder mixture is ob::.aimd by spray dry-~ng an appropriate ratio of alcohol/she:~_lac~'caffe ~..ne solu.tio_r~ at 10 o solids .
Example 25 - A ?00 ~e:in~ 30o active caffeine po~ader mixture is obva:inec.-~ by spray dry.ng an alcohol/~ein/caffeine solution at 10~ solids.
Example 26 - A 4u shzel lac, 60 ~ active ca-vfeine w 23 _ powde r mixture is abv~aincd by fluid-ber. coating caffeine with an alcohol/shellac so=~.ution at 3C° solids..
Example ~7 -- A 5G% shellac, 40o active caffeine powder m~_xt~?re is attained by fluid-bed coating caffeine with an alcohol /shellac seiutian at 3C'~ solids .
Example 23 - A ~a0 0 ~ei_rl, ~0 ~ active caffeine pcwder mixture is a~wcained. by j~luid-beca coating caf:f:eine ~J with an alcohol/Zein solution at 25° s~~li ds a ~~,xample 2~f - An 85° wax, 15 o active caffeine powder mixture is attained by spray chilling a mixture of molten wax and caffeinea Example 30 - A 7~~% wax, 30~ active caffeine po:ader mixture is obtained by spray cl~.~lling ~;. mixture of molten wax and caffeineo IJxamp 1 a 31 - r., 70 ~ Zein, 30° act5_ve caffe:~re povrder mi xture is c~ tain.ed by spray drying a hot aqueous mixture of caffeine and rein d~.spe~rsed in an acueous, high-~0 pI-I (pI-I of 1i . 6-12 . C ) media at IO o solids n Example 32 - F~ 20=~ 2ein, 80 ~ active caffeine powder mixture is abtairmd by _flu~_d-bed' coating caofeine with an aqueous, hih-pI-i (pI~I=1.1..6-12.0; 7e~.n d:i.spersion of 10~ solids.
2~ Example 33 - A 20 ~ ZE.in, 20 o she3.lac, 60 o active caffeine powder mixture is obtained by spray drying an alcohol/shellaa/caf~~eine mixture and t~~.er: fluid-bed coating the spray dried product for a second coating of alcohol and Zeino ~0 Examples G3 ,~c 33 wou f d all ~yi~;e neayv ~, coreplete encapsulation and would delay t:he release of caffeine when u:~ed in the sugar ow: sug;..~rless g;_~.n fo~.~zE;u"~atvon~> in 'Table !! o Tie :~ighe.r levels o~.' coat~.ng would give a lorge:r delayed release of caffeine than. the lower levels of casting..
3~
- ?4 Other polymers that are inore water soluble and used in coating wo~!~~c', have a faster rel<Wa:~e of ~l:he caffeine.
Example :~ ~ - An 80 o g~latin, 20 o acti-c~e caffeine powder mixture is obtained by spray drying a hoL
c~elaLir:/caf Lei_ne ::~o~_~.~;ticri at 'G ~ solids Example 35 - A 3Uo hydroxypropylrnethyl cellulose (HPMC; , 70 o caffeine po~,ader mixture is obta_i.ned by fluid-bed coati ng caffeine wit~i an aqueous solution ov IFMC at 10 s 1C solids .
E~>arnple 30 - A 50 o maltedextr-r, 50 ~ active caffeine powder mi;~tare i.s obt~,.;.ned by spray drying a not aqueous solution of caffeine and maltodextrin at 3J=~ solids.
hxampie 3 7 - A ~!0=, gum ar~~bic; ~0 ~ aci~ive caf feine powder mixture is obtained by fluid-bed coating caffeine with an aqueous sol.u~~ian of gum arabic at 30 o solids .
The coated caffe~.ne from Examples 34 and 35, when used in t'ne chewing gum formulas in Tab~Le 4, wo~zld give fast release of Gaff=nine. The product coated ~.~ith 2~ maltcdextrin and gum ara~.>is in a.xa.mples 36 ancd :37, when u;~ed in the guru. formulas in 'fable ~, would s':ow very fast .release of caffeine in c'ne~~.i.mg g~:m compared to c:a~cf~:ine added directly.
Caffeine could also be used in gwm as an agglomerated caffeine to give fast or delayed caffeine release. Agglomerated caf:~eino can be prepared as in the following examplesv ;;xample 3~3 -- A l.'3 o hydrcxyprop~jlmethy:l cellulose (HPMC} , 85° active c:~ffei.ne poEP.'der mixture is prepared by 3t} agglomerating caffeine a~L:d ~IL~i~C blended together, with water being added, and the res~~:lting :product being dried and ground.
Exarvple 39 -- A I5 ~ g~~~.atin, 85 o actlvE~ caffeine:
powder mixture is made b~~ agglomerating caffeine and gelatin blended together, ~~~i~uh water be ing added, and the. resulting product being dried and ground.
~'~~ ~~123kG5 _ ~z~ _ 3'~:'~IUB~GI~~~'~7 oaf~ei ne powder rc°axture ie a~.ade by agg:~omerating ~aaff2~Tle wl~y'~. ~."~,.~. ca.~.fi'OilC~.i. :aC7.~5.g~':~..C~2w ~C7~.~:~?.,~'a.Z.:~lg ~&~m Fein,_ and drying arid grinding the re~~.~.ta.ng product Ex~.mple ~~. - ~ :~~~ shellac, 8~~ ~ act~.~~e caffeine powder m~.xc.ure i~ made by agga.o~.eratiF~g _ oa~feine w~.t:~ an ~~~..coha~ uo:j~~:ior cor~raY.~~~.ag shellac, and d~.yi~!g ar_d g:~ir.d~_ng t~.e r~.~s~~~.~:zr~J
product>
0 .' Example ~-~ - r-~ :~0 a ~~~MC~ 80~'s ~.c.t:iv'e caffQine powder mixture is obtained by agglomerateng asp H~~C and ca~fe~ A a ~n~.~~~.~.re ~~~.ended togethe~g wxt~~
water being added and the resulting.product being dx°1ed a~~3 gro~r~da °15 EXamnle ~~ - ~ 70~s 'Jeing 80~ actxtre eaffeir.e po~~rder. rcn~a~xre ~.;~ ca"~~:.airze~I bv~ aGrgl orne:~at~.:~g caffeine and Zeirl ~.ys~o~'.~~~ed irl hicrh~-p~=~ ~~b~ater ~.1v5--12 0 0 ) at 15-°s solids g vrzF~h the rest~ltirzg ~rod~ac:t~
~e~_ng dra.ed arid g:cc~~cnd 20 Example ~~ - ~_ :~0 ~ waxF 80~ acti~re coffee he powder m~.~d~a~a.re ~ ~ obt~air~ed ~a~~ ~.gg~.ome:~at~.s~g caffeine and molten wax,, and cooling and grinding ~.he resulting prad~:.c~t Example ~~ - ~ ~S a m~a~.todextrin, 85 25 ac~.i~re caffeine pc~~~der miact~~°a is obt<~.i~:ed Ly agglorr~erating a b~e~~.d c~~ caffeine amd ~r!altoc~ex~.rir.s then adda.rg «ater~ d~pz~~,~ aid c~r~.ndi~ar~~
Za.~.l of r~e abo~Ye a~i~wtu~°es can ~e added to any of the follocalr~g t~.es of ohewing gmn foula~ a '~°~3~~.~
Se,r.r~arSu.c~-ar~esS:xf4r3es ~~i~a s s ~ S~a~arles Su ~~- Sc~rbitc~ly7i~l~. 4~ath s tdater L~;casinNo ~4acer Cum Base Ig .s I ~ .2 . ~~5 .5 :5 . ~5 .5 l Suc~ar 55.~ ~ :,:~.0 ..,.~ __ .._ 1~ Sorbitol _.. ~.0 5Z_E3 ~~.~ 5x..~
itol _- ~- $.0 8.0 ~.'~.0 Corxa Syrup L3 _ I :~ . M _ _ _ _ _ :~ ~.
x~ycasin/
5orbitol .
I~.quiti. _ ~ a . 5 ~a.7,mss _ _ . ~
~by Glycerin 1.a- _d.~ 1.5 ~.S ~.5 Lecithir~ __ ~_ 0.2 0_2 ~.2 l~e~trone P~oncahydr ate 9 ~ ._ ~ w _ _ w ~ _ ~ _ ~
Flavor o.5 0.~ 1.5 I.5 I.5 ?Q Level. of .~ot~.ve Caffeine Owv X3.5 ~..t~ ~.0 :! .G
~
~c3~ ~.lC~tIIL'~ SOrb:i?~.ol~ .IQ's' uOY'.J~.~O~,, .~ ~
&' 4Pu.'t~E.-'r~
!k~3 hydrogenated ;staroa x:y~.rolyza~e syrtap If each of t'_ne exa~T~p ~.es of agglomerated material (8-45) were evaluated in t_he formulations shown in Table 5r some samples would rive ~~:affeirze a dela°~,~ed release and others a fast :release. Sa~npl.es using ae=LnY waxJ and sheJ_1 ac 3~ wculd yield the slowest release rate w:~ereas s~amplcs with HF~iC and gelatin. would y~_eld the next slowest rel ease.
I'~altodextrin ~~aould ive a rya: t release compared to c;ao seine added directly to t:~~~ cu:n.
Partially% coated or gully~ ceatPd caffeine can also be used in sugar t~,%pe gum formulations containing ether sugars, such as in the fol ;~_owi~~g v~ormul.aticns A-Go ,_ f _.
'~ ~s~
('6~~. . ,y 3 Cum 3a8e ?9.z 19. ~ ~.9.'? .~9.y>~9.2 x.9.2 1J.2 Sugar 5~.5 4"-~.r ~ ~L~.S 4:9.5 a~.S 53..5 ~~.5 G lyc~. riot ~ . 4 ~. . ~. ~, . ~ ~. . ~ W . g: 1.
~ > a.~ ~
Cozn ~.9.Q . 2:3.~ ~.9.c7 23.0 ~~.0 ~.6.G
~9.~J
Syrup ~7~x~rose a_ _- 5~(~ __ __ __ _..
~3C~~6~ _ _ - m .. .. _ .. m, a ~ _ .. _ Fruc~.c~se __ _m ' S.D _~ __ ..- __ Invert _- __ __ ~p p __ __ __ Sugar T~':~.~.~os~ ~_ __ .._ __ '__ ",~.p __ Pala~iraose _ - - _ _ _ _ . _ _ ~, Com Syrup __ 5ora __ _. __ __ __ So~.ids Pepp~zminv Fla~ror ~.9 0." ~.9 ~..p ~.9 tt.:3 0>9 z~eve 1 of ~c~a.ve 1. 0 ~. . ?3 1 . U ~...'~ . 0 ~. . ~~ 7.
i's . 0 Calf eizze Thane foT-anulat? ans also cont~.ain sugax may alcohol-s such as so~:b~ tol, zzar~n~ to~~F
.~rlitol, Z~.Ct~CO~., 2Tlc.,.~....t~.t0~., ~t.~"~'C:7l:i!c'7.~..~'.'.X~..~~~, 5~."1~C~~~C~1"'sc%la~~.:~.a..~l~.
~y~Gl.Jr~r~ ~~~~~~"~.5.....~.oi~.~ .:J~.~a~..~~.~~..~''..~'J
o~ F'~'...ro'srle~e~~. r ~o~'IF11~.ZC'3.t~oTlm'".7 V,t~.th ~3aLt~.~..t.~.'~~
~,..oatE~.'~.
o~ ~f.~~.~~
G'oat'EC~.
caffeine can a:~s~ be ~ac~e using ~ra~iou:~
sugar a~cohc~ls, such as the follo~~T:~r~r~fcarniulat:~o~~~s ~i-~v 2 ~; _ ~~~Il~': 'i rT ' J ~. I; ~~ tai U h ~, ~~3.f-S~ 2J.J~ ~~.aJLS.~ ~.J.~ ~ ZS.$J X5.5~7~J..~J~~i i.~J
Sorbi~ol 53.C ~ 46.C~~:0 ~~..C ~~~C 4.? 3~.C:37.C ~~~.C
.,C
Sorbi~o~ ...
:Liquid/ ~ 1 ~ C~~ S
C~
1 1~.C~.C m- ,eC _.. -- e ~
7.C ..
Cc.'i~a i83 ' ' ~ a~
l~aa~rti~03. -- ~O.C~3.C)S.0 ~.C f3..C S.C f~.0 E.C
1'a..sayts.~0~. .._ __ 5 0 _.. -.. S __ .._ ~_ 0 Xy-~. i ~ 02 ~ _ ~.5 :~. _ .. 5 ~. _ - u- . C ~ .. a 5 m Cl > 0 .
G C
~a~~i~oi a- __ __ _.. z~.o __. ...___ __ Hydrogenated- _ ..- _ -... - ~5 :LO _ _ _ _ _ . ~ _ i.~ C
somaltulose .
.~
_ Glycerin 2.C 2.~,~?.C7 8.C 8.0 n.~ 3.C 6.0 -__ Fl~~ror z.s ~. i.5 1.5 ~..5 ~..~ z.5 1.5 -~.5 Le~re. of .~c t i v~
1.C? 1.~ ._.0 ~..0 :~.~tl.Ca ? 1.0 ~.0 ~3'F~~'11'1.2 ,.0 ta) L~;rca~in, a? e~~.~orst.sse :~ivo~lic~tx~.C~
1 so~
All of these formu.lairio.ns in Table 6 and ''able 7 which "use vhe agglomerated caf.~=eine as described in th«
~5 examples (38-45) and ,n the p._rc~~rious encapsulated examples (23,-35 j would be a<pected tc g ~~re a de.l_a~red. rel easof caffeine or a fast release o_'~ caffeine compared to a product made by adding caffeine c~irect~! y to gmtl as a r~owder.
Nlul tiple step agglom~~ratien/'e:ncapsulat~_on 3(~ procedures can also be u~.~~ed. :in making :re'.ease mcdifzed caffeine 'nor use ~ n ~,.he ,~or~~~ulations i:n 'I'a~les 5~ 6 and 7 .
Lxamples of mul tiple step tr_eai~ments a:r:e here describede example ~6 - Caffeinr~ 1s spray dzied with maltodextrin at 3C~ solids to prepare ~.~ ~ovder. This poCader 3~ is then agglomerates: with a "-~y'ar_oxypro:~>ylmethyl se 1 lulose (r-:~-EMC) i.z~ a rati o -:~f 85/:x.5 pc~wc~er/~aPMC~ wetved w~.th watef - 2~ -and dried. After gr:~nding th.e rosinting powder wi 11 contain about 68o active caf:Ceine, 17o maltodextrin and 15% HPMC.
Exa:rple ~7 - Caffeine is agg?_omerated grit h HpMC in a ratio of 85/15 ca-_'!eino/z-IP1~1C. After drying and grinding, the resul~~ing powder is il~~id-bed coated ~rit:l~ an alcchol/s hellac solution a~~ .about 25° solids to give a f~_nal produc ~ contas_n f ng aaout 60 ~ ac;tive oaf feine, 10 o HPMC; and about 30 o si~ellac.
E:>ample C~8 - Caifein~: is agglomerated wits H~MC in a ratio of 85/15 cafveine/h~l~~lCe After drying and grinding, the resulting powder is agglomerated with a 15« solids, hi gh-p.-I, aqueous solution of Z~:irs to g:i.sre ~: f:i_na~_ product containing about 6C o active caf:fei ne, ~ 0 a HPMC, and 30 IS Zero.
Example 49 - Cafveine: is spray dried with a 25 solution of gelatin . ~'he spray dried ~_roduct is tl~~:~n agglomerated w9_th a 7_5 o solidsp hi g1u-pII, aqueous solution of Zeino The final product wile r.:ontain about 50~ active caffeine, 20o gelatin, and 30~ Zein.
Example 50 - Caffe ins: is .aggl.omerated witi~ molten wax in a ratio of 85/15 caffeine/wax. Lvrhen the: rnixture cools and is ground, it a.s fyu~_d-bed coated with a 25 ~ 2ein - 75o alcohol solution, diving a final product containing 60% active caffeiney 10o wax az~.d 30° Zein.
These examples 4e~-50~- when used in zany of the formulations noted in Tables 5, 6, and 7 above, give caffeine ~ delayed re.7_easeu These mulv:iple step procedures can actually give more delayed release than t:~.<~ single step processes . L~Iultiple step processes of mor a than two s reps may give even longer delayed release tines, but may ercnerG-~.ly beco.ne less cosy effecvive ar_cless efficient.
Pref erably, spray drying c~~n be=_ the -fi:rst step with additional steps of fl,~id-'sued coating, spray r_hill.ing and agglomeration being part of the latter steps.
_. ~C _ Log absorption type examples, ti'ae delayed release rate of caffeine is dependent or, the type otabsorbi3ig material. Most material s 1i k~s silicas, s~.li_cates, Cc~.~lulcse, carbonates, and hyarw~xide:~ we>uTd be expected to g~_ve a more delayed ,elease than amorphous sugar and sugar alcohols. Some examples:
)Jxample 51_ - A hot TO % solution o1= caffei n~~ is 0 sprayed ontc a preci~:;iLatoc~~ silica to al:~:~or~: the caffeine.
The mixture is dried and ground. The final product is about 50% active caffeine.
example 52 - A hot 10% solution i:: sprayed onto a pharmasorb clay cafft:>ine. The mixture .is d.~=ied and ground and gives a final product of about ~0% clay and 20% active caffeine.
l~~xample 5~ -- A :LO=o solution of cavfc;ine is sprayed onto a microcrysta?_~~a_ne cellulcse powde>-. 'fhe mixture is dried and ground and gives a product that is about ?0%
m~_o.rocrystalline cel__~ulose and 30 ~ acti.ve c<~ffei_ne o Example 5 ~' - l~ 10 % so~luti on c~f caa~feine =~s sprayed onto a high absorption starch. The :ri~:t~:re is dried and ground and gives a product that is about b0'~ starch and 200 active caffeine.
iJ::ample 55 - :~1 lu'o sclut ion c>f ca:Cfeine _~s ~:pra yed onto a calcium carbomace powder. ~'he mixture is dried and ground and gives a p~~oduct of about ~0% caladium carbonate aryd 10% active caffe_~_ne.
Example 56 - A hov' 10 % soluti.or~ oi. caf:Ce~~:,:c is sprayed onto a highiz,r absorptive dextrose material., The mixture is dried a-r~d ground and. gives a praduet of about 80%
dextro:ae and 20° act:~:~cro caffeine.
Exaz~~;ple ~7 - A hot 1C % solution o2. caffeime is sprayed onto a sorbi;~ol powder to absorb the material. The mixture is dried a:~;:l ground and. gives a product of about 90%
-- 3:!
sorbitol anal l o o active ~;affea.E~e a The samples prepared in exam~~}les 51-57 can be used in gum formulations as noted i n fables 50 6~ a~~d 7 a i'hose preparations which have caffeine absor'.~:eci onto a m~ L.ere_~al teat is not water soluble are expected to give a delayed release and those that are water solub.~_e are expected tc give fast releasem ~0 Another r~~odification or absox-pt~ion technique is to dry the caffeine tog-ethe_~ ~rita~ a sL?c~ar or sugars alcohol, or resolidify the caf feine with sugar or ~;uga.r alcoho~~ when mixed together in a molten sta~'~ea E.~ample 5C - affeine is added to molten sorbitol ~5 in a ratio of 9C parts SOrb~to;~ to 10 part,, caffeineo After mi~:ir~g, the blend is cooled and groundu Example 59 - Caiffei.nE~ is added L. c: molten den>trose in a rat,~io of 90 parts dextrose to t 0 parts: caffeine a After mixing, the b1_end icooled and ground., Example CC; - 4"~ caffeine i.s dissc>lved in 96 ~ r:igh fructose corn syrup Th.e ns_d>t~~.re is e~~~apo~~ated to a low moisture and groundp The product of e~:amples 50-6C; may be added to the gum formulations shown is Tables 5, 6 and 7m 25 zany of t~_e examples listed are v,ing-le step processes ~ I-Iowover, more deli°-~red release c:f the caff~a Lne may be obtained by combir~ir:~; t~~e various px-ocesses of encapsulation, agglomeration absorption, a.r~d entrap_mento Any of the preparations made i~~7 examples 51.-6G can be 3Q further 'treated in fluid--bed coating, spray chilling, or coacervat-~on processes to encarJsulate the ~~roduct, and can be ~agc~=_omerated S~rii~I~: vari o~:s rn~teri_a.ls and proceduretv in a varisty of multiple step prccesses~
3~
- .~~
The caffe~.r~.e carp a~.:~o be used with a variety of high intensity sweeteners and blended together before encapsulat~.c~~A, agglo~~erat:i.on, absorption, and e~°~trap~clent ~ '~'h.is car:1 redt.zce bitterness assoc:~~.ted ~adyth eawfeine. Soinsw examp l es area Example off. ~ Caffea~~xe and ~.~par~:ame are blended together ii a ~/~. ratso ~.s a ~o~~ad.c,ro This mixtyare is then sp:=ay chilled with wax in a ratio of ? 0 60/4 mixture/wax ~~o obtain a powder c~:on~.~lining 40ro caffeinep 20% aspartaz-~e; and ~~0% wax ~xa%~tp..~.C~ t~.G -' ~c3.f ~E.'~_Ze1~..' and t~3~.L1.1T2c1tJ.n In a ~/1 ratio are ci~.ss~:~lve~. an. water ~a°ith a ~.Cn solution of gelatin anal spray driedm This spray d~°i ed ;oowd.er is then agglomerated ~rzth a ha.ghrpF~ a~.r-;ueou.s ~5-°s Zeir solutions The m~.x~:ure is dried and ground, and gives a product containing ~U~ caffe.ir~e, ~.0~ tha.umatin, 35% gelatin, anC ~~;o ~eina Exampae.~~:~ ~ :'~'affei~l~.e and: a~.itam.e i~~s a '7/'2 :2U ratio are prepared iZ:s r."~. hot ~....F~% ~olut:i.~Xiw Thi ~
solution is sprayec4 onto a high absor~~ti on sil.xca powders The n~ixtzz~ae is dri ed , ground s.nd f~ui d~bed coated with an a~.cc~holjshellac~ mixtures gi~ring a product that conta~_ns 35% caffeine, 5p alitame, 400 ~5 s~.l~.ca, and 20 o sne~.? acs Example ~4 °- Caffeirbe and soda.r...amm cyclamate in a :i/~: ratio are b? ended to~~et~aex~ a~~ a p~~~rder arid then agglomerated ~~.tn ~patex .~:nd h.ydro~~.~~aropylmethyl cellulose (HPMC) ~ This ~alend is dr~.eLi~ ground and 50 agglomerated further ~rith a high-pH, a~"~eo~.~s l5%
solution of Zein to obtain a product con ta:~r_ir_g 3~
sodium cyclamate, :34o caffeine, ~..~% H~~~G and ~0%
G~ein o Example ~:~ - c~'affe r~.e and gaLy~cyrn:h~.~in in 35 a ~.r~ ratio are b~r;~a:xded togc~.t.er a~ a 7o~~idE:~° aid f~.axid-bed coated ~~~.~~h a so:~u.t~.oz~ of 25=~ shellac. ~.r~
alcohol o The coated product a s agg~..oz~.creted further with water ar_cl hydroxypropyl methyl ce F °! u? ose (HP1~C) to obtain a product containing 30a caffeineT 300 glycyrrhi~in, 25° shellac, and 15o HPMC:b Example ~6 - Caffeine and sodium saccharin in a ratio of ~_/1 are bl.e,.~ded toget~-.er as a powder and fluid-bed coated with a solution of 35° s'nE:llac in alcohol. '=I'he coated product is agglomerated further faith water and hydraxypropylmethy~_ ~:~el lulose ( ~3PMC) to obtai n a product containing 30o caffeine, 30% sodium saccharine ~5o shellac, l0 and f 5 0 ~IPMC a If the b1_~:nds of caf~:eine and. other high-int:en:~ity sweeteners of examples 61-~6 are tested in gum formulations such as those note! in T-abler ~ , 5, 6 ~~nd 7, a significant delayed release of t::~e sweetener arad reduced caffeine bitt=erness G.:ould be expected ~ This de ~ eyed release would irnp~Yo~e tree qualit~r. of flavor A The fcllowi :ng are exarnpl es of fiber extruded PVr.~C/caffeine blends to give a delayed eel ease of caffeinr~ and give reduced b_i.tterness:
Example ~7 - Methurr~ riolecular weight PVAC and caffeirAe at a ratio of 3i'1 are blended together as a poiader and extruded. The fibers are cooled arid ground to c.~ive a product containing 75~ PV!~C and 25~ caffeine.
Example ~8 - Mt~d~.'~ura r~~oleCUlao weight PVAC, caffeine and aspartame at a ratio of 12/~ll are blended together as a powder and extruded , the= resulting fibers are ground and give a product containing ?0~ PVAC, 24o caffeine and 6~ aspartamea Example 59 - M~>dium molecular weight PVACp caffeine, aspartame, and sodium gluconate at a ratio of 16/4/4/1 are blended together ~,.s a po~~~der and extrud.ed~ 'she fibers are ground and gizres a product containing 64~ PVAC, .L6°~ caffei no, 16'-o sodiur g~lucc>r~ate, and ~ ~ aspartan~te.
Sodium gluvanate is ~, bitter:~ess inhibitor than can be mixed wit: caffeine before beinc, encapsula ted or entrapped. This bitterness inhibitor <~lor~g with other.
bitterness inhibitors sac.h as sodium salts of chloride,.
... 3 ,~ _ ascorbic acid, glutamic acid arad citric acid, as well as other Various organic cempoundes, can b~4 add.ed to catffeine to reduce bitterness.
Example 70 - A 20o hot aqueous solution of maltodextr_in is mixed with a. 4 0 ~ hot sc>luti.on of sodiL:m g.7_uconate. Two liters of this mixture is cc}mbined ~a:~_th 100 grams of caffeine, dispersed a~~d spray dried. A final product containing 50% maltodextrin, 35~ sc7diam gluconate i0 and 17a caffeine is obtas_n.edm Example 71 - A 2400 ml quantity of a 25=,, hot aaueous solution a:C mal todextr_in is m~_xed ~~ith 50 c~~-~a~rs of aspartame to form a suspension. To this i~~ added a r_ot aqueous solution of 400 grams =~f sodium gluconate, 200 grams I~ of caffeine, 1200 grams of hot water. This rW xture is spray dried to obtain a pcwder containing ~8a, mal.todextrin, 32%
c scdium gluconate, 16~ caffeine and ~° aspartame.
E~>ample '72 - '~'o a 24 ~0 gram c~uant:ity of a 25 ~ hot solution of maltodexarin, 200 ~-grams of citl_ic acid and 50 20 g=~ams of aspartame care added and suspended To th.~.s ~T:ixture is added a hot aaueous solution of X100 grams of sodium gluconate, 200 grams of caff~-we and 1200 grams of hot water. This mixturE. is spray buried to obtain a powder containing 41~ malvode~:trin, 20° sodium gluccnate, ~~_9°
25 caffeine, 1~% citric. acid and 3o aspartame.
The abova e~~amples are made t.o o~>tain not only a fast release of caf f eine ii> dr wing gur,~, based on maltodextrin encapsulation, but also to obtain fast -release of a sweetener and ~~i'~ter_r~.ess inhibito_~s to counteract ~0 bitter effects of caffeine.
Iv should be appreci::~ted that th~~ m.ethods and compas:itions ov the present invention are capable of being incorporated in the form of a variety of embodiments, only a feq~.j of. which have been i.llustr_:~ted and described above. The 35 ir:vention may be emk::ods_ed in other forms w~.thout departing from its spirit or essen tial cr=aracteristic:s . It ~ ~~ _ a..~:
~~c~ 9~ia~ie~ .~.,~~,a~" , , xvzll be apprec7 ate. t~-zat the a~,dit~.o~ o~ some other i:rzgred~er~ts, process steps, z.t:eri~.l~ ~~~ ~.o~~pcar;er~~.s nod spec~~ica~.~~ ir~c~.~.ded ~~.il~. saa~~e an ad~re~°se ~.~p~.ct on the prese~.~: ~.n~~e~t.~.or~m ~°he ~~est ::node o~
the ~n~rent.~.ora ~a~ ~:here~ore c:~.c~~.ude inc~:~edi~:~.t.sy process steps r ma~er.ia~.s or c:or~~porzerzts ot~~er than those Lisped ai~o~re for i~.c~.~s~.o~? or ~se~ ~.r. tire a.~.~rera.tion~ ~~o~ae~ery t.:ne c~:escrioec~ ea~cmd:~~te~at.s are to be cons~.dered i~ a~.l ~ respects o~z~~ a.s i~.l~stra~~.ve and not ~°es~r:~c~~.~re ~ aid t~~.e scope ~~
the in~er~tio~ i.s, ~~.ere~ore, ~.r~d~.cat.ed b~ the appended c~.aaxns r~.t.~e~° than ~S~ tae .fore:goi x~g descriptionm ~1~. charges ;~h~.ch come ~ri.~.h~.n the meaning- a~zd rar~~e of ec~tai valerzcry o~ the, claims are ~5 to be embraced ~aythi n t.beir scope
dextrose, fructose, maitod~o~xtrin or other built sweeteners, as wel 1 as sugar a ~ cohols suet: as sorbitol, rn~~amitol, xylitol, maititol, lactitol, hydrogenated iscrnaltulose and hydrogenated star e: hydrolyzates.
Lricr to encapsulation, caffeine may be combined with high-intensity SweP4e'':er_s,. including b~.r not limited to thaumatin, aSpartalTte, aiI_taIPe, aCesul°ame ~~, .SaCCi:aryn aCld and its salts, glycyr_Nhizin, cyclamate. and its salts, stevioside and dihydrochalcone:s . Co-cncap:~ulaL~_on of caffeine along U;it.~ a high-:int:.ensity swe_=etener may reduce the bitterness or caffe__ne and cor~.tro:L the sweetener rel ease with caffeine. Tr:is can improcre the quality of the gum product and increa se consumer aocept.abiW~_ity.
In addition to use of high-intensity sweetenersr S bitterness inhibitors such as sodium gluccnate, sodium ascorbate c.r other soc gum salts may be combineca wi. ~h caffeine prior to encapsu?atien to reduce the cverall bitterness caused b~T caffeine 2nd-resul~~ in a gum product having s_ncreased co:~sume.~ acceptability.
DFTA:CI~ED D~'SCR1PTI0'~t OF T~aE PREFFRRrD ;_,M30DIVE~:~TS
Caffeine :~ s a natural chemic~;1 fcund i.n a variety of food prcdwcts such as coffee, tea; cocoa, c1-~_ocolate, and various other beveraf.ges .. Caffeia~e is known as an effective.
I5 stimulant to increas~ energy and reduce drowsi=ness.
Caffeine has a naturally bitter taste. The bitterness, however, a~.:tually ir;~proves the flavor percepticn o~- some beverages such as coffee and carbonated be~,.eraces~
G~hen caffeine is added to chewing gum at a level cf about 0.2% to about ~o, caffeine imparts an int~snse bitterness to the chewing gum that lasts t~nroucrhout the chewing peri od. "'he higher the level used the: stronger the bitterness. At about 0.2~, which is about 5 mg per 2.7 gram stick, the bi tterness is below the =~.lmeshold lir:?~_t and 2~ is not readily di.s c;~,~.rn.~bl~~ . Taste lim°.~ts u_n chewing gum.
are generally about C.4~ (?0 mg) to about ~o (200 mg) of caffeine in a stick of gum. 'r~~e o0-80 mg lezTel of caffeine is about the level of cafLeine found in a comrent~_onal cup ey coffee. The ta_r_get level cf caffev.ne in stv_ck gum is about ~0 mg per sticky with a _r_ange of about 25-60 mg, so that a five stick package of gum would contair< about 200 mg of caffeine, or the equivalent of cafl:o ine i.r_ two strong cups of coffee. However, at this levE;1 caffei~~e bitterness cver~,Thelms the f~.a~ror in. itial 1y and lasts throughout the chewing period.
~~~~ 9b1231bS - S _ ~'~~J'd~~9b11~~77 ~$it.h t~Ae caffeine release x~~od~.f:i.e~. ~.o ~'esust in a fast release of caffeine '~~a~.t~.'2 t~~.e chewing gum solu~? es ar.,d sweeter~ers, the bitterness can be effeci~.ive:l~' reducec.._ vief high.-~~~tex2s~.t~P
sweeteners car ~e ~:lended with caffeine to release a t~~"re ~allle ~~.TTlea ir~:!ws ~c;3C3 Carl redL7.C~v-: 4~.,~'lE' hi~~;E.'~'%"~eS~
effecv. Ot:~e~' che:~~~~.ca:Ls that irrxhibi~° i~it.teLn~as r~tx~%
be b1 ended with caffeine Lo al so ~°ed.uce ~aitterness.
Caffeine is r~~s~ a h~.gh~.y waFaer so~.~~~~le '~ 0 substance and, therefore9 has a znoderate~.y slow re~.ease froze ch.ewia~.g gum. Caffeine iv 2 . L°s soluk~le 1Y1 ~ w c'~'d~.e?" at room ~~..'TL1'',r7era~4.T;Iane r ~S~ So~g l~b:~~~ : 3.n 'W'a.te~
at 80°C and 40o sol~le in boiling water. this gives caffei_le a r~.c~de~ate~ y s.l.o~~ r~e~.eG:.se as sa~own 1S ~elowm Chewing ~:~.z°c:e ~' Cafye~.ne 12f_~ easy 0 min --S xztixx S 6 my~ Ad.
20 miry 88 4 J m~ ~'i ~'7 Gezaeral~y,4 higl~:~ ~r water soLn~o~.e .rxgredier~ts are ahca~.~. 80-~Oa reieaseci aster oxz:3.y 20 five minutes of chewingt For caffeirer c~n.~y about S0~ is rn~_eased, ~rh~.le tie other S0o a.=.~a-~aix-xs i.aa tae gum after f~.ve ~.n~;4es c~f chewing. Afver 20 ~.:aru~.es almost 90~ of Gaffe-one :~s releasedm ~~~erz if c~.ffe:~.xze ~.s dissolved in hot wat.-e:~°
2S and mixed in the g°~-~e ~rhen the gam. iscool°d or ~c~~t o.t rooz'~a temperatures ca~:fe~.ne z~ay ret'u:~°r~. to it>~
~.~oxma~. cx~rstalline Mate End release a~. the san'ze rate as shorn abo~re.
Caffeine ~~alt ccazn~ou:~~.~.s suc~~ ~.s r~aff~:ine SO citrate, caffeine soa.iuxr~. ~enzoatei caffeine sodium salicylate, °~~laich ~.a.y ~rc~ rs~ors a~rater sc~~~.'~~a~.e anal less hitte~° than caffe~n~:g xnay° ~.3,so he encs.°y~scxlated or __.
entrapped for cont~=oiled relea.,ae in accordance with the present inventions Caffeine can be added to the°v~r;_ng gum as a poc,Tder, as an aqueous di::,pe_°s~.om~., ar dispersed ;~n glycer~in, propylene giyCOl, corn sy~vup, hydrogenated starch hydrol yzate, or any other compatible aqueous d_LSpersiorm For aqueous di.spersi.on°s, an emulsifier can also be m:i:~ed in the so~~.z~t~_or, -~;~.th the caff~~iv~e and the m~i.xture Iii added to a chewing gume ?1 flavor can also be added to the caff_eyne/emulsifier mixtuw:e. The emu~_sion formed can be added to chewing gum. fovlrdered caffes_ne may ~~_Lso he mixed into a molten ;nh=,~~_.ng gum base during base manufacture or prior to manufactur-.~~ of the gL.mm Caff~a_r~e may also be 15 mixed with base ingredients during base manufacture o ~S Sta'ed pre'vlOLl~i~i ~ ~:a~fel:'lE: r~"leaSeS slowly from c'zewing gum d.~aring l.~~e ear 1 y stags of mastication of the gum because o °~ it s lo~~= solubility in wa ter.. Physical modifications of v he caffeir_e by encapsulation wlv~h a 2~ highly water solu~~7_e substrate will irlcrea:7e ~_ts release in chewsng gum by increasing the solubility or ds.ssolution rate ef caffeine. w~ny =tandard technique Cahicln gi~res partial or full encapsulation of the caffeine can be usedo These techniques ;_rl~:lude, but are nct limited v~o, spray 2~ drying, spray ch i~_,~lngr f~~.uid-bed coati ng and coacerzration o These encapsulation tecrna_aues. may be used ind:~vidual_ly ~_n a single s tep process or _~.n a~:.y combinat~_o.n ?.n a multiple step processes The preferred technique for fasv~ release of caffeine is spray dryi_n.g a 3G Caffeine :nay also be encapsul ate~:l or entra:oped to give a delayed release from chewing gun. A slow, even release of caffeine car: give a reduced bit~._.~ernc~ss ovei=
long period of t_imc~ and blo-_n_d taore eas_l y ~.aith ~_onger lasting flavors and. sw~et~=ncrsa craffeen-~: nay be encapsulated wi th s;°=reetenersg speci.fical-1 y hicJh-intensity sweeteners such as ...
thaumatin, dihydreChalc<>ness acesulfame F~, aspartame:
sucralcse, alitame, saccharin and cyclamatese These can al so A.ave the effect of reducing bitterness o ~ddit.ior.a~_ S bitterness inhibitors can also be combined with cai~feine and sweeteners to give << reduced bitterness with delayed release caffeineo The encapsulation techniques described herein are standard coating tee'<:nic°2ues and generazll y give varying I~ degrees of coating ~yrom partial tc full coating, depending on the ccating composition used in tre process Generally, compositions that '_nave high organic solubility, good film-forming properties and low water solubility give better delayed re lease of caffoir~e, ~r'~~ile com;~osi bona ttzat have IS high water solub:ilv'~y give better fast r_olease a Such low ;water-solubility compositions include :acrylic ~~olyrt.ers and copolymers, carbc~ny~~inyl polymer, polyaAn.ides, polys t~rrene, polyvinyl acetate, pclyvinyl acetate phthalate, polyv_,_nylpyrrolidcr~:~ and waxes n Althou,h al 1 cf the~,e 2Q materials are possible for encapsulation of caffeine, or_ly food-grade materials shawl d be considc.r_ed. T~r~« standarc!
good-grade coatiZG materi.=~1 s that are -gcod f_lrn forrners but not water soluble are shellac and Zei_n_ Others which are more water soluh:'.ea, but good. film .forriers, are materials 25 like agar, al ginates, a rrride range of cellulosr~ derivatives like ethyl cellulos~:o rnethyi cei:LuloscF soc.~ium hydroxymethyl cellulose, and h°~droxypiopylmethyl cellulose, dextrin, gelatin, and modified starche:se These ingredients, which ~~re generality approved :~~or ~:ood use, may 3G give a fast release when used as an encapsulant for caffeine. Other enoapsulan'~s ~~.ike aca~~ia or maltodextrin can also encapsulate caffeine arid give a :East release rate of calfeine in gum The amount:. of coatinc; or encapsulating material 3~ on the caf:Eeine may also c:ontro 1 the lr=ngth of time for its release from chewier gun4.
- g -Generally, tile higher th,: le~fel of coating and 'the lo~rer the amount of acti;re ca ffeine, the slocaer the release during mastication with i_o~t yrat's== soluble corlpo.sitions.
S The release rate is generally not instantaneousr but.
gradual over an extended period of tune. To obtain tile delayed release to blend with a gum's flavor release; the erscapsulant should be a rui°nimur.~. of abom~:, 20 ~ of the coated caffeine. Preferably, the encapsul_ant should be a minimum of about 300 of the coated caffeine, and most preferably should be a minimum of about 40~ o.f. th~~ coated caf.f_eine.
Depending on the coating m~:ter:ial, a hz.gher or lower amount of coming material rnay be needed to give the desired release.
IS another :~:ethod oz. giving a modified release of caffeine is agglomerat~_on with an. agglomerating agent which partially coats the caffeine. This method includes tile step of mia:ing cafio_ne and an agglomerating agent with a small amount of irate,r or solve:'at. °~he mixture is ~>repar_ed in sue:: a h:ay as tG :aJe lndlV'ldual wc~t. particles :ii:
contact with each other so that a partLal coating can be applied. After tire ~.,rater or other solsrent is removed, the mixture is ground and used as ~ 'powdered, coated caffci_ne.
I~latGric~iS triut can be: ushd a:~ the aC(C'iOITIt-':Cdi~:l_nCx ~S agent arc the same as those used in. encapsL:lata.on mentioned previousl y. I-iowever, since the coa',~ing is onl y a partial encapsulat icn and ~°4~ffeine is not very water soluble, some agglomerating agents are more effective in increasing the caffeine's release than others. Some of the batter agglomerating agents for delayed release a:~e the organic polymers mike acrylic poll.-°mers and COpolyr(lers, poiy'Vi.nvl acetate, polyvinylp~,.=rrolidone, waxes,. ahellac ar..d ?ein.
Other agglomerating agents are not as c~WFecti_ve in g:i_ving a delayed release as are the polymers, coaxes;. shellac and ~5 Zein, but calf_ be used to give some delayed release. Gther agglomerating agents that give a fast :rel~ease include, but are not limited to, agar, a;~_gi~nate:~, a wide range oT caater soluble cellulose derivatives li?~e ethyl cellu7_ose, methyl cellulose, sodium hydroxymethyl cellulose, hydroxypropyl:~.ethyl cellulose, dextrin, gelatin, modified starches, and vegetable gums like guar gum, locust bean gum and carrageenan ~ Eve~a though. the agglomerated caffeine is only partial~~.y coated, when the quantity of coati:~g is increased compared to t=ae quantity of caffoine, IO the re' ease of caffeine can al.5o be modified f or mastication. mho level of coating used In the agglomerated product is a minimum of about 5~e Preferab:ly, the coating level is a minimum of_ about 1_5~ and more preferably about 2Go. Depending on the, agglomerating ageni:, a higher or 1S lower amount of agent marl be needed to give the desired .release of the caffeine.
Caffeir_e rnay be coated ir~ a two-v~tep process or a mu7_tiple step process. Caffei=-a may be encapsulated with any of the material's as descrix~ed previously anal then the 2U encapsulated caffeine can be a-gglo~.erated as pareviouv~ly described to obtain an encapsulated/agglomerated/caffeine product that could be used in chewing gun to give a delayed release of the caffeine.
~Cn a:~other_ embodiment of th:i.s ins; ention, caffeine 25 may be absorbed onto another component wsich is porous and become er_tr-apped in the ma,..rix of the porous Componento Coxrmon materials used for absorbing caffeine ir<cl ude, but are not limited to, silicas, sil_Lcatesr pharmasorb clay, sponge'_ike beads or microbeads, amorphous carbonates ana 3(3 hydroxides, including aluminum and calcium lakes, all of wrhich result in a delayed release of caffeine. Other water soluble mat erials including amorphous ~uga~rs such as spray-dried dextrose, sucrosef alditols and Tregetable gums and ether spray-dried materials result in ~ faster release of .~5 caffeine _ ~~'~ 98123~~5 .- ~~ ° ~'~'/~T59f11$977 Depending on the type of absorbent materials and hom it is prepared, t~.ze ~.~rno~xnt of ca.fie~ne t'_~at can be loaded on°~.o the e.:bsorbent ~ril.l vary. Generally raa~~er~.a~.s lice ~o'a.yme:rs o~°
spongel~.ke beads o~- microbeads, amorphoc~s s~zgars aa~s~
alditols arid amorphous carbonaires and h~ydrcxides absorb about 10~ to about ~CJ~ of the ~reic~rzt of th_e absorbent . Othea: materials 1~.;~e sxlic;as ar~c~
pharmasorb clays ~.~ay be able tr-,~ absorb about ,~c~~s to ~.0 about 80~ of the ~~,e~.g~ht of the. absorbe:r~t.
The genera's. proced~zre for absorbing caffeine onto the absorbent is as follovas. ~n absorbent like gur~ec.°~' sil ica po~,~der can bL zr:i xed in a po°~rder blender and ~.n aa-ueous ;solut~.on of caffe9_ne can be sprayed onto 4he~ powder as z~~.aca.:c~ag contir~:~aes .
The aaueous solution can be about '~ to ~a solids, and higher solid le~rels to ~.~-30~ may be used if -te:mperatures up to ~~aL are ~~sed. generally grater is the eoh,rent, but other so~.~rents like a~.cohol 20 could also be used :~a~ appro~red for use ix-~. foodm .~s the powder mixes, the ~.~.gt~i d is sprayed onto the potader . ~prayzrtg is stopped before the ~.~ix bec~ornes damp. Tne still free-f.lo~~i ng po~rder is renoved frozr~
the mincer and. dried to remove the ~:ater oi~ other 2~ so~.vert, end is t~yer~ ground to a specz~:i~ part:zcle size.
After_ t?~e caffeine is absorbed or fixed onto an absorbent, the fix..ative/caffe~.z'~e ca.n be coated by encapsulation. wither f~xll or part~.a~.
3~- encaps~alatic>n may be used, depe.nc3arag on gv~e ~oat~x~g coz~npos~.tion used i~a the process. ~~a.l~. encapsul~at~.or~.
rnay be obtained by coat.~.ng w~ai t~:~ a poly~:~e~r as ~.n spray drying, spray chi~..li~r.g~ fltaid-beck coating~
coace~ation, or any -other star..dard technique. A
35 partial. er~capsu~.ation or coating can be obtained by agglomeration o~r t~~e fixative ;caffeine mixture usi~ag.
any of the materia~.disco sed above.
~'~raother ~'o~rcz eu encapsuLatic~7:~ i s by .
entrapment of an i~g~°ed~.ert by fiber ext-rus~.on or °
- ! ~. _' fiber spinr~i_ng into a ~o~.ymera Polymers that can be used for extrusion are P~J~~, rydrcxypropyl cellulose polyet:nylene, arid other types of plastics polymers. T
process of erlcapsu~-alien by fiber oxtrv.:~sion is disclosed in U.S. PatenL ~~oa ~,~73,537, which is he:rcby incorporated by reference. The water insoluble polymer may be preblended with caffeine prior to fiber extrusion, or may be added avter the polymer ~..s melted. ~~s the e:rtrudate is extruded, IO it results in smalt_ fibers than are cooled arid ground.
This type of encapsulationlentrapmer~t generally gives a very long, delayed release of an active ingredient.
The four primary methods to obtain a modified release of caffeine are: (~ ) ez~.capsulation by spray drying, IS fluid-bed coating, spray chilling and coacervation to give full or partial en~.apsulation, (2~ agglomeration to give partial encaps~alat pony (:~) fixation or absorption ~~rhich also gives partial e~ncapsulati;~n, and (~; entrapment into an extruded compound. 'Pl:ese four methods, combined in any 20 usab:ie manner whicx= physically isolates caffeine and modifies its dissol;rability or modiTies the releas4~ of caffeine, <ire included in this invention, A method of isolating caffeine from ether chewing gum ingredients is to add caffeine to uhe dusting compound 25 of a chewing gum. ~-; rol.:Li ng or dusting compound rray be applied to the surface of chewing chum a;~s it is formed.
"'his rolling or dust.ir~g compound serves to reduce sticking of the chewing gum product to vvachinery° as it is formed and as it is wrapped, and sticking of the product to its 30 wrapper after it is carapped and is being stored.. The rolling compound comprises caffeine powder in comb~_nation with mannitol, sorbf_t~oif sacroso, starch, calcium carbonate, talr_~, otr_e-= orally ~icceptab ~_e substa.nce.s or a combination thereof. The rolling compound constitwces from 3~ about 0.250 to about 10°, but preferably about to to about 1 s) ~.
~° by daeight of the chewing gum compositeon. ~rhe amount of J O
caffeine powder ~.dded to the rolling compound is about O.OS~ to about 200 of the rolling compound or about 5 ppzn ~.o about 2000 ppm of the the>ai~g c~~m c:omposition . Th~_s method o~ using cap ~ei~-~e powder in the che~,Ping guzn allows for a lower usage level of caffeine, gives the caffeine a fast release rate, ~~educ.:as caffeine bitterness when used with sweeteners ar_d redLzces or eliminates any possibV.e I0 reaction of t_ne caffeine caith gum base,, flavor components, or other components, yielding improved shelf stability.
Another method of isolating caffeine is to use it in the coating/pann~ng of a pellet chewing gum. Pellet or ball gum is prepared as conventional chewing gum, brt I5 formed into pellets that are pillow shaped or into balls.
~'he p~llet:s/balls c~-~n 'hen be sucxar Coa~od or panned by conventional panniuct techniques to malce ~ unique sugar coated pellet gum. Cafi~elne is very st~ab~~_e bute not I_ighly >aater soluble and can be easily dispersed in a sugar 20 sol uti.on prepared ~lor sugar parming. Ca~:feiz~e can also ,be added as a powder blended with other po~hrders often used in some types of conve:~ teorlal pannirdg procedures . Using caffeine in a coating isolates it from other gum ingreds_ents and moc~dies its rel ease rate in chewing gum.
25 Levels of caffeine may bve abou'L 100 pprn (0 . 0.L° ; to about 25, 0C0 ppm (2.5° ) iz~ the coating ar_d about 50 ppm (0. 005° ) to about 10, 000 pp.n (1 ~; of the w~,~i.ght: of the c~~.ewin,~ gum product . fhe ~-aeig~t of the coating may be about 20 o to about 50 0 of the wewgha o=: the finishE;d gram product .
30 Conventional pae~ning procedures generally coat ~,.,rith suc.~~~ose, but ~~:ecent advances in parzrzing have allowed the use of other ca=bohydrate material's to be used ir_ the place Of silCrOSe. SOme C7~~: tllC:Se COmponen-ts in:~lude, but are not limited to; dextrose, maltose, palatinose, xylitol, 35 lacti tol , hydrogena:ed ~.somaltulose and other new aldito 1 s or a combination thereof. These materials may be blended with panning modifiers including, :out not l~_mited toq gum arabic, maltodextrins, corn syrup, gelatin, cellulose type materials like carboxymethyl cellulose ac hydro~;ymethyl cellulose, starch and modified starches vegetable gums like alginates, loC~~.~>- bean. gum., guar c~umF and gum tragacanth, insolub~.e carbonates like calcium ca.rbo:nate or magnesium carbonate and ta~~c. Antitack: agents rnay a7_so be added as panning modifiers which allow for 'the use of a variety of carbohydrates arid sugar alco~iols in i::he development of new pa~~ned or coated gum products. Ilavors may also be added. with tie sugar coating and wit: c~~ffeine to yield unique product characteristics.
IS Another type of pan coating would also isolate caffeine frorn the cn~wing gum ~_ngredieats. This technique is referred to as film coat~_ng and is more corr~rnon in pharmaceuticals than in chewing gum, but procedures are similar. A film like shellac, Zero, or cellulose-type material is applied onto a pellet-type product form~_ng a.
thin film on the surface of the product. The film is applied by mi.x.i_n.g t°ne polymer, a p1 ast:Lciz~~_ and a solvent (pigments are o~..wional ) and spraying t:~ve mixture onto the pellet surface. ihi s i.s done :in conver~~tion.al type panning 2S equipment, or in more ad.wanced side-ver~.t~d coating pans .
Tv~'hen a solvent 1 ike al cool is usod, eVt:ra precautions are needed to prevent fires and explosions, and spec~saJ_ized equipment must be u;.;ed.
Some film polyi~ners can use water as the solvent in film coating. he cent ad~rances ~.r~ polymer researcrs and in film coating technology eliminates the problem aJsoc_i.<_;t~ed ;.with LIi~L u:;e of flammable solvents in coaLinc_ These adz-ances crake it possibJ_e to apply aqueous films to a pellet or chewing gum product. Although. caffeine is not 3~ nighi.y water soluble, it may be added ~!o this aqueous film - l4 -solution and applied with the filrn to tie pellet or chewing gum product. The agueous film, or ever the alcohol solvent fl lm, in which caffe~:~ne ~.'~s dispersed mail also cc;ntain a flavor along ~frit~~. th~~ po~~~ymer and piast.=~ci zc~r.
The prey=;.o~.~sly desCr_.bed er~ca.~~su ~_ated, agglomerated or absorbed caffeine may readily bF
incorporated into a chewing gum composition. 'a"~~e remainder of, the chewing gum ingredients are none:ritical to the l0 present invention. What is, the <.oatec~i particles of caffei ne can be inco~:~crated into convents_ona~'~ chews ng gum for:mul~{tior~s in a conventional manner. Coated r_affoine may be used in a sugar c~ieGaing gum or a sugarless Chewing gum.
The coated r_affeine may be- used. in ei than regular checaing ~S gum or bubble gum.
Tn general; a chewing garn con:auos_it:ion typically comprises a water-so:Luble bulk ~~.,o:rtion, a water-insoluble chewable gum base port=on and typically water-insoluble flavoring agents. T~:e water-soluble portion dissipates 20 with a portion of the flavoring agent over a period of time during chewing. T.~e gum base i~o.rtion is retairaed in the mouth throughout t'.de crew.
The insolu~~le gum base general l y comprises elastomers, resins, fats and o~.lsr waxes, softeners and 2S inorganic fillers. ~lastorners may include polyisobutylene, isobutylene-isoprene copolymer and styrene butadiene rubber; as well as natural latexes such as chlc.le. Resins include polyvinylaceva~e armd te.rpene resins. Fats ar_r.~ owls may also be included in the gum baser including tal~_ow, 30 hydrogenated and partial7_y hydrogenated vegetable oils, and cocoa butter. Commonly employed waxes include paraffin, mlc.rocrystalli:.e and natural waxes such as -beeswax and carnauba. According to the preferred e:mbodimenwt of tho present invention, the insoluble gum base constitutes 3S betiaeex about 5 o and about 95 o by weight of tk~e gu,°rao r3ore p-~eferabaly the insoluble gum base comprises bet~reen about 1o% and about ~t~ o by Freight o.~ the gum, and ?~osv preferably h~:~_~teen about COs and a:~ou~. 3~~ by a~e~.ghv o.f the guru.
The guru b~.se ~.yp~~.ca~~.y a'1 so :~nc~.x~des a filler component. ".~."he ~=i:~~.er coznp~ner~t umay be ~~alcium carbonate, ~~~a.g~.es~.~.~m carbonate, talc, dicalcii:m phosphate or the like. The filler may cons t ~ tote be t~ree~~. about 5 %' and about 6 ~ ~s by ~reaght 20 of the gum base.. ~:~~efe~~ab~.y, the filler compra..ses about 5 o to about. 5~~~ by ~?eigh~: of the guru bass:.
Gum bases typ~ca.l~.y G0.lso oo~.ta~.n softeners, includa.ng glyceYal monostearate and glycerol triacetaveo further, guru bases rc~ay also conta~.n optional °ing~°e~°~ze:a~a such as ant~o~cidar~ta, celor;~, and ezn~zlsi.fm~~ers v ~'he present ~7..n~Yer:~tior;~
contemplates employ:{ng any comn-cerc~ally ac~;epta.ble gum base.
The taater--soluble portion of the chewing 20 gum may further co~rz~orise softeners, s~reeteners, flavoring agents and combinations heweof.
Sof te~:ers are added to ~:,he c'her~ing gum :gin c;rder to optima~ze the cheV~ab~.l~.ty and rlo~zth feel ~f the gum.
Softeners, also ~~~o..~jn ~::~. ~.:.he art as pl<~.s~..zc:izex~s or ?5 plasticmzx~~g agents; generally constitF"te ?~et~aeen about 0 a ~~ and abouw 1~ a by Freight of tl~e che~airig gum. Softeners con~emr~lated by the present ~.n~rention include g'myce~y~.r:i, a.eci.th~.xa a.nd corc~i~.atzons thereo:~~ . 'w'u~~°ther y ac~u.eon.:~ wweeter~.er 30 solution) such as t~~.ose ccant~~.ming sorb~.to_a, hydrogenated starch hydrolyxates, corn. syrup and combinations thereof may be used as softeners and binding agents in g-'~n.
~s mentio..eaed ~,bo~re, the coat.e.d caffeine of 3~ ~.he present invention zn~.y be used ~n s~~.ge.r or sugarless gum fo~°su~wations . Sugar s~reeteners generally include sacoharlde-containing components corrcmo:~ly ~noin t~~e chewing gum art ~h~.c~.
comer ~ se, but are nr~,t limy te_d to, :sucrose, dextrose, ° a'~'~ )8/r3~~ej ._ ~.~ - g'~'~''/"sW ~u13.~'~ iT
~.ai~ose8 dextrinF d°wied invert s~xgare f:r-~.~tose, levulose, galactoseco:~a~ syrup solids and the like, alone or in aa~y comination. sugarless sv~eeterae~°
~? nclude componenvs Y~9i~.h sweetening ch;~.xact~~ris~,ics but which are de~roa.d of the cor~only kTZO~n sugars alld CoILl~~l.s~,, bud a=?T'u. nC.e~. ~ .7~yTt~.ted to, cal.5.gi~~.' c~~.~:o~'1C'_i.
such as soxbitolg ~nannitoE., <~'~a~to~., h.~:drogenated starch h~-dxol~rzatesg ma~~.~.~to~ and the l..~fce~ ~.~one ox . ; n a:~~ oombination . , - 1~ ~ Depending on the particular o.affe~.ne .
release pa~o~W~.e and s:~ze:Lf~-s~.ab~.~.~.c~r nf~.~a~aded, ~.he coated caffeine of the pxesent ~.n~rent~.on ca:a also be used in combination w~.tS. ~ncoated h~.g~A-~potenc~
sweeteners or wi~~~ ~-~igh-potency s~,reec~:~~ews coat"ed .3.5 with other materials and by other techniquesa Z-1 v.~a~o~°~.xzg age~~t ~na~r a~.so :gym present. ~r~
the chewing gwm in an axraourat ~a.~.hin tzve range ~sf prom abo~:c~. a m ~.~ ~.o ~bou~ ~_~% , prefe~°a~~~.~r f:~or~ a~bo~.~:~.
. 5 o to s.bout~ 3 0 : b ~y k~re~.gi~t o ~ the gu.:°r~. ~'lae lav-oy°ing ae~ents ~ria.~ corr!!pr.~.se essent~.a~. oi~.s, synthetic flavors,, ox :m~.~.~urew thereof: i~acaudi~.ag, but not limited ~.o oils deri°~ed from plants and ~xuyts s~xcr~ as c~~.x~~.s oils, -~:~~a.it essences, peppex~znnan~, oil, speermint oil; clove oil, oil of 25 sadintergreen, anis;_:, and ta~.e like. Art:if ~ cabals .~la°~orinc-~ components are ~.~.so cont2a~tp~..ated for use in gt::~s of the present in~.ren;:ion. Those spilled in she art ~:~1~. recogn:~~.ze that n~aura~. a:~.~d arti~.a.~.ia~.
flavc.xing agents z~.a~r be combined i?~ and ser~sorall~ .
30 acceptable blend. ~~.1. ;such flavors and, flavor blends are cos~templa°ced b;~~ the: present: ~.n.°~ent~.on.
Optional ingredients such as colorsp emuls~.fa.exs arid pha:~aceuta.ca 1 agents mad be acLded to t:he chewing gums. .
3~ rn genex°a:;t, cheRFring gum is ~~mn~fact~.~°ed bar sequentza~,l~T adding t-~.e ~z-ar~c~u.:~ chewz:~-~g gu:ca~
ingrec3ierWs to a coarcmexciall~ a~,rai°! ab~.e ~W:.~cer knock.
in the art. ~lfte~~° ~~.he ingredien°~s ha~~e peen tho~-oughl~r mixed, the g°~a mass ~.s~ discharged from .~ s.::~ ~,yn.au.y I l ci~le mixer and shaped ~r~~:o the ~.es~red. ~or~r such as ~~r rolling in~.c~ she~~.s :=zand cu~.'~.ing a~n~.~ s~.,:~..c:~s,, extx-uding in~r~ ch~,~s~s or c°as~~.~.~.g in tca ~:~e~'~lets m ~e~.e~°al l~ ~ the :~ngr ~:d'l e~.~s ~~ ~°e ~axe~. hy~
first melting t:ne gbase and ~.d.d~.ng ~.~. ~~ ~.~°~g~
rur~nir~g mixer. '~'~.e l~~s~: 5~ay c~ls~ ~e ~.e7 ced ~n the mixer itself. ~o:~cr or er~ulsa.fiers m~~~ ~.~.;~o be added ac this ~~.r~.e . ?~. ss~~ ~ener such as g~.y~cer:~n ~~n~~
c11 sO l'3e added ~.~ i:.?"s:l..s ~m._II''~e,~ ~.~.~Tl~' '4d'~~~"i u~'r~.a~
czIld c'~.
~0 portion o~ t:.he bu°? king :~gen ~ o _~'~.r~her pcart.ion<a o~
~~e a~ulkix~~g agent as?~y L:he~~ be ~.c~ded tc: ~~te Ix~ixer. Z~
fla~ror~.ng ~.ge~.t is ti~.~.lw~ bedded vri~mh ~.he ~ilaal portion o~ the bulking ~.ge~tm ~°he ccawec~ r~a~~c~a:ne of the present inc~enta.ol~ :~.s ~~°e~erabl~r added a..°rter ~ 5 the ~in~..1 portzc~n o~ bu~_ltil~zg ~ge~t. and ~l a~ror h~.~re been added.
'I'he entire ~rri:~4ir~g procedure t~,~y~ica'? l~~
cakes from ~i~re to z_i~tee~? rnirs~:.tes,. bc~;~ ~l.ol~?ger anixing cirnes rr~y sc~~ecz~.es be ~°e~.irec~.. ~.~:'~~se 20 skilled ice. the art ~7ii.l :~'eoagxli~e tha~~ r.n~
~rariations of the a~c~~re c~.es~r~_:~ed proGed~.re ar~~~ be cal 1 c'~ed a '~'xa~~~es ~'he ~ca~? lr~~r~.I7.g e~ar~p~.es of t~~e. in~ence~.on and comg~arac.i~e e:~~:~ple,s :ire ~~rc~~i.dec~. ~'~y ~~~ c~
expls.r~ation and a.11 ~sL.rs.t:~.c~.. _ she ~.c~°~~z:~as ~.~~.ated in ~'~.bl~~ :~ comprise ~rara.ows sugar ~or~~n.p~las ° ;~ ~rhich c~.ze~e_-~~~e can be added co gum ~.~ter t a..s d.issc~l~red ih -~arius ~.c~~a.ec~as cape scyl~e.n is .
_ ~8 _ ~rs~E z ~xaxay~.e Bxp~. Bxamgle Bx~nttp~_ q~xample ;~~.xainple J L
Sugar G3..9 ~~ ~ 9 G0. 3 G0. E3 G0.,,3 53 .3 Gun Bale 19 . 2 19 a 3 19 2 w9 . ~$ ~9 A :2 ~.9 . 2 Gl~~ex~.r~ 3_ . ~ ~ . a~. 0 m J 0 . 0 0 . C 1. .
Corn ~,5 ..~ 1.5 . 9 ~.2 ., 9 ~.2 0 =3 ~.~ . a SYp ~ec~_~P~ira 0 . 2 d ~ 0 .2 0 . ~ ~ 0 . ~, 0 . 7 Feppera~An t 0.9 0.9 C.9 0.9 0.9 0.9 Flavor Lic~.lid/
Cageine $ blind O.S C.0 G.0 G.tJ G.Cv 20.0 Example y . and 2 -~ Caffeine por,~rder can be added directly to the gum.
Example ~ w A " 0 . 0 gram portion of caffeine car.
be dissolved in 90.0 grams of hot water, -r,aking a 10.0 2~3 solution, and added to gum.
Example 4 -- A 5.0 gram portion of caffeine can be dissol;red in 95.0 grams of hot propylene glycol, making a S.Oo solu tion, and added to guru.
Example 5 ~- ~1 ~ . Cl gra.m portion of caf:Ceine can be 25 dissol,~ed in 95.0 gr:~m of llOt glycerin, making <~ 5.0 solution, and added to g~~,~m.
Example 6 - t~ %.5 gram portion of caffeine can be dissolved in hot earn syrup, making a 2.5~ solution, and added to gum.
3G Tn the next examples of a sugar gum formulation, caffeine can be di.solved ~.~n hc>t water and emulsifiers can be added tc the aqueous soa_ution. Example sclucions can be prepared by dlSSO~'~T.lng 10 crams of caf_~eine in 90 grams hot water and adding 5 grams o:L emulsifiers o:~ ~ra.rious 35 hydrop~z,il ~.c-lipophi.lic balance ~~iL~} val.ues to tie $~~' ~'~5'i~:iia1"3 _ ~ ~ _ d't~~IW~~Uiiio:l l l solution. The mixtures can then be used in the fol~.a~lxng forrz;uls.s a ~:~~~ 2 ;:ar~. ~~
~~ampl ~xamp~. ~~~:e ~mpl ~xar~;pl ~~carxpl a a ~ ~: ~: a 7 $ 9 10 11 12 St.~gar 50.7 50.7 50.~ 5tJ.7 50.7' Sfl >
gage 19.2 x.3.2 19.2 ' 19.2 29.2 19.2 Cozxa Syrup 12 . 9 1 ~ . 9 12 . 12 . 9 - 12 . 12 ~) 9 .
g G? ycerir_ 1. ~ ~ . ~ 1. ~ _ 1. ~ 1. 4 1.
~
Dextrose ~Sonohydrate 9.9 S.9 9.9 9.9 9.9 9.9 Peppermint 0.9 0.9 0.9 0.9 0.9 0.9 F? avor Caffaine/
emulsifier =hater 5.0 5.0 5.fl 5.0 5.0 5.0 2diacture Hone ~L~=2 a~=~ HZ~a6 HLB=9 H~-12 ~YaTri~J~.eS ~ - a'~3.e saIT:eta'le ~rJr!1t1~atltJl7.s 1~ ~ aS
made in examples - L~ , res~aect~.vely, except that the '?
flavor c ap b~ m~xec:~ togevher ts~e ~~.queoyas ~r:Ltlz caffeine soiutian a_~~d err~uls~.~zedbefore:.> ng r~he a~.da.
mixture to the batcbz. .
gum Catfea.~aecarp a:Lso be ersdec intovarious bl base ing red1ea~ts A ty ~.'1 cal formula as . base ?s f ollo~:s 'tft .
Polyv~.r~~%e~. acetate ~'7 ~ynthetlc rubber Paraffin ~~ax 13 2 t~ ~'a~. ~
~lyceral ~ianos=rearate Terpene ~Zes~.r C:alciu:~ ~arbo~.;~te ~ a.~t_ler ~:~a,~;~ ~s;~~~~s ~ ~~ w ~3~~r~~~~n~~~rr sof toned ~r~or to ~.I~eir s~d~.~.~:~on in ~.~~e base ~nt~fac~~ring pr,:,~cess ~ To ~h.~~ preso~~a:.ened ba0.~e corr~ponen~~ caffe~..ne ca~~ be added ar~.d mixed.g a~~d ~~Ler~
the presoftened base/c~.fiei no .b_Lend can be adcLed to r:vake the finished base o 1~~ the folio=~~i~~g exa~~p3.es a caffeine can be ~n~~ed fvrst v~y~.~h one ~~:~ the base ingredients o and 'r_r~.e mixed ~.zz~~redient~ can ~~~.e~:~ ~be used in ~aka.ng a b:~se. '~~ze i~~.grediej~.z..s b:-~e~.de:d ~~a.ti~
caffeine car 'chef. ~e used at vhe le°~re:ls i~°sdxcatLd :gin the typical base vcu~.a above ~xa:aple ~.9 - Tire te°~°pene re:,:~~.m;.sec~ to make the base is ~3°~ pc;l~r~erpene resin a~.~. ~m z5 caffeine.
example :2C - ~'he pc~.y~y°i~?~~. :~_ce~.a.te ~ESecs~o make the base is X80 1~.;~a~ ~.Y~q poly~ri~.~°1 acweta~:e and 2~s caffeineo ~xarn.ple ~~ _ Tne paraffin ~,~r~.x used ~:o ~~a~~e ~0 the base is 96% paraff~.n z~ax arid ~o c:affe~.n.em ~affe~.a~e zt~ay aa.so be added ~_o are ot~:~er~aV~_se complete c~L~Tn base.
~°xamp? a '%~ ~ U ~, 5 o caffei?7.e can be xnx.xed Sri th 99 > ~ o of a ~;a~.~ base ha-~ina t~.e ~.:~.~o~re listed ~5 typical foranula. °~he ~.a~:feir~.e can be: added ~~~ar L~'e end of t~se process after al ~. ~~he other ingreda_ents aLa addedm _.
The sara~p:Les of finwshed -base jade ~:a.t~a caffeine added t~o ,~~ fferent k~ase co~r~.~onents cG.n tl~er~
be e~raluated in =.W ;~uga~ -r.ype che~ir:g ~~;c &worm~:~late;~
as fr~l~o~s m ~~'~ 98?23Io~ _ ~~ _ ~/v~iS961~~~~i :~~LJ' 3 ~, s:
~; ~~, m For e~~.~ri~'~e~ ~~3 ~L~. ~~. ai:~
Stx~ar ~ ~ a 2 ba:~~ 1~ o ~ a ~c~r~~ ~~x4a~
~~~r~~.ex:i.r3 3. m 67 ea~~ ros ~
_ 15 ~ir.~~cal2~rd~ate ~ ~ ~
~ep~ermi~.~.
~'~wa~Or. ~9 ~ ~
2G ~.~3~a ~'~7.~ ~~c~,~O."_'er~..Cc?J.
~.e~.r~. O~ Cc'~.w~'~T'de La? ~1'1G
f 1.Y"11S'I1~C gL2I:1 1.S ~
m ~' n a ~Sl.Tlg a:.~'1~ fo~.~.~~93.T1~$ff~~2"11Lt1.c'~.'s,:.~..C3~7 of a i~..~C~cr 25 or sugar-free gu:-n, a ~rari~~t~c~f er~ca~~u~.ai.eci C a ~ f a 3.32 ~ S aFt1''~7 cl'C Er' ~ ~:
~ 2.~-~ C ~:? T3 ~ E? ~'t.~"a ~ 'L7 22. -''F,.FLE
~
yWt.
a) ~.uc~arFree Su a=w Sorbitol X8.8 --Sugar - 54 a -' viannitol 8 r -G;.am Base ~ 25 ~ 20 3 ~
~:~
Glyceri?: 8 . I .
5 . ~
I0 Corn Syrup - 12..0 Lycasin brand. 6.~
riydrogenated Starch Hydr olyzates Dextrcse - 10.0 Mono:~ydra to Peppermint ~. . ~ 0 . 9 ~0 T'1 a V~Or Active Caffeine 1.00 1.C)u for spray dryings the solids :'.evel of an aaueous or alcoholic solution can be about 5-30~, but preferred levels are indicated in the examples 1_sted.
Example 23 - An 80o s:~ellac, 20o active caffeine 3C~ pcwder mixture is ob~~ainecl by spray drying an alcoho~w~/sheilac/caffeine solution at to~.a:~ solids of i0~a Example 2C - A 50~ s~ellacp 50o active caffevne powder mixture is ob::.aimd by spray dry-~ng an appropriate ratio of alcohol/she:~_lac~'caffe ~..ne solu.tio_r~ at 10 o solids .
Example 25 - A ?00 ~e:in~ 30o active caffeine po~ader mixture is obva:inec.-~ by spray dry.ng an alcohol/~ein/caffeine solution at 10~ solids.
Example 26 - A 4u shzel lac, 60 ~ active ca-vfeine w 23 _ powde r mixture is abv~aincd by fluid-ber. coating caffeine with an alcohol/shellac so=~.ution at 3C° solids..
Example ~7 -- A 5G% shellac, 40o active caffeine powder m~_xt~?re is attained by fluid-bed coating caffeine with an alcohol /shellac seiutian at 3C'~ solids .
Example 23 - A ~a0 0 ~ei_rl, ~0 ~ active caffeine pcwder mixture is a~wcained. by j~luid-beca coating caf:f:eine ~J with an alcohol/Zein solution at 25° s~~li ds a ~~,xample 2~f - An 85° wax, 15 o active caffeine powder mixture is attained by spray chilling a mixture of molten wax and caffeinea Example 30 - A 7~~% wax, 30~ active caffeine po:ader mixture is obtained by spray cl~.~lling ~;. mixture of molten wax and caffeineo IJxamp 1 a 31 - r., 70 ~ Zein, 30° act5_ve caffe:~re povrder mi xture is c~ tain.ed by spray drying a hot aqueous mixture of caffeine and rein d~.spe~rsed in an acueous, high-~0 pI-I (pI-I of 1i . 6-12 . C ) media at IO o solids n Example 32 - F~ 20=~ 2ein, 80 ~ active caffeine powder mixture is abtairmd by _flu~_d-bed' coating caofeine with an aqueous, hih-pI-i (pI~I=1.1..6-12.0; 7e~.n d:i.spersion of 10~ solids.
2~ Example 33 - A 20 ~ ZE.in, 20 o she3.lac, 60 o active caffeine powder mixture is obtained by spray drying an alcohol/shellaa/caf~~eine mixture and t~~.er: fluid-bed coating the spray dried product for a second coating of alcohol and Zeino ~0 Examples G3 ,~c 33 wou f d all ~yi~;e neayv ~, coreplete encapsulation and would delay t:he release of caffeine when u:~ed in the sugar ow: sug;..~rless g;_~.n fo~.~zE;u"~atvon~> in 'Table !! o Tie :~ighe.r levels o~.' coat~.ng would give a lorge:r delayed release of caffeine than. the lower levels of casting..
3~
- ?4 Other polymers that are inore water soluble and used in coating wo~!~~c', have a faster rel<Wa:~e of ~l:he caffeine.
Example :~ ~ - An 80 o g~latin, 20 o acti-c~e caffeine powder mixture is obtained by spray drying a hoL
c~elaLir:/caf Lei_ne ::~o~_~.~;ticri at 'G ~ solids Example 35 - A 3Uo hydroxypropylrnethyl cellulose (HPMC; , 70 o caffeine po~,ader mixture is obta_i.ned by fluid-bed coati ng caffeine wit~i an aqueous solution ov IFMC at 10 s 1C solids .
E~>arnple 30 - A 50 o maltedextr-r, 50 ~ active caffeine powder mi;~tare i.s obt~,.;.ned by spray drying a not aqueous solution of caffeine and maltodextrin at 3J=~ solids.
hxampie 3 7 - A ~!0=, gum ar~~bic; ~0 ~ aci~ive caf feine powder mixture is obtained by fluid-bed coating caffeine with an aqueous sol.u~~ian of gum arabic at 30 o solids .
The coated caffe~.ne from Examples 34 and 35, when used in t'ne chewing gum formulas in Tab~Le 4, wo~zld give fast release of Gaff=nine. The product coated ~.~ith 2~ maltcdextrin and gum ara~.>is in a.xa.mples 36 ancd :37, when u;~ed in the guru. formulas in 'fable ~, would s':ow very fast .release of caffeine in c'ne~~.i.mg g~:m compared to c:a~cf~:ine added directly.
Caffeine could also be used in gwm as an agglomerated caffeine to give fast or delayed caffeine release. Agglomerated caf:~eino can be prepared as in the following examplesv ;;xample 3~3 -- A l.'3 o hydrcxyprop~jlmethy:l cellulose (HPMC} , 85° active c:~ffei.ne poEP.'der mixture is prepared by 3t} agglomerating caffeine a~L:d ~IL~i~C blended together, with water being added, and the res~~:lting :product being dried and ground.
Exarvple 39 -- A I5 ~ g~~~.atin, 85 o actlvE~ caffeine:
powder mixture is made b~~ agglomerating caffeine and gelatin blended together, ~~~i~uh water be ing added, and the. resulting product being dried and ground.
~'~~ ~~123kG5 _ ~z~ _ 3'~:'~IUB~GI~~~'~7 oaf~ei ne powder rc°axture ie a~.ade by agg:~omerating ~aaff2~Tle wl~y'~. ~."~,.~. ca.~.fi'OilC~.i. :aC7.~5.g~':~..C~2w ~C7~.~:~?.,~'a.Z.:~lg ~&~m Fein,_ and drying arid grinding the re~~.~.ta.ng product Ex~.mple ~~. - ~ :~~~ shellac, 8~~ ~ act~.~~e caffeine powder m~.xc.ure i~ made by agga.o~.eratiF~g _ oa~feine w~.t:~ an ~~~..coha~ uo:j~~:ior cor~raY.~~~.ag shellac, and d~.yi~!g ar_d g:~ir.d~_ng t~.e r~.~s~~~.~:zr~J
product>
0 .' Example ~-~ - r-~ :~0 a ~~~MC~ 80~'s ~.c.t:iv'e caffQine powder mixture is obtained by agglomerateng asp H~~C and ca~fe~ A a ~n~.~~~.~.re ~~~.ended togethe~g wxt~~
water being added and the resulting.product being dx°1ed a~~3 gro~r~da °15 EXamnle ~~ - ~ 70~s 'Jeing 80~ actxtre eaffeir.e po~~rder. rcn~a~xre ~.;~ ca"~~:.airze~I bv~ aGrgl orne:~at~.:~g caffeine and Zeirl ~.ys~o~'.~~~ed irl hicrh~-p~=~ ~~b~ater ~.1v5--12 0 0 ) at 15-°s solids g vrzF~h the rest~ltirzg ~rod~ac:t~
~e~_ng dra.ed arid g:cc~~cnd 20 Example ~~ - ~_ :~0 ~ waxF 80~ acti~re coffee he powder m~.~d~a~a.re ~ ~ obt~air~ed ~a~~ ~.gg~.ome:~at~.s~g caffeine and molten wax,, and cooling and grinding ~.he resulting prad~:.c~t Example ~~ - ~ ~S a m~a~.todextrin, 85 25 ac~.i~re caffeine pc~~~der miact~~°a is obt<~.i~:ed Ly agglorr~erating a b~e~~.d c~~ caffeine amd ~r!altoc~ex~.rir.s then adda.rg «ater~ d~pz~~,~ aid c~r~.ndi~ar~~
Za.~.l of r~e abo~Ye a~i~wtu~°es can ~e added to any of the follocalr~g t~.es of ohewing gmn foula~ a '~°~3~~.~
Se,r.r~arSu.c~-ar~esS:xf4r3es ~~i~a s s ~ S~a~arles Su ~~- Sc~rbitc~ly7i~l~. 4~ath s tdater L~;casinNo ~4acer Cum Base Ig .s I ~ .2 . ~~5 .5 :5 . ~5 .5 l Suc~ar 55.~ ~ :,:~.0 ..,.~ __ .._ 1~ Sorbitol _.. ~.0 5Z_E3 ~~.~ 5x..~
itol _- ~- $.0 8.0 ~.'~.0 Corxa Syrup L3 _ I :~ . M _ _ _ _ _ :~ ~.
x~ycasin/
5orbitol .
I~.quiti. _ ~ a . 5 ~a.7,mss _ _ . ~
~by Glycerin 1.a- _d.~ 1.5 ~.S ~.5 Lecithir~ __ ~_ 0.2 0_2 ~.2 l~e~trone P~oncahydr ate 9 ~ ._ ~ w _ _ w ~ _ ~ _ ~
Flavor o.5 0.~ 1.5 I.5 I.5 ?Q Level. of .~ot~.ve Caffeine Owv X3.5 ~..t~ ~.0 :! .G
~
~c3~ ~.lC~tIIL'~ SOrb:i?~.ol~ .IQ's' uOY'.J~.~O~,, .~ ~
&' 4Pu.'t~E.-'r~
!k~3 hydrogenated ;staroa x:y~.rolyza~e syrtap If each of t'_ne exa~T~p ~.es of agglomerated material (8-45) were evaluated in t_he formulations shown in Table 5r some samples would rive ~~:affeirze a dela°~,~ed release and others a fast :release. Sa~npl.es using ae=LnY waxJ and sheJ_1 ac 3~ wculd yield the slowest release rate w:~ereas s~amplcs with HF~iC and gelatin. would y~_eld the next slowest rel ease.
I'~altodextrin ~~aould ive a rya: t release compared to c;ao seine added directly to t:~~~ cu:n.
Partially% coated or gully~ ceatPd caffeine can also be used in sugar t~,%pe gum formulations containing ether sugars, such as in the fol ;~_owi~~g v~ormul.aticns A-Go ,_ f _.
'~ ~s~
('6~~. . ,y 3 Cum 3a8e ?9.z 19. ~ ~.9.'? .~9.y>~9.2 x.9.2 1J.2 Sugar 5~.5 4"-~.r ~ ~L~.S 4:9.5 a~.S 53..5 ~~.5 G lyc~. riot ~ . 4 ~. . ~. ~, . ~ ~. . ~ W . g: 1.
~ > a.~ ~
Cozn ~.9.Q . 2:3.~ ~.9.c7 23.0 ~~.0 ~.6.G
~9.~J
Syrup ~7~x~rose a_ _- 5~(~ __ __ __ _..
~3C~~6~ _ _ - m .. .. _ .. m, a ~ _ .. _ Fruc~.c~se __ _m ' S.D _~ __ ..- __ Invert _- __ __ ~p p __ __ __ Sugar T~':~.~.~os~ ~_ __ .._ __ '__ ",~.p __ Pala~iraose _ - - _ _ _ _ . _ _ ~, Com Syrup __ 5ora __ _. __ __ __ So~.ids Pepp~zminv Fla~ror ~.9 0." ~.9 ~..p ~.9 tt.:3 0>9 z~eve 1 of ~c~a.ve 1. 0 ~. . ?3 1 . U ~...'~ . 0 ~. . ~~ 7.
i's . 0 Calf eizze Thane foT-anulat? ans also cont~.ain sugax may alcohol-s such as so~:b~ tol, zzar~n~ to~~F
.~rlitol, Z~.Ct~CO~., 2Tlc.,.~....t~.t0~., ~t.~"~'C:7l:i!c'7.~..~'.'.X~..~~~, 5~."1~C~~~C~1"'sc%la~~.:~.a..~l~.
~y~Gl.Jr~r~ ~~~~~~"~.5.....~.oi~.~ .:J~.~a~..~~.~~..~''..~'J
o~ F'~'...ro'srle~e~~. r ~o~'IF11~.ZC'3.t~oTlm'".7 V,t~.th ~3aLt~.~..t.~.'~~
~,..oatE~.'~.
o~ ~f.~~.~~
G'oat'EC~.
caffeine can a:~s~ be ~ac~e using ~ra~iou:~
sugar a~cohc~ls, such as the follo~~T:~r~r~fcarniulat:~o~~~s ~i-~v 2 ~; _ ~~~Il~': 'i rT ' J ~. I; ~~ tai U h ~, ~~3.f-S~ 2J.J~ ~~.aJLS.~ ~.J.~ ~ ZS.$J X5.5~7~J..~J~~i i.~J
Sorbi~ol 53.C ~ 46.C~~:0 ~~..C ~~~C 4.? 3~.C:37.C ~~~.C
.,C
Sorbi~o~ ...
:Liquid/ ~ 1 ~ C~~ S
C~
1 1~.C~.C m- ,eC _.. -- e ~
7.C ..
Cc.'i~a i83 ' ' ~ a~
l~aa~rti~03. -- ~O.C~3.C)S.0 ~.C f3..C S.C f~.0 E.C
1'a..sayts.~0~. .._ __ 5 0 _.. -.. S __ .._ ~_ 0 Xy-~. i ~ 02 ~ _ ~.5 :~. _ .. 5 ~. _ - u- . C ~ .. a 5 m Cl > 0 .
G C
~a~~i~oi a- __ __ _.. z~.o __. ...___ __ Hydrogenated- _ ..- _ -... - ~5 :LO _ _ _ _ _ . ~ _ i.~ C
somaltulose .
.~
_ Glycerin 2.C 2.~,~?.C7 8.C 8.0 n.~ 3.C 6.0 -__ Fl~~ror z.s ~. i.5 1.5 ~..5 ~..~ z.5 1.5 -~.5 Le~re. of .~c t i v~
1.C? 1.~ ._.0 ~..0 :~.~tl.Ca ? 1.0 ~.0 ~3'F~~'11'1.2 ,.0 ta) L~;rca~in, a? e~~.~orst.sse :~ivo~lic~tx~.C~
1 so~
All of these formu.lairio.ns in Table 6 and ''able 7 which "use vhe agglomerated caf.~=eine as described in th«
~5 examples (38-45) and ,n the p._rc~~rious encapsulated examples (23,-35 j would be a<pected tc g ~~re a de.l_a~red. rel easof caffeine or a fast release o_'~ caffeine compared to a product made by adding caffeine c~irect~! y to gmtl as a r~owder.
Nlul tiple step agglom~~ratien/'e:ncapsulat~_on 3(~ procedures can also be u~.~~ed. :in making :re'.ease mcdifzed caffeine 'nor use ~ n ~,.he ,~or~~~ulations i:n 'I'a~les 5~ 6 and 7 .
Lxamples of mul tiple step tr_eai~ments a:r:e here describede example ~6 - Caffeinr~ 1s spray dzied with maltodextrin at 3C~ solids to prepare ~.~ ~ovder. This poCader 3~ is then agglomerates: with a "-~y'ar_oxypro:~>ylmethyl se 1 lulose (r-:~-EMC) i.z~ a rati o -:~f 85/:x.5 pc~wc~er/~aPMC~ wetved w~.th watef - 2~ -and dried. After gr:~nding th.e rosinting powder wi 11 contain about 68o active caf:Ceine, 17o maltodextrin and 15% HPMC.
Exa:rple ~7 - Caffeine is agg?_omerated grit h HpMC in a ratio of 85/15 ca-_'!eino/z-IP1~1C. After drying and grinding, the resul~~ing powder is il~~id-bed coated ~rit:l~ an alcchol/s hellac solution a~~ .about 25° solids to give a f~_nal produc ~ contas_n f ng aaout 60 ~ ac;tive oaf feine, 10 o HPMC; and about 30 o si~ellac.
E:>ample C~8 - Caifein~: is agglomerated wits H~MC in a ratio of 85/15 cafveine/h~l~~lCe After drying and grinding, the resulting powder is agglomerated with a 15« solids, hi gh-p.-I, aqueous solution of Z~:irs to g:i.sre ~: f:i_na~_ product containing about 6C o active caf:fei ne, ~ 0 a HPMC, and 30 IS Zero.
Example 49 - Cafveine: is spray dried with a 25 solution of gelatin . ~'he spray dried ~_roduct is tl~~:~n agglomerated w9_th a 7_5 o solidsp hi g1u-pII, aqueous solution of Zeino The final product wile r.:ontain about 50~ active caffeine, 20o gelatin, and 30~ Zein.
Example 50 - Caffe ins: is .aggl.omerated witi~ molten wax in a ratio of 85/15 caffeine/wax. Lvrhen the: rnixture cools and is ground, it a.s fyu~_d-bed coated with a 25 ~ 2ein - 75o alcohol solution, diving a final product containing 60% active caffeiney 10o wax az~.d 30° Zein.
These examples 4e~-50~- when used in zany of the formulations noted in Tables 5, 6, and 7 above, give caffeine ~ delayed re.7_easeu These mulv:iple step procedures can actually give more delayed release than t:~.<~ single step processes . L~Iultiple step processes of mor a than two s reps may give even longer delayed release tines, but may ercnerG-~.ly beco.ne less cosy effecvive ar_cless efficient.
Pref erably, spray drying c~~n be=_ the -fi:rst step with additional steps of fl,~id-'sued coating, spray r_hill.ing and agglomeration being part of the latter steps.
_. ~C _ Log absorption type examples, ti'ae delayed release rate of caffeine is dependent or, the type otabsorbi3ig material. Most material s 1i k~s silicas, s~.li_cates, Cc~.~lulcse, carbonates, and hyarw~xide:~ we>uTd be expected to g~_ve a more delayed ,elease than amorphous sugar and sugar alcohols. Some examples:
)Jxample 51_ - A hot TO % solution o1= caffei n~~ is 0 sprayed ontc a preci~:;iLatoc~~ silica to al:~:~or~: the caffeine.
The mixture is dried and ground. The final product is about 50% active caffeine.
example 52 - A hot 10% solution i:: sprayed onto a pharmasorb clay cafft:>ine. The mixture .is d.~=ied and ground and gives a final product of about ~0% clay and 20% active caffeine.
l~~xample 5~ -- A :LO=o solution of cavfc;ine is sprayed onto a microcrysta?_~~a_ne cellulcse powde>-. 'fhe mixture is dried and ground and gives a product that is about ?0%
m~_o.rocrystalline cel__~ulose and 30 ~ acti.ve c<~ffei_ne o Example 5 ~' - l~ 10 % so~luti on c~f caa~feine =~s sprayed onto a high absorption starch. The :ri~:t~:re is dried and ground and gives a product that is about b0'~ starch and 200 active caffeine.
iJ::ample 55 - :~1 lu'o sclut ion c>f ca:Cfeine _~s ~:pra yed onto a calcium carbomace powder. ~'he mixture is dried and ground and gives a p~~oduct of about ~0% caladium carbonate aryd 10% active caffe_~_ne.
Example 56 - A hov' 10 % soluti.or~ oi. caf:Ce~~:,:c is sprayed onto a highiz,r absorptive dextrose material., The mixture is dried a-r~d ground and. gives a praduet of about 80%
dextro:ae and 20° act:~:~cro caffeine.
Exaz~~;ple ~7 - A hot 1C % solution o2. caffeime is sprayed onto a sorbi;~ol powder to absorb the material. The mixture is dried a:~;:l ground and. gives a product of about 90%
-- 3:!
sorbitol anal l o o active ~;affea.E~e a The samples prepared in exam~~}les 51-57 can be used in gum formulations as noted i n fables 50 6~ a~~d 7 a i'hose preparations which have caffeine absor'.~:eci onto a m~ L.ere_~al teat is not water soluble are expected to give a delayed release and those that are water solub.~_e are expected tc give fast releasem ~0 Another r~~odification or absox-pt~ion technique is to dry the caffeine tog-ethe_~ ~rita~ a sL?c~ar or sugars alcohol, or resolidify the caf feine with sugar or ~;uga.r alcoho~~ when mixed together in a molten sta~'~ea E.~ample 5C - affeine is added to molten sorbitol ~5 in a ratio of 9C parts SOrb~to;~ to 10 part,, caffeineo After mi~:ir~g, the blend is cooled and groundu Example 59 - Caiffei.nE~ is added L. c: molten den>trose in a rat,~io of 90 parts dextrose to t 0 parts: caffeine a After mixing, the b1_end icooled and ground., Example CC; - 4"~ caffeine i.s dissc>lved in 96 ~ r:igh fructose corn syrup Th.e ns_d>t~~.re is e~~~apo~~ated to a low moisture and groundp The product of e~:amples 50-6C; may be added to the gum formulations shown is Tables 5, 6 and 7m 25 zany of t~_e examples listed are v,ing-le step processes ~ I-Iowover, more deli°-~red release c:f the caff~a Lne may be obtained by combir~ir:~; t~~e various px-ocesses of encapsulation, agglomeration absorption, a.r~d entrap_mento Any of the preparations made i~~7 examples 51.-6G can be 3Q further 'treated in fluid--bed coating, spray chilling, or coacervat-~on processes to encarJsulate the ~~roduct, and can be ~agc~=_omerated S~rii~I~: vari o~:s rn~teri_a.ls and proceduretv in a varisty of multiple step prccesses~
3~
- .~~
The caffe~.r~.e carp a~.:~o be used with a variety of high intensity sweeteners and blended together before encapsulat~.c~~A, agglo~~erat:i.on, absorption, and e~°~trap~clent ~ '~'h.is car:1 redt.zce bitterness assoc:~~.ted ~adyth eawfeine. Soinsw examp l es area Example off. ~ Caffea~~xe and ~.~par~:ame are blended together ii a ~/~. ratso ~.s a ~o~~ad.c,ro This mixtyare is then sp:=ay chilled with wax in a ratio of ? 0 60/4 mixture/wax ~~o obtain a powder c~:on~.~lining 40ro caffeinep 20% aspartaz-~e; and ~~0% wax ~xa%~tp..~.C~ t~.G -' ~c3.f ~E.'~_Ze1~..' and t~3~.L1.1T2c1tJ.n In a ~/1 ratio are ci~.ss~:~lve~. an. water ~a°ith a ~.Cn solution of gelatin anal spray driedm This spray d~°i ed ;oowd.er is then agglomerated ~rzth a ha.ghrpF~ a~.r-;ueou.s ~5-°s Zeir solutions The m~.x~:ure is dried and ground, and gives a product containing ~U~ caffe.ir~e, ~.0~ tha.umatin, 35% gelatin, anC ~~;o ~eina Exampae.~~:~ ~ :'~'affei~l~.e and: a~.itam.e i~~s a '7/'2 :2U ratio are prepared iZ:s r."~. hot ~....F~% ~olut:i.~Xiw Thi ~
solution is sprayec4 onto a high absor~~ti on sil.xca powders The n~ixtzz~ae is dri ed , ground s.nd f~ui d~bed coated with an a~.cc~holjshellac~ mixtures gi~ring a product that conta~_ns 35% caffeine, 5p alitame, 400 ~5 s~.l~.ca, and 20 o sne~.? acs Example ~4 °- Caffeirbe and soda.r...amm cyclamate in a :i/~: ratio are b? ended to~~et~aex~ a~~ a p~~~rder arid then agglomerated ~~.tn ~patex .~:nd h.ydro~~.~~aropylmethyl cellulose (HPMC) ~ This ~alend is dr~.eLi~ ground and 50 agglomerated further ~rith a high-pH, a~"~eo~.~s l5%
solution of Zein to obtain a product con ta:~r_ir_g 3~
sodium cyclamate, :34o caffeine, ~..~% H~~~G and ~0%
G~ein o Example ~:~ - c~'affe r~.e and gaLy~cyrn:h~.~in in 35 a ~.r~ ratio are b~r;~a:xded togc~.t.er a~ a 7o~~idE:~° aid f~.axid-bed coated ~~~.~~h a so:~u.t~.oz~ of 25=~ shellac. ~.r~
alcohol o The coated product a s agg~..oz~.creted further with water ar_cl hydroxypropyl methyl ce F °! u? ose (HP1~C) to obtain a product containing 30a caffeineT 300 glycyrrhi~in, 25° shellac, and 15o HPMC:b Example ~6 - Caffeine and sodium saccharin in a ratio of ~_/1 are bl.e,.~ded toget~-.er as a powder and fluid-bed coated with a solution of 35° s'nE:llac in alcohol. '=I'he coated product is agglomerated further faith water and hydraxypropylmethy~_ ~:~el lulose ( ~3PMC) to obtai n a product containing 30o caffeine, 30% sodium saccharine ~5o shellac, l0 and f 5 0 ~IPMC a If the b1_~:nds of caf~:eine and. other high-int:en:~ity sweeteners of examples 61-~6 are tested in gum formulations such as those note! in T-abler ~ , 5, 6 ~~nd 7, a significant delayed release of t::~e sweetener arad reduced caffeine bitt=erness G.:ould be expected ~ This de ~ eyed release would irnp~Yo~e tree qualit~r. of flavor A The fcllowi :ng are exarnpl es of fiber extruded PVr.~C/caffeine blends to give a delayed eel ease of caffeinr~ and give reduced b_i.tterness:
Example ~7 - Methurr~ riolecular weight PVAC and caffeirAe at a ratio of 3i'1 are blended together as a poiader and extruded. The fibers are cooled arid ground to c.~ive a product containing 75~ PV!~C and 25~ caffeine.
Example ~8 - Mt~d~.'~ura r~~oleCUlao weight PVAC, caffeine and aspartame at a ratio of 12/~ll are blended together as a powder and extruded , the= resulting fibers are ground and give a product containing ?0~ PVAC, 24o caffeine and 6~ aspartamea Example 59 - M~>dium molecular weight PVACp caffeine, aspartame, and sodium gluconate at a ratio of 16/4/4/1 are blended together ~,.s a po~~~der and extrud.ed~ 'she fibers are ground and gizres a product containing 64~ PVAC, .L6°~ caffei no, 16'-o sodiur g~lucc>r~ate, and ~ ~ aspartan~te.
Sodium gluvanate is ~, bitter:~ess inhibitor than can be mixed wit: caffeine before beinc, encapsula ted or entrapped. This bitterness inhibitor <~lor~g with other.
bitterness inhibitors sac.h as sodium salts of chloride,.
... 3 ,~ _ ascorbic acid, glutamic acid arad citric acid, as well as other Various organic cempoundes, can b~4 add.ed to catffeine to reduce bitterness.
Example 70 - A 20o hot aqueous solution of maltodextr_in is mixed with a. 4 0 ~ hot sc>luti.on of sodiL:m g.7_uconate. Two liters of this mixture is cc}mbined ~a:~_th 100 grams of caffeine, dispersed a~~d spray dried. A final product containing 50% maltodextrin, 35~ sc7diam gluconate i0 and 17a caffeine is obtas_n.edm Example 71 - A 2400 ml quantity of a 25=,, hot aaueous solution a:C mal todextr_in is m~_xed ~~ith 50 c~~-~a~rs of aspartame to form a suspension. To this i~~ added a r_ot aqueous solution of 400 grams =~f sodium gluconate, 200 grams I~ of caffeine, 1200 grams of hot water. This rW xture is spray dried to obtain a pcwder containing ~8a, mal.todextrin, 32%
c scdium gluconate, 16~ caffeine and ~° aspartame.
E~>ample '72 - '~'o a 24 ~0 gram c~uant:ity of a 25 ~ hot solution of maltodexarin, 200 ~-grams of citl_ic acid and 50 20 g=~ams of aspartame care added and suspended To th.~.s ~T:ixture is added a hot aaueous solution of X100 grams of sodium gluconate, 200 grams of caff~-we and 1200 grams of hot water. This mixturE. is spray buried to obtain a powder containing 41~ malvode~:trin, 20° sodium gluccnate, ~~_9°
25 caffeine, 1~% citric. acid and 3o aspartame.
The abova e~~amples are made t.o o~>tain not only a fast release of caf f eine ii> dr wing gur,~, based on maltodextrin encapsulation, but also to obtain fast -release of a sweetener and ~~i'~ter_r~.ess inhibito_~s to counteract ~0 bitter effects of caffeine.
Iv should be appreci::~ted that th~~ m.ethods and compas:itions ov the present invention are capable of being incorporated in the form of a variety of embodiments, only a feq~.j of. which have been i.llustr_:~ted and described above. The 35 ir:vention may be emk::ods_ed in other forms w~.thout departing from its spirit or essen tial cr=aracteristic:s . It ~ ~~ _ a..~:
~~c~ 9~ia~ie~ .~.,~~,a~" , , xvzll be apprec7 ate. t~-zat the a~,dit~.o~ o~ some other i:rzgred~er~ts, process steps, z.t:eri~.l~ ~~~ ~.o~~pcar;er~~.s nod spec~~ica~.~~ ir~c~.~.ded ~~.il~. saa~~e an ad~re~°se ~.~p~.ct on the prese~.~: ~.n~~e~t.~.or~m ~°he ~~est ::node o~
the ~n~rent.~.ora ~a~ ~:here~ore c:~.c~~.ude inc~:~edi~:~.t.sy process steps r ma~er.ia~.s or c:or~~porzerzts ot~~er than those Lisped ai~o~re for i~.c~.~s~.o~? or ~se~ ~.r. tire a.~.~rera.tion~ ~~o~ae~ery t.:ne c~:escrioec~ ea~cmd:~~te~at.s are to be cons~.dered i~ a~.l ~ respects o~z~~ a.s i~.l~stra~~.ve and not ~°es~r:~c~~.~re ~ aid t~~.e scope ~~
the in~er~tio~ i.s, ~~.ere~ore, ~.r~d~.cat.ed b~ the appended c~.aaxns r~.t.~e~° than ~S~ tae .fore:goi x~g descriptionm ~1~. charges ;~h~.ch come ~ri.~.h~.n the meaning- a~zd rar~~e of ec~tai valerzcry o~ the, claims are ~5 to be embraced ~aythi n t.beir scope
Claims (24)
1. A method of producing a chewing gum containing physically-modified caffeine in order to control the release rate of the caffeine comprising the steps of:
a) mixing a quantity of caffeine with a modifying agent to form a physically-modified caffeine;
b) adding a quantity of the physically-modified caffeine to a chewing gum formulation to provide a caffeine level in the gum of from about 01.2% to about 5%.
a) mixing a quantity of caffeine with a modifying agent to form a physically-modified caffeine;
b) adding a quantity of the physically-modified caffeine to a chewing gum formulation to provide a caffeine level in the gum of from about 01.2% to about 5%.
2. The method of claim 1 wherein said modifying agent is an encapsulating agent.
3. The method of claim 2 wherein the caffeine and encapsulating agent are also mixed with a solvent and the resulting mixture is dried prior to being added to the chewing gum.
4. The method of claim 3 wherein the encapsulating material is selected from the group consisting of maltodextrin, gum arabic, Zein and shellac.
5. The method of claim 3 wherein the mixture is spray dried and the solvent is selected from the group consisting of alcohol and water.
6. The method of claim 3 wherein a high-potency sweetener selected from the group consisting of aspartame, alitame, salts of acesuifame, cyclamate and its salts, saccharine and its salts, thaumatin, monellin, dihydrochalcones and combinations thereof is mixed in the mixture in combination with the caffeine.
7. A chewing gum made according to the method of claim 3.
8. The method of claim 2 wherein the caffeine is fluid-bed coated with a solution of encapsulating agent and solvent in order to decrease the rate of release of the caffeine in the chewing gum.
9. The method of claim 8 wherein the solvent is selected from the group consisting of alcohol and water.
10. The method of claim 8 wherein the encapsulating material is selected from the group consisting of shellac and Zein.
11. The method of claim 8 wherein an additional high-potency sweetener selected from the group consisting of aspartame, alitame, salts of acesuifame, cyclamate and its salts, saccharin, and its salts, thaumatin, monellin, dihydrochalcones and combinations thereof is mixed in the mixture in combination with caffeine.
12. A chewing gum according to the method of claim 8.
13. The method of claim 2 wherein the caffeine is encapsulated by coacervation in order to decrease the rate of release of the caffeine in chewing gum.
14. The method of claim 2 wherein the caffeine is mixed with a molten encapsulating agent and the caffeine is encapsulated by spray chilling in order to decrease the rate of release of the caffeine in the chewing gum.
15. The method of claim 14 wherein the encapsulating agent comprises wax.
16. The method of claim 2 wherein the caffeine is mixed with a polymer as the encapsulating agent and the resulting mixture is extruded into fibers in such a way as to encapsulate the caffeine in order to decrease the rate of release of the caffeine in the chewing gum.
17. The method of claim 16 wherein the polymer is selected from the group consisting of PVAC, hydroxypropyl cellulose, polyethyiene and plastic polymers.
18. The method of claim 1 wherein the caffeine is mixed with an absorbent as the modifying agent.
19. A method of producing a chewing gum containing physically-modified caffeine in order to control the release rate of caffeine comprising the steps of;
a) mixing a quantity of caffeine with an agglomerating agent and a solvent to partially coat the caffeine;
b) removing the solvent from the mixture of caffeine and agglomerating agent to form a dried material; and c) adding a quantity of the dried material to a chewing gum formulation to provide a caffeine level in the gum of from about 0.2% to about 5%.
a) mixing a quantity of caffeine with an agglomerating agent and a solvent to partially coat the caffeine;
b) removing the solvent from the mixture of caffeine and agglomerating agent to form a dried material; and c) adding a quantity of the dried material to a chewing gum formulation to provide a caffeine level in the gum of from about 0.2% to about 5%.
20. The method of claim 19 wherein the level of coating on the agglomerated caffeine is at least about 5%.
21. The method of claim 19 wherein the level of coating on the agglomerated caffeine is at least about 1.5%.
22. The method of claim 19 wherein the level of coating on the agglomerated caffeine is at least about 20%.
23. The method of claim 19 wherein the dried material is ground to a powder prior to adding the dried material to the chewing gum.
24. A method of producing a chewing gum containing a physically-modified caffeine salt compound in order to control the release rate of the caffeine salt compound comprising the steps of:
a) mixing a quantity of a caffeine salt compound with a modifying agent;
b) drying the caffeine salt compound/ modifying agent mixture; and c) adding quantity of the dried material to a chewing gum formulation to provide a caffeine salt compound level in the gum of from about 0.2% to about 5%.
a) mixing a quantity of a caffeine salt compound with a modifying agent;
b) drying the caffeine salt compound/ modifying agent mixture; and c) adding quantity of the dried material to a chewing gum formulation to provide a caffeine salt compound level in the gum of from about 0.2% to about 5%.
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CA002271889A CA2271889C (en) | 1996-11-27 | 1996-11-27 | Method of controlling release of caffeine in chewing gum and gum produced thereby |
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CA002271889A Division CA2271889C (en) | 1996-11-27 | 1996-11-27 | Method of controlling release of caffeine in chewing gum and gum produced thereby |
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CA002431848A Expired - Lifetime CA2431848C (en) | 1996-11-27 | 1996-11-27 | Method of producing chewing gum containing caffeine and gum produced thereby |
CA002431856A Abandoned CA2431856A1 (en) | 1996-11-27 | 1996-11-27 | Method of controlling release of caffeine in chewing gum and gum produced thereby |
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US10709661B2 (en) | 2015-09-11 | 2020-07-14 | Andrew Guise | Oral particulate composition |
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1996
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- 1996-11-27 CA CA002431856A patent/CA2431856A1/en not_active Abandoned
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US10709661B2 (en) | 2015-09-11 | 2020-07-14 | Andrew Guise | Oral particulate composition |
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