CA1171838A - Long volatile-containing hydrocolloids having controlled release and method of producing same - Google Patents
Long volatile-containing hydrocolloids having controlled release and method of producing sameInfo
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- CA1171838A CA1171838A CA000390962A CA390962A CA1171838A CA 1171838 A CA1171838 A CA 1171838A CA 000390962 A CA000390962 A CA 000390962A CA 390962 A CA390962 A CA 390962A CA 1171838 A CA1171838 A CA 1171838A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F5/00—Coffee; Coffee substitutes; Preparations thereof
- A23F5/46—Coffee flavour; Coffee oil; Flavouring of coffee or coffee extract
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- Jellies, Jams, And Syrups (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fats And Perfumes (AREA)
- Non-Alcoholic Beverages (AREA)
Abstract
ABSTRACT Swellable hydrocolloids, such as gums, are contacted with compatible volatile compounds which are sorbed thereby. With proper selection of the hydrocolloed, this procedure may be used for frac-tionating a mixture of volatile compounds into more polar and less polar components. The volatile-loaded hydrocolloid is particularly useful for providing a consistent in-use headspace aroma to a packaged product, such as a soluble food powder.
Description
~ ~ 7~ ~ 3 Case 2813 DESCRIPTION
VOLATILE-CONTAINING HYDROCOLLOIDS
HAVING CONTROLLED RELEASE AND
METHOD OF PRODUCING SAME
Powdered food products such as soluble beverage powders (e.g., soluble coffee, powdered soft drinks, soluble tea, orange-flavored breakfast drinks) can be relatively devoid of aroma as compared to their source material (e.g., roasted coffee) or the mate-rial with which the powdered material is sought to be associated (e.g., fresh oranges). It is general-ly desirable to provide the consumer with a pleasant aroma upon opening a package (e.g., glass jar) of a powdered food product. Quite often, these products are marketed in multi-serving packages such that the package may be opened many times over a period of several weeks before the contents are fully con-sumed. It would be preferred that a pleasant pack-age headspace aroma were provided each time thepackage were opened.
To date, mo6t such powdered products have focused on providing an initial headspace aroma to the package by the addition of either natural and/or synthetic aromatic compounds. There is a need to ~71~38
VOLATILE-CONTAINING HYDROCOLLOIDS
HAVING CONTROLLED RELEASE AND
METHOD OF PRODUCING SAME
Powdered food products such as soluble beverage powders (e.g., soluble coffee, powdered soft drinks, soluble tea, orange-flavored breakfast drinks) can be relatively devoid of aroma as compared to their source material (e.g., roasted coffee) or the mate-rial with which the powdered material is sought to be associated (e.g., fresh oranges). It is general-ly desirable to provide the consumer with a pleasant aroma upon opening a package (e.g., glass jar) of a powdered food product. Quite often, these products are marketed in multi-serving packages such that the package may be opened many times over a period of several weeks before the contents are fully con-sumed. It would be preferred that a pleasant pack-age headspace aroma were provided each time thepackage were opened.
To date, mo6t such powdered products have focused on providing an initial headspace aroma to the package by the addition of either natural and/or synthetic aromatic compounds. There is a need to ~71~38
- 2 -develop aromatization techniques which will provide a controlled release of aromatics so that both an initial headspace aroma and a relatively-consistent, in-use headspace aroma can be obtained.
05 ~hile the majority of the description presented herein relates to aromatizing orange-flavored break-fast drinks with orange oil, such a presentation i5 for convenience of description only, and the inven-tion is not meant to be limited thereby, as this invention is applicable for the sorption and con-trolled release of volatile components in many varied food-related environments.
As those skilled in the art are aware, citrus oils, such as orange oil, contain about 90% d-limo-nene, a readily-oxidized, hydrocarbon component which is desirably removed from citrus oils, as is approached in the production of terpeneless citrus oil. Terpeneless oils, however, are considerably more expensive than regular cold-pressed oil. The desirable components of citrus oils are primarily variou~ aldehydes, alcohols, ketones and esters. It would be desirable if a simple process could selec-tively fractionate and fix these desirable, polar (e.g., nonhydrocarbon) components, while excluding undesirable hydrocarbon components, such as terpenes DISCLOSURE OF THE INVENTION
This invention relates to the use of polymeric, long-chain, essentially-unbranched, swellable hydro-colloids, such as gums, preferably modified cellu-lose gums, to sorb various volatile components whencontacted with a vapor or liquid phase of said component. The hydrocolloid may be hydrophilic in nature, e.g., methylcellulose, which will preferen-tially sorb polar hydrophilic, volatile components, ~7:~338
05 ~hile the majority of the description presented herein relates to aromatizing orange-flavored break-fast drinks with orange oil, such a presentation i5 for convenience of description only, and the inven-tion is not meant to be limited thereby, as this invention is applicable for the sorption and con-trolled release of volatile components in many varied food-related environments.
As those skilled in the art are aware, citrus oils, such as orange oil, contain about 90% d-limo-nene, a readily-oxidized, hydrocarbon component which is desirably removed from citrus oils, as is approached in the production of terpeneless citrus oil. Terpeneless oils, however, are considerably more expensive than regular cold-pressed oil. The desirable components of citrus oils are primarily variou~ aldehydes, alcohols, ketones and esters. It would be desirable if a simple process could selec-tively fractionate and fix these desirable, polar (e.g., nonhydrocarbon) components, while excluding undesirable hydrocarbon components, such as terpenes DISCLOSURE OF THE INVENTION
This invention relates to the use of polymeric, long-chain, essentially-unbranched, swellable hydro-colloids, such as gums, preferably modified cellu-lose gums, to sorb various volatile components whencontacted with a vapor or liquid phase of said component. The hydrocolloid may be hydrophilic in nature, e.g., methylcellulose, which will preferen-tially sorb polar hydrophilic, volatile components, ~7:~338
- 3 -such as aldehyes, ketones, alcohols, esters, etc., while excluding hydrophobic hydrocarbon volatile components. Alternatively, the hydrocolloid may be water-insoluble (i.e., hydrophobic~ in nature (e.g., 05 ethylcellulose) which will sorb both polar (hydro-philic) and nonpolar (hydrophobic) volatile com-ponents. The hydrocolloids useful in this in~ention may be either synthetically-derived and/or naturally-occurring and include isolated fractions of natural a~ex~ such a~ d~lysaccharide fractions rich in galactan and preferentially also containing mannan which fractions may be obtained from various grain and seed materials.
It has been found that polymeric, essentially-unbr~ ~ed macromolecular hydrocolloids, such asgums, are able to sorb and be swelled by compatible, low-molecular-weight volatile materials. This sorption and swelling appears to occur because molecules of a compatible volatile component are able to diffuse into a macromolecular substance.
This can be explained by the fact that the macro-molecules of a hydrocolloid are rather loosely packed and, as a result of thermal motion of flex-ible chains, very small gaps into which compatible volatile molecules can penetrate are regularly formed between the macromolecular chains. As used herein, the term "swellable" refers to the ability of a substrate to be swelled by a volatile aroma compound and does not have reference to swelling with water.
It has further been found that to enable a sufficient amount of volatile components to be sorbed by the hydrocolloid it is preferable that the volatile contact the hydrocolloid in either a liquid - ~ 7~ 8 38 or an essentially-saturated vapor phase. Mere contact between a hydrocolloid and a compatible volatile in a vapor phase having a low relative vapor pressure will not result in significant sorp-05 tion within a reasonable time. Of course, if timeis not a factor, significant loadings can take place upon contact with vapor phases having a relative vapor pressure as low as 0.2i however, in commercial operation, it will usually be preferred that the relative vapor pressure exceed 0.5. Usually contact between the gum and volatile will be effected in a closed system; however, passage of the volatile through a bed of hydrocolloid particles could also be employed.
lS The volatile-loaded hydrocolloids of this invention are suitable for use with powdered food products up to about 5% by weight, typically from about 0.1% to 2% by weight. Higher levels of hydro-colloids would usually create adverse organoleptical (viscosity) effects. Usually the volatile-loaded hydrocolloid will be dry-blended with a powdered product. It would, however, be possible to incor-porate the loaded hydrocolloid in a packaged product in other ways, such as affixed to the package it-self. De6irably, the loaded hydrocolloids will contain at least 0.5% vol/wt. (ml/gm) of sorbed volatile6, preferably at least 1% vol./wt., usually, at least about 5% vol/wt., and may range as high as 15% or more.
The hydrocolloids suitable for use in this in-vention may be any of the food-grade, commercially-available materials known to those in the art.
Suitable examples of such are carboxymethyl cellu-lose, calcium alginate, gllar, xanthan, polyvinyl-~ 7 ~ ~ 3 ~
,~ 5 _ pyrrolidone, ethyl cellulose, methyl cellulose, hydroxypropyl cellulose, and polyvinyl acetate.
Starches and their hydrolysis products (e.g., dex-trins) do not function in a manner e~uivalent to the os aforementioned materials.
The moisture level of the hydrocolloid which is contacted with the volatile is not critical. Mois-ture levels in excess of 2% by weight are quite suitable in the practice of this invention and, in certaln instances, may be preferred. Typically, a hydrocolloid may be used at the moisture content at which it is commercially available, usually on the order of 2-10% moisture by weight, and typically between about 5 and 10% moisture by weight.
It has been found that higher moisture contents in the hydxocolloid will increase the headspace aroma provided by a sorbed volatile (i.e., raise the partial pressure of the volatile over the hydrocol-loid). Lower moisture contents favor the retention of the sorbed volatile within the hydrocolloid.
Volatiles which are not released from the hydrocol-loid as headspace aroma will be liberated upon contact of the hydrocolloid with water. These liberated volatiles may then, assuming sufficient guantity is present, provide a flash aroma and/or a flavor depending on whether the volatiles are re-leased to the atmosphere or are retained in the water.
When the volatile-loaded hydrocolloid of this invention i8 to be combined and packaged with other ingredients, such as powdered materials, the respec-tive moisture content of these ingredients and the hydrocolloid should be controlled such that at ~7~838 equilibrium conditions the desired amount of head-space aroma is developed. Transfer of moisture from the hydrocolloid to the other ingredients will reduce the amount of headspace aroma that would 05 otherwise by achieved. Conversely, transfer of moisture from the other ingredient to the loaded hydrocolloid will increase the headspace aroma. It can be seen, therefore, that by selective manipula-tion of the moisture contents of the ingredients contained in the product it is possible to control the release of volatiles from the hydrocolloid. The moisture content of the powdered material which is combined with the volatile-loaded hydrocolloid will usually be less than 5% by weight and typically will be less than 2% by weight.
It should be appreciated that the loading of volatiles onto hydrocolloid substrates in accordance with this invention ls by means of sorption and ~s an equilibrium system. The volatiles are not ir-reversibly fixed within the substrate and will exerta positive vapor pressure above the substrate.
Subjecting the volatile-loaded hydrocolloids of this invention to vacuum conditions will remove the sorbed volatiles. Exposing the loaded hydrocolloids to the open atmosphere, even a dry atmosphere, will also result in the loss of essentially all the sorbed volatiles.
Essential oils, such as orange oil, lemon oil and spearmint oil, have been successfully utilized in accordance with this invention, and as these essences contain a mixture of hydrocarbon and non-hydrocarbon components, it is possible to selec-tively sorb components depending on the choice of the hydrocolloid used as the substrate. Thus, the organoleptic character of the sorbed volatiles may be controlled and determined basis the selection of hydrocolloid. It is also within the scope of this 05 invention to sorb single component aromas, such as acetaldehyde (B.P. 21C), isobutyraldehyde (B.P.
64C) and ethyl butyrate (P.P. 121C), onto gum substrates.
BEST MODE FOR CARRYING OUT THE INVENTION
Several sodium carboxymethyl cellulose (CMC) gums were evaluated (Table l) for their ability to sorb d-limonene at 30C (contacted at the 0.5%
weight level), and it was found that a lower molecu-lar weight and a higher degree of substitution (more polar) reduces d-limonene uptake. It was also found that moisture contents in excess of 2% by weight reduces d-limonene uptake. This indicates that highly-sub6tituted, lower molecular weight CMC gums having a moisture content in excess of 2% by weight would be preferred to sorb desirable, polar aroma-tics from orange oil.
T~BLE 1 Approximate Degree of Molecular % d-limonene 25 CMC Substitution Weiqht sorbed 12M31P 1.2 250,000 0 9M31P 0.9 250,000 4 7MF 0.7 250,000 27 7HG 0.7 700,000 44 4HlF 0.4 700,000 62 Several food grade CMC gums were loaded with 5%
terpeneless orange oil and then swept with an inert gas for 2,000 seconds on a Thermal Evolution Analy-~7 ~ 8 38 zer (TEA) to determine the amount (expressed as micrograms (as carbon) per gram of gum) of orange aroma released (Table 2).
05 Approximate Aroma Molecular Degree of Released CMC _ Wei~ht Substitution ( gtg) 9H4XF 700,000 0.9 1800 7HXF 7~0,000 0.7 1485 7MF 250,000 0.7 1025 4M6SF 250,000 0.4 1625 The only difference between 7ME and 4M6SF is the degree of substitution. Therefore, a higher degree of substitution holds the orange aroma more tightly. Since 7MF and 7HXF differ primarily in terms of molecular weight,it would appear that higher molecular weights favors faster release. The results of Tables 1 and 2 indicate that, to selec-tively sorb and retain desirable aromatics from orange oil, CMC gums having a higher degree of substitution, preferably above 0.4, and a lower molecular weight, preferably less than 500,000, should be selected.
Valencia orange oil (25-fold) was placed in a closed vessel with an equal amount of several dif-ferent undried gums (at least 2% moisture), the oil level being 5% by weight of the gum. After a 24-hour equilibration period, the saturated vapor in the headspace was analyzed by gas chromatograph for d-limonene content (Table 3).
TABLE ~
d-limonene peak Gum (103 GC counts/cc) Control (no gum) 53.8 05 CMC 7HXF 56.1 Ca alginate 59.4 CMC 9HXF 56.8 Guar 51.1 Xanthan S9.4 PVP 51.7 Ethocel 9.6 It can be seen from Table 3 that most of the gums did not sorb a significant amount of d-limonene from the orange oil, whereas water-insol~ble ethyl lS cellulose picked up most of it. All of the gums of Table 3 were found to have sorbed desirable aromatic components of the orange oil.
Water-soluble hydroxypropyl cellulose and methyl celluloses have been found to be equal to or better than most CMCs as sorbents for the nonhydro-carbon components of citrus oils. Xanthan gum, which is comprised of linear, high-molecular weight (over 106) molecules of low flexibility and which posses~es high viscosity, and guar gum, which is comprised of branched, high-molecular weight (2-3 x 105) molecules, have also been found to be suitable, but less preferred, sorbents for the nonhydrocarbon components of citrus oils.
The specificity in the adsorption/swelling of gums can be shown by the respective sorption of selected nonpolar and polar components of spearmint oil on a water-soluble and water-insoluble gum.
Equal amounts of hydroxypropyl cellulose and ethyl-cellulose were put into a closed vessel with an ~71838 identical amount of spearmint oil. The amount of two nonpolar ~hydrocarbon) components of spearmint --namely, d-limonene and -pinene, and the major polar (nonhydrocarbon) component -- namely, l-carvone, 05 present in the headspace of the vessel was deter-mined by means of a gas chromatograph, and this value was compared (Table 4) to that obtained by a like amount of spearmint oil in the vessel with no sorbent present.
Gum Flavor Component (Peak area as Z of control) -pinene d-limonene l-carvone Hydroxypropyl Cellulose 72 75 27 Ethyl Cellulose 37 19 18 As can be seen from Table 4, and consistent with the preceding disclosure, a polar, water-soluble gum, such as hydroxypropyl cellulose, will sorb polar compounds preferentially over hydrocarbon volatiles. Nonpolar, water-insoluble gums, such as ethyl cellulose, will sorb both hydrocarbon and nonhydrocarbon volatiles.
Carbohydrate materials, such as potato starch, tapioca and a dextrin (Capsul, a product of National Starch and Chemical Corporation) were tested for their sorption/swelling capacity as compared to a hydrocolloid such as polyvinylpyrrolidone (350,000 molecular weight). These materials were exposed to a saturated vapor phase of isobutyraldehyde (B.P.
64C) under the same conditions. The amount of sorbed isobutyraldehyde was assessed by sweeping the loaded materials with nitrogen gas at 30C for 600 1 ~ 7~ 8 3 8 seconds and then continuing to sweep at 80C until no significant aroma was released. The total aromas released this way were: PVP much more than 4,500 g (as carbon)/g (not completely desorped even at 05 80C); tapioca 39 g (as carbon)/g; potato starch 13 g ~as carbon)/g and Capsul dextrin 100 g (as carbon)/g. This data shows the almost negligible uptake of isobutyraldehyde by tapioca, potato starch or dextrin.
The loadings, on a weight basis, for the tapi-oca, potato starch and dextrin materials were ap-proximately 0.008%, 0.003% and 0.02%, respectively.
Two undried (at least about 5% moisture) cellu-lose gums were placed in separate desicators to-gether with a small vial of liquid acetaldehyde.The gums were thus exposed to a saturated acetalde-hyde vapor for a period of 24 hours at a temperature of 5C. At the end of this period, the weight gain was obtained and is set forth in Table 5.
TABTP S
Weight Increase Weight Weight of of Gum _ of Gum Acetaldehyde After 24 hrs.
(g) (g) (w/w%) hydr~xypropyl cellulose 7.7 0.78 5.6 CMC 7HOF 10.6 1.09 5.2
It has been found that polymeric, essentially-unbr~ ~ed macromolecular hydrocolloids, such asgums, are able to sorb and be swelled by compatible, low-molecular-weight volatile materials. This sorption and swelling appears to occur because molecules of a compatible volatile component are able to diffuse into a macromolecular substance.
This can be explained by the fact that the macro-molecules of a hydrocolloid are rather loosely packed and, as a result of thermal motion of flex-ible chains, very small gaps into which compatible volatile molecules can penetrate are regularly formed between the macromolecular chains. As used herein, the term "swellable" refers to the ability of a substrate to be swelled by a volatile aroma compound and does not have reference to swelling with water.
It has further been found that to enable a sufficient amount of volatile components to be sorbed by the hydrocolloid it is preferable that the volatile contact the hydrocolloid in either a liquid - ~ 7~ 8 38 or an essentially-saturated vapor phase. Mere contact between a hydrocolloid and a compatible volatile in a vapor phase having a low relative vapor pressure will not result in significant sorp-05 tion within a reasonable time. Of course, if timeis not a factor, significant loadings can take place upon contact with vapor phases having a relative vapor pressure as low as 0.2i however, in commercial operation, it will usually be preferred that the relative vapor pressure exceed 0.5. Usually contact between the gum and volatile will be effected in a closed system; however, passage of the volatile through a bed of hydrocolloid particles could also be employed.
lS The volatile-loaded hydrocolloids of this invention are suitable for use with powdered food products up to about 5% by weight, typically from about 0.1% to 2% by weight. Higher levels of hydro-colloids would usually create adverse organoleptical (viscosity) effects. Usually the volatile-loaded hydrocolloid will be dry-blended with a powdered product. It would, however, be possible to incor-porate the loaded hydrocolloid in a packaged product in other ways, such as affixed to the package it-self. De6irably, the loaded hydrocolloids will contain at least 0.5% vol/wt. (ml/gm) of sorbed volatile6, preferably at least 1% vol./wt., usually, at least about 5% vol/wt., and may range as high as 15% or more.
The hydrocolloids suitable for use in this in-vention may be any of the food-grade, commercially-available materials known to those in the art.
Suitable examples of such are carboxymethyl cellu-lose, calcium alginate, gllar, xanthan, polyvinyl-~ 7 ~ ~ 3 ~
,~ 5 _ pyrrolidone, ethyl cellulose, methyl cellulose, hydroxypropyl cellulose, and polyvinyl acetate.
Starches and their hydrolysis products (e.g., dex-trins) do not function in a manner e~uivalent to the os aforementioned materials.
The moisture level of the hydrocolloid which is contacted with the volatile is not critical. Mois-ture levels in excess of 2% by weight are quite suitable in the practice of this invention and, in certaln instances, may be preferred. Typically, a hydrocolloid may be used at the moisture content at which it is commercially available, usually on the order of 2-10% moisture by weight, and typically between about 5 and 10% moisture by weight.
It has been found that higher moisture contents in the hydxocolloid will increase the headspace aroma provided by a sorbed volatile (i.e., raise the partial pressure of the volatile over the hydrocol-loid). Lower moisture contents favor the retention of the sorbed volatile within the hydrocolloid.
Volatiles which are not released from the hydrocol-loid as headspace aroma will be liberated upon contact of the hydrocolloid with water. These liberated volatiles may then, assuming sufficient guantity is present, provide a flash aroma and/or a flavor depending on whether the volatiles are re-leased to the atmosphere or are retained in the water.
When the volatile-loaded hydrocolloid of this invention i8 to be combined and packaged with other ingredients, such as powdered materials, the respec-tive moisture content of these ingredients and the hydrocolloid should be controlled such that at ~7~838 equilibrium conditions the desired amount of head-space aroma is developed. Transfer of moisture from the hydrocolloid to the other ingredients will reduce the amount of headspace aroma that would 05 otherwise by achieved. Conversely, transfer of moisture from the other ingredient to the loaded hydrocolloid will increase the headspace aroma. It can be seen, therefore, that by selective manipula-tion of the moisture contents of the ingredients contained in the product it is possible to control the release of volatiles from the hydrocolloid. The moisture content of the powdered material which is combined with the volatile-loaded hydrocolloid will usually be less than 5% by weight and typically will be less than 2% by weight.
It should be appreciated that the loading of volatiles onto hydrocolloid substrates in accordance with this invention ls by means of sorption and ~s an equilibrium system. The volatiles are not ir-reversibly fixed within the substrate and will exerta positive vapor pressure above the substrate.
Subjecting the volatile-loaded hydrocolloids of this invention to vacuum conditions will remove the sorbed volatiles. Exposing the loaded hydrocolloids to the open atmosphere, even a dry atmosphere, will also result in the loss of essentially all the sorbed volatiles.
Essential oils, such as orange oil, lemon oil and spearmint oil, have been successfully utilized in accordance with this invention, and as these essences contain a mixture of hydrocarbon and non-hydrocarbon components, it is possible to selec-tively sorb components depending on the choice of the hydrocolloid used as the substrate. Thus, the organoleptic character of the sorbed volatiles may be controlled and determined basis the selection of hydrocolloid. It is also within the scope of this 05 invention to sorb single component aromas, such as acetaldehyde (B.P. 21C), isobutyraldehyde (B.P.
64C) and ethyl butyrate (P.P. 121C), onto gum substrates.
BEST MODE FOR CARRYING OUT THE INVENTION
Several sodium carboxymethyl cellulose (CMC) gums were evaluated (Table l) for their ability to sorb d-limonene at 30C (contacted at the 0.5%
weight level), and it was found that a lower molecu-lar weight and a higher degree of substitution (more polar) reduces d-limonene uptake. It was also found that moisture contents in excess of 2% by weight reduces d-limonene uptake. This indicates that highly-sub6tituted, lower molecular weight CMC gums having a moisture content in excess of 2% by weight would be preferred to sorb desirable, polar aroma-tics from orange oil.
T~BLE 1 Approximate Degree of Molecular % d-limonene 25 CMC Substitution Weiqht sorbed 12M31P 1.2 250,000 0 9M31P 0.9 250,000 4 7MF 0.7 250,000 27 7HG 0.7 700,000 44 4HlF 0.4 700,000 62 Several food grade CMC gums were loaded with 5%
terpeneless orange oil and then swept with an inert gas for 2,000 seconds on a Thermal Evolution Analy-~7 ~ 8 38 zer (TEA) to determine the amount (expressed as micrograms (as carbon) per gram of gum) of orange aroma released (Table 2).
05 Approximate Aroma Molecular Degree of Released CMC _ Wei~ht Substitution ( gtg) 9H4XF 700,000 0.9 1800 7HXF 7~0,000 0.7 1485 7MF 250,000 0.7 1025 4M6SF 250,000 0.4 1625 The only difference between 7ME and 4M6SF is the degree of substitution. Therefore, a higher degree of substitution holds the orange aroma more tightly. Since 7MF and 7HXF differ primarily in terms of molecular weight,it would appear that higher molecular weights favors faster release. The results of Tables 1 and 2 indicate that, to selec-tively sorb and retain desirable aromatics from orange oil, CMC gums having a higher degree of substitution, preferably above 0.4, and a lower molecular weight, preferably less than 500,000, should be selected.
Valencia orange oil (25-fold) was placed in a closed vessel with an equal amount of several dif-ferent undried gums (at least 2% moisture), the oil level being 5% by weight of the gum. After a 24-hour equilibration period, the saturated vapor in the headspace was analyzed by gas chromatograph for d-limonene content (Table 3).
TABLE ~
d-limonene peak Gum (103 GC counts/cc) Control (no gum) 53.8 05 CMC 7HXF 56.1 Ca alginate 59.4 CMC 9HXF 56.8 Guar 51.1 Xanthan S9.4 PVP 51.7 Ethocel 9.6 It can be seen from Table 3 that most of the gums did not sorb a significant amount of d-limonene from the orange oil, whereas water-insol~ble ethyl lS cellulose picked up most of it. All of the gums of Table 3 were found to have sorbed desirable aromatic components of the orange oil.
Water-soluble hydroxypropyl cellulose and methyl celluloses have been found to be equal to or better than most CMCs as sorbents for the nonhydro-carbon components of citrus oils. Xanthan gum, which is comprised of linear, high-molecular weight (over 106) molecules of low flexibility and which posses~es high viscosity, and guar gum, which is comprised of branched, high-molecular weight (2-3 x 105) molecules, have also been found to be suitable, but less preferred, sorbents for the nonhydrocarbon components of citrus oils.
The specificity in the adsorption/swelling of gums can be shown by the respective sorption of selected nonpolar and polar components of spearmint oil on a water-soluble and water-insoluble gum.
Equal amounts of hydroxypropyl cellulose and ethyl-cellulose were put into a closed vessel with an ~71838 identical amount of spearmint oil. The amount of two nonpolar ~hydrocarbon) components of spearmint --namely, d-limonene and -pinene, and the major polar (nonhydrocarbon) component -- namely, l-carvone, 05 present in the headspace of the vessel was deter-mined by means of a gas chromatograph, and this value was compared (Table 4) to that obtained by a like amount of spearmint oil in the vessel with no sorbent present.
Gum Flavor Component (Peak area as Z of control) -pinene d-limonene l-carvone Hydroxypropyl Cellulose 72 75 27 Ethyl Cellulose 37 19 18 As can be seen from Table 4, and consistent with the preceding disclosure, a polar, water-soluble gum, such as hydroxypropyl cellulose, will sorb polar compounds preferentially over hydrocarbon volatiles. Nonpolar, water-insoluble gums, such as ethyl cellulose, will sorb both hydrocarbon and nonhydrocarbon volatiles.
Carbohydrate materials, such as potato starch, tapioca and a dextrin (Capsul, a product of National Starch and Chemical Corporation) were tested for their sorption/swelling capacity as compared to a hydrocolloid such as polyvinylpyrrolidone (350,000 molecular weight). These materials were exposed to a saturated vapor phase of isobutyraldehyde (B.P.
64C) under the same conditions. The amount of sorbed isobutyraldehyde was assessed by sweeping the loaded materials with nitrogen gas at 30C for 600 1 ~ 7~ 8 3 8 seconds and then continuing to sweep at 80C until no significant aroma was released. The total aromas released this way were: PVP much more than 4,500 g (as carbon)/g (not completely desorped even at 05 80C); tapioca 39 g (as carbon)/g; potato starch 13 g ~as carbon)/g and Capsul dextrin 100 g (as carbon)/g. This data shows the almost negligible uptake of isobutyraldehyde by tapioca, potato starch or dextrin.
The loadings, on a weight basis, for the tapi-oca, potato starch and dextrin materials were ap-proximately 0.008%, 0.003% and 0.02%, respectively.
Two undried (at least about 5% moisture) cellu-lose gums were placed in separate desicators to-gether with a small vial of liquid acetaldehyde.The gums were thus exposed to a saturated acetalde-hyde vapor for a period of 24 hours at a temperature of 5C. At the end of this period, the weight gain was obtained and is set forth in Table 5.
TABTP S
Weight Increase Weight Weight of of Gum _ of Gum Acetaldehyde After 24 hrs.
(g) (g) (w/w%) hydr~xypropyl cellulose 7.7 0.78 5.6 CMC 7HOF 10.6 1.09 5.2
Claims (9)
1. A method of providing a relatively-consistent, in-use headspace aroma to a packaged powdered product which com-prises contacting a polymeric, long-chain, essentially-unbranched swellable hydrocolloid, having a moisture content in excess of 2%
by weight, with a vapor or liquid phase of an aromatic volatile at a level of at least 0.5% vol./wt., and dry-blending the aroma-loaded hydrocolloid with a powdered product, and thereafter pack-aging the blend.
by weight, with a vapor or liquid phase of an aromatic volatile at a level of at least 0.5% vol./wt., and dry-blending the aroma-loaded hydrocolloid with a powdered product, and thereafter pack-aging the blend.
2. The method of claim 1, wherein the powdered product has a moisture content less than 2% by weight.
3. The product of claim 1, wherein the hydrocolloid is a gum.
4. The product of claim 3, wherein the gum is a modi-fied cellulose gum.
5. The product of claim 1, 2 or 4, wherein the vol-atile aromatics have boiling points below 30°C.
6. The product of claim 1, 2 or 4, wherein the hydro-colloid has sorbed therein at least 0.5% by weight of acetaldehyde.
7. The method according to claim 1, 2 or 4, wherein the aroma-loaded hydrocolloid is packaged with the powdered prod-uct at a level of from 0.1% to 5% by weight.
8. The method according to claim 1, 2 or 4, wherein the aroma-loaded hydrocolloid is packaged with the powdered prod-uct at a level of less than 2% by weight.
9. The method according to claim 1, 2 or 4, wherein the moisture content of the hydrocolloid is between 5% and 10%
by weight.
by weight.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US21706380A | 1980-12-16 | 1980-12-16 | |
| US217,063 | 1980-12-16 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1171838A true CA1171838A (en) | 1984-07-31 |
Family
ID=22809543
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000390962A Expired CA1171838A (en) | 1980-12-16 | 1981-11-26 | Long volatile-containing hydrocolloids having controlled release and method of producing same |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JPS57125671A (en) |
| KR (1) | KR830006919A (en) |
| AR (1) | AR228077A1 (en) |
| AU (1) | AU7820381A (en) |
| CA (1) | CA1171838A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5736180A (en) * | 1993-12-21 | 1998-04-07 | Peiffer; Bernd | Spice impregnated edible wrapping foil |
-
1981
- 1981-11-26 CA CA000390962A patent/CA1171838A/en not_active Expired
- 1981-12-03 AU AU78203/81A patent/AU7820381A/en not_active Abandoned
- 1981-12-10 AR AR287701A patent/AR228077A1/en active
- 1981-12-15 JP JP56202370A patent/JPS57125671A/en active Pending
- 1981-12-15 KR KR1019810004931A patent/KR830006919A/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5736180A (en) * | 1993-12-21 | 1998-04-07 | Peiffer; Bernd | Spice impregnated edible wrapping foil |
Also Published As
| Publication number | Publication date |
|---|---|
| AR228077A1 (en) | 1983-01-14 |
| KR830006919A (en) | 1983-10-12 |
| AU7820381A (en) | 1982-06-24 |
| JPS57125671A (en) | 1982-08-05 |
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| Date | Code | Title | Description |
|---|---|---|---|
| MKEC | Expiry (correction) | ||
| MKEX | Expiry | ||
| MKEX | Expiry |
Effective date: 20011126 |