CN110680010B - Magnolia bark gel bead for cigarettes - Google Patents

Magnolia bark gel bead for cigarettes Download PDF

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Publication number
CN110680010B
CN110680010B CN201911052290.3A CN201911052290A CN110680010B CN 110680010 B CN110680010 B CN 110680010B CN 201911052290 A CN201911052290 A CN 201911052290A CN 110680010 B CN110680010 B CN 110680010B
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China
Prior art keywords
parts
magnolia
gel beads
volatile oil
officinalis
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CN201911052290.3A
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CN110680010A (en
Inventor
蹇顺华
吴成刚
张瑞萍
李星
彭建
孙炜炜
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China Tobacco Hubei Industrial LLC
Wuhan Huanghelou Flavoring and Essence Co Ltd
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China Tobacco Hubei Industrial LLC
Wuhan Huanghelou Flavoring and Essence Co Ltd
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/02Manufacture of tobacco smoke filters
    • A24D3/0204Preliminary operations before the filter rod forming process, e.g. crimping, blooming
    • A24D3/0212Applying additives to filter materials
    • A24D3/0216Applying additives to filter materials the additive being in the form of capsules, beads or the like
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/061Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Fats And Perfumes (AREA)
  • Disinfection, Sterilisation Or Deodorisation Of Air (AREA)

Abstract

The invention discloses a magnolia bark gel bead for cigarettes, which comprises the following components: 0.5-5 parts of mangnolia officinalis volatile oil, 60-80 parts of polyethylene glycol, 10-20 parts of sodium stearate, 10-20 parts of propylene glycol, 30-50 parts of low-methoxyl-group pectin, 20-40 parts of calcium chloride, 5-10 parts of chitosan and 5-10 parts of guar gum; also provides a preparation method thereof, which comprises the following steps: s1, heating and uniformly stirring mangnolia officinalis volatile oil, low-methoxyl-group pectin, guar gum, sodium stearate and propylene glycol, cooling to 4 ℃, dripping into a calcium chloride solution, stirring, adding polyethylene glycol, and performing crosslinking curing to obtain pre-composite gel beads; s2, adding a sodium tetraborate solution, and curing at room temperature to obtain composite gel beads; s3, transferring the composite gel beads into a chitosan acetic acid solution for crosslinking and curing to obtain magnolia officinalis gel beads; the cigarette filter tip has a fresh, pungent and sweet flavor when added into a filter tip, can keep the flavor for a long time, reduces the stimulation of smoke to the throat, and has controllable flavor intensity.

Description

Magnolia bark gel bead for cigarettes
Technical Field
The invention relates to the field of tobacco essence and flavor, in particular to a magnolia officinalis gel bead for tobacco.
Background
The cortex magnoliae officinalis is a common traditional Chinese medicine, has the effects of relieving cough and eliminating phlegm, helping digestion and guiding qi downward, and eliminating dampness and harmonizing stomach clinically, is proved by pharmacology to have the remarkable effects of reducing blood pressure and inhibiting pathogenic microorganisms, and the cortex magnoliae officinalis volatile oil contains eucalyptol and isomers thereof, accounts for about 40-55% of the total amount of the volatile oil, is provided with alkenes, phenols and the like, has a fresh sweet fragrance in tobacco, is coordinated with the smoke, can well reduce the throat irritation caused by the smoke, and is a good cigarette spice.
The flavoring in the filter tip has the advantages that the flavoring of a plurality of cut tobaccos is incomparable, the essence added in the filter tip does not participate in combustion, and various toxic and harmful components can not be generated due to thermal cracking, so the filter tip is not limited by the license list of the tobacco additives, the relatively low-temperature suction condition can ensure that the fragrance of the fragrant raw materials is purer, however, the flavoring of the filter tip has a plurality of defects, the fragrance of the essence is easy to permeate outwards, the obvious external fragrance can be generated when the cigarette packet is disassembled, the essence is easy to dissipate, the fragrance is not lasting, and the like.
In the prior art, the gel beads have the excellent characteristics of simple preparation process, mild conditions, high controllability, high encapsulation efficiency, good heat resistance, good stability and the like, and the preparation of the gel beads is mainly completed by utilizing the ionic crosslinking action between polysaccharide and multivalent cations, the covalent crosslinking action between polysaccharide and glutaraldehyde and the electrostatic action between polysaccharide, for example, sodium alginate and Ca are used2+The gel beads have large water content, high porosity, low strength and poor adsorption and diffusion efficiency, are not beneficial to slow release of the fragrance and quickly dissipate the fragrance.
Disclosure of Invention
In order to solve the problems, the invention provides the magnolia officinalis gel bead for the cigarette, which is added into a filter tip, has fresh, pungent and sweet fragrance, can keep fragrance for a long time, reduces the stimulation of smoke to the throat, and has controllable fragrance intensity.
The technical scheme of the invention is that the magnolia bark gel bead for the cigarette comprises the following components: 0.5-5 parts of mangnolia officinalis volatile oil, 60-80 parts of polyethylene glycol, 10-20 parts of sodium stearate, 10-20 parts of propylene glycol, 30-50 parts of low-methoxyl-group pectin, 20-40 parts of calcium chloride, 5-10 parts of chitosan and 5-10 parts of guar gum.
Preferably, the molecular weight of the polyethylene glycol is 1000-.
Further, a preparation method of the magnolia bark gel bead for cigarettes is also provided, and comprises the following steps: s1, adding the volatile oil of cortex Magnoliae officinalis into the mixture of low methoxyl pectin, guar gum, sodium stearate and propylene glycol, shearing and emulsifying at high speed with span-80, adjusting pH to 7, dropping into calcium chloride solution, stirring, adding polyethylene glycol, and crosslinking and solidifying to obtain pre-compounded gel beads; s2, adding a sodium tetraborate solution, and curing at room temperature to obtain composite gel beads; s3, transferring the composite gel beads into a chitosan acetic acid solution for crosslinking and curing to obtain the magnolia bark gel beads.
Preferably, the preparation method of the magnolia officinalis volatile oil comprises the following steps: grinding cortex Magnolia officinalis to particle diameter of 2-10mm, soaking cortex Magnolia officinalis in distilled water at room temperature for 8-24 hr, distilling under normal pressure for 1-5 hr, condensing to recover distillate, and separating oil and water to obtain oil phase to obtain volatile oil of cortex Magnolia officinalis.
Preferably, the heating temperature of S1 is 85-95 ℃.
Preferably, the dropping rate of S1 is 2 ml/min.
Preferably, the screen filtering is further included between S2 and S3, and the aperture of the screen is 1-5 mm.
The main chain of the low methoxyl pectin consists of alpha-1, 4-glycosidic bond connected with D-galacturonic acid, and the side chain is L-
Rhamnose or feruloyl, wherein carboxyl on molecular chain can react with Ca2+、Ba2+And the multivalent cations are subjected to a cross-linking effect to form an egg lattice structure, and a core material mixed with the egg lattice structure, namely the mangnolia officinalis volatile oil, can be embedded, but the mangnolia officinalis volatile oil is released quickly and leaves fragrance for a short time due to the porosity of the structure, so that in order to reduce the porosity and prevent the leakage of the mangnolia officinalis volatile oil, chitosan serving as cationic polysaccharide and low-methoxy pectin gel beads are subjected to mirror interaction to form a polyelectrolyte complex to reduce the porosity, namely the chitosan is used as a polyelectrolyte composite membrane to form a plurality of layers of gel beads, and the fragrance leaving time of the mangnolia officinalis volatile oil is prolonged.
Meanwhile, in order to improve the embedding rate of gel beads on the volatile oil of the mangnolia officinalis, the dispersion degree of the volatile oil of the mangnolia officinalis in the low-methoxyl pectin is very important, as the main component of the volatile oil of the mangnolia officinalis is eucalyptol and isomers thereof, and then alkenes, phenols and the like are added, and propylene glycol and polyethylene glycol are used as dispersion carriers, the compatibility of the volatile oil of the mangnolia officinalis and the low-methoxyl pectin is improved, so that the volatile oil of the mangnolia officinalis is uniformly dispersed, and the embedding rate is further improved.
Guar gum and mangnolia officinalis volatile oil are embedded in the low-methoxyl pectin gel together, after sodium tetraborate is added, the guar gum and the sodium tetraborate form semi-solid reversible acid gel, the guar gum and the low-methoxyl pectin form an interpenetrating network structure, and the comprehensive performances such as heat resistance, stability and the like are greatly improved.
Polyethylene glycol reacts with calcium chloride to form a coordination compound, according to the theory of a hybridization orbit and a coordination field, mainly because calcium ions react with-C-O-C-groups of the polyethylene glycol, the calcium ions attract electron clouds of oxygen in the-C-O-C-groups, lone pair electrons on oxygen atoms are partially transferred to outer empty orbitals of the calcium ions to form O-Ca coordination bonds, namely a coordination structure is formed, on one hand, the low methoxyl pectin is helped to consume redundant calcium ions, the problem that the concentration of the calcium ions is too high, and the permeability of gel beads is reduced due to too high gel strength is solved, on the other hand, compared with the gel beads, the polyethylene glycol has stronger fluidity, and can be extruded to permeate out of a polyelectrolyte composite membrane formed by chitosan, the fragrance strength can be controlled, when the fragrance strength is strong, squeezing the gel beads, wherein the volatile oil of cortex Magnolia officinalis is popped out with polyethylene glycol, and when the fragrance is desired to be lasting and light, the product is naturally sucked.
The invention has the beneficial effects that:
1. chitosan, a cationic polysaccharide, and low-methoxyl pectin beads are subjected to mirror interaction to form a polyelectrolyte complex, so that the porosity is reduced, multi-layer gel beads are formed, and the fragrance retention time of the magnolia officinalis volatile oil is prolonged;
2. propylene glycol and polyethylene glycol are added as dispersion carriers, so that the compatibility of the magnolia volatile oil and the low methoxyl pectin is improved, the magnolia volatile oil and the low methoxyl pectin are uniformly dispersed, and the embedding rate is further improved;
3. guar gum and sodium tetraborate form semi-solid reversible acid gel, guar gum and low methoxyl pectin form interpenetrating network structure, and the comprehensive properties such as heat resistance, stability and the like are greatly improved;
4. the polyethylene glycol and calcium chloride react to form a coordination compound, on one hand, the low methoxyl pectin is helped to consume redundant calcium ions, the problem that the gel bead permeability is reduced due to overhigh calcium ion concentration and overlarge gel strength is avoided, and on the other hand, the fragrance strength of the mangnolia officinalis is controlled when the product absorbs the water.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
Preparing the magnolia officinalis volatile oil: crushing 100g of magnolia officinalis into blocks of about 2mm-10 mm; adding 300 plus 500g of distilled water, soaking at normal temperature for 8-24h, heating and refluxing at 85 ℃ under normal pressure for 1-5h, collecting distillate by a condenser, and performing oil-water separation to obtain the magnolia officinalis volatile oil.
Example 2
Dissolving 0.5g of mangnolia officinalis volatile oil in 10g of propylene glycol, mixing the propylene glycol solution of the mangnolia officinalis volatile oil with 100ml of low-methoxyl pectin solution with the concentration of 0.3g/ml and 100ml of guar gum solution with the concentration of 0.5g/ml, adding 0.5g of span-80, homogenizing at 85-95 ℃ for 5min, adjusting the pH to 7, stirring uniformly, adding 10g of additive sodium stearate, vacuumizing to remove bubbles, cooling to 4 ℃, dropwise adding 100ml of calcium chloride solution with the concentration of 0.2g/ml at the speed of 2ml/min, stirring while dropwise adding 60g of polyethylene glycol, and carrying out cross-linking reaction for 1h to obtain pre-composite gel beads;
adding 20ml of sodium tetraborate solution with the concentration of 0.1g/ml, curing for 1 hour at room temperature, and filtering to obtain composite gel beads, wherein the aperture of the screen mesh is 1-5 mm;
after absorbing the water on the surface of the composite gel beads, transferring the composite gel beads into 100ml of chitosan acetic acid solution with the concentration of 0.05g/ml, and carrying out crosslinking reaction for 1 hour to obtain the magnolia officinalis gel beads.
The Magnolia officinalis gel beads are placed in a filter tip, and a sample is sucked, so that the fragrance lasts for 2 h.
Example 3
Dissolving 5g of mangnolia officinalis volatile oil in 20g of propylene glycol, adding 0.5g of span-80 into 100ml of low-methoxyl pectin solution with the concentration of 0.5g/ml and 100ml of guar gum solution with the concentration of 1g/ml, homogenizing at 85-95 ℃ for 5min, adjusting the pH value to 7, stirring uniformly, mixing uniformly at 85-95 ℃, adding 20g of additive sodium stearate, vacuumizing to remove bubbles, cooling to 4 ℃, dropwise adding 100ml of calcium chloride solution with the concentration of 0.4g/ml at the speed of 2ml/min, stirring while dropwise adding 80g of polyethylene glycol, and carrying out cross-linking reaction for 1h to obtain pre-composite gel beads;
adding 20ml of sodium tetraborate solution with the concentration of 0.1g/ml, curing for 1 hour at room temperature, and filtering to obtain composite gel beads, wherein the aperture of the screen mesh is 1-5 mm;
after absorbing the water on the surface of the composite gel beads, transferring the composite gel beads into 100ml of chitosan acetic acid solution with the concentration of 0.1g/ml, and carrying out crosslinking reaction for 1 hour to obtain the magnolia officinalis gel beads.
The Magnolia officinalis gel beads are placed in a filter tip, and a sample is sucked, so that the fragrance lasts for 12 h.
Example 4
Dissolving 2g of mangnolia officinalis volatile oil in 15g of propylene glycol, adding 0.5g of span-80 into 100ml of low-methoxyl pectin solution with the concentration of 0.4g/ml and 100ml of guar gum solution with the concentration of 0.8g/ml, homogenizing at 85-95 ℃ for 5min, adjusting the pH to 7, uniformly stirring, uniformly mixing at 85-95 ℃, uniformly stirring, adding 15g of additive sodium stearate, vacuumizing to remove bubbles, cooling to 4 ℃, dropwise adding 100ml of calcium chloride solution with the concentration of 0.3g/ml at the speed of 2ml/min, stirring while dropwise adding 70g of polyethylene glycol, and carrying out cross-linking reaction for 1h to obtain pre-composite gel beads;
adding 20ml of sodium tetraborate solution with the concentration of 0.1g/ml, curing for 1 hour at room temperature, and filtering to obtain composite gel beads, wherein the aperture of the screen mesh is 1-5 mm;
after absorbing the water on the surface of the composite gel beads, transferring the composite gel beads into 100ml of chitosan acetic acid solution with the concentration of 0.08g/ml, and carrying out crosslinking reaction for 1 hour to obtain the magnolia officinalis gel beads.
The magnolia officinalis gel beads are placed in a filter tip, a sample is sucked, and the fragrance can last for 7 hours.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (4)

1. The magnolia bark gel bead for cigarettes is characterized by comprising the following components: 0.5-5 parts of mangnolia officinalis volatile oil, 60-80 parts of polyethylene glycol, 10-20 parts of sodium stearate, 10-20 parts of propylene glycol, 30-50 parts of low-methoxyl-group pectin, 20-40 parts of calcium chloride, 5-10 parts of chitosan and 5-10 parts of guar gum; the preparation method of the magnolia bark gel bead for cigarettes comprises the following steps:
s1, adding the volatile oil of cortex Magnoliae officinalis into the mixture of low methoxyl pectin, guar gum, sodium stearate and propylene glycol, shearing and emulsifying at high speed with span-80, adjusting pH to 7, dropping into calcium chloride solution, stirring, adding polyethylene glycol, and crosslinking and solidifying to obtain pre-compounded gel beads; s2, adding a sodium tetraborate solution, and curing at room temperature to obtain composite gel beads; s3, transferring the composite gel beads into a chitosan acetic acid solution for crosslinking and curing to obtain the magnolia bark gel beads.
2. The officinal magnolia gel bead for cigarette as claimed in claim 1, wherein the molecular weight of the polyethylene glycol is 1000-2000-.
3. The magnolia bark gel bead for cigarettes as claimed in claim 1, wherein the preparation method of the magnolia bark volatile oil comprises the following steps: grinding cortex Magnolia officinalis to particle diameter of 2-10mm, soaking cortex Magnolia officinalis in distilled water at room temperature for 8-24 hr, distilling under normal pressure for 1-5 hr, condensing to recover distillate, and separating oil and water to obtain oil phase to obtain volatile oil of cortex Magnolia officinalis.
4. The officinal magnolia gel bead for cigarettes as claimed in claim 1, wherein a screen filter is further included between S2 and S3, and the aperture of the screen filter is 1-5 mm.
CN201911052290.3A 2019-10-31 2019-10-31 Magnolia bark gel bead for cigarettes Active CN110680010B (en)

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Publication number Priority date Publication date Assignee Title
CN113749293A (en) * 2021-09-24 2021-12-07 云南巴菰生物科技股份有限公司 Gel particle for cigarettes and preparation method thereof
KR102544686B1 (en) * 2021-12-23 2023-06-15 주식회사 엘지화학 Cellulose acetate based resin composition
CN116019220B (en) * 2023-02-28 2024-05-17 劲牌持正堂药业有限公司 Method for reducing bitterness of radix Puerariae extract and improving water solubility thereof

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