CN113397084A - Novel natural preservative based on perillaldehyde and preparation method thereof - Google Patents

Novel natural preservative based on perillaldehyde and preparation method thereof Download PDF

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Publication number
CN113397084A
CN113397084A CN202110373497.1A CN202110373497A CN113397084A CN 113397084 A CN113397084 A CN 113397084A CN 202110373497 A CN202110373497 A CN 202110373497A CN 113397084 A CN113397084 A CN 113397084A
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perillaldehyde
natural preservative
novel natural
emulsifier
preparation
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Inventor
张宁慧
秦雨昕
王颂恩
梁安琪
韩陆
程润庚
赵雨豪
李昕冉
田俊
夏雯
刘曼
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Jiangsu Normal University
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463Organic compounds; Microorganisms; Enzymes
    • A23L3/3481Organic compounds containing oxygen
    • A23L3/3499Organic compounds containing oxygen with doubly-bound oxygen
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/10Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/262Cellulose; Derivatives thereof, e.g. ethers
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Nutrition Science (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

A preparation method of a novel natural preservative based on perillaldehyde comprises the following steps: the method comprises the following steps: mixing 48.2% Span80 and 51.8% Tween20, adding 0.25% perillaldehyde, 3% emulsifier, 96.75% water, homogenizing and emulsifying at 50 deg.C to obtain perillaldehyde emulsifier, and mixing with 0.6% agar to obtain solid volatile agent of perillaldehyde. The natural preservative has the natural fragrance of the plant essential oil and good preservative effect, is milk white in color, cylindrical in shape, smooth in appearance and free of obvious particles, can give out faint scent to make people feel pleasurable, and can also play a role in preserving in a gas form.

Description

Novel natural preservative based on perillaldehyde and preparation method thereof
Technical Field
The invention relates to the technical field of natural preservative preparation, and particularly relates to a novel natural preservative preparation method based on perillaldehyde.
Background
Fungi and mycotoxin easily cause food, fruits, vegetables, traditional Chinese medicinal materials and the like to be mildewed and deteriorated, and about 10 hundred million tons of agricultural products are polluted by the fungi and the mycotoxin every year according to statistics of Food and Agricultural Organizations (FAO) of the United nations. The method not only causes huge resource waste and economic loss, but also brings potential safety hazards, seriously threatens the health and life safety of people, and has attracted global wide attention.
The plant essential oil and the active ingredients thereof have the characteristics of good antibacterial activity, good biodegradability, relative safety to human bodies and the like, can make up for some defects of chemical synthetic agents, are natural in origin, have low risk of generating drug resistance in pathogenic microorganisms, and can be used as one of important sources of natural preservatives.
The existing product is prepared from essential oil into water agent or missible oil, which brings inconvenience in storage, transportation and use. Therefore, the plant essential oil perillaldehyde is loaded into the gel matrix to prepare the emulsion agent, and the proper gel material with the specific reticular molecular structure is selected, so that the release of the perillaldehyde can be slowed down, and a good slow release effect is achieved. Solidifying a liquid substance is an ideal option, and not only can exert the activity of the liquid itself, but also can improve the economic benefit. The research idea of using the method for food preservation has high innovation at home and abroad.
Disclosure of Invention
The invention aims to provide a preparation method of a novel natural preservative based on perillaldehyde serving as a main component of perilla essential oil, and solves the technical problems that liquid essential oil is difficult to transport and store and chemical preservatives have large side effects.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a novel natural preservative based on perillaldehyde comprises the following specific steps:
s1: the value of Hydrophilic-Lipophilic Balance (RHLB) is initially screened by the spreading method. Calculating the HLB value after mixing the alternative perillaldehyde and the ingredients according to the proportion of various surfactants in the composition and the HLB value: HLB blend ═ h (WA × HLBA + WB × HLBB + WC × HLBC + …)/(WA + WB + WC + …).
S2: the emulsification method is an emulsification method for measuring the required HLB value of the perillaldehyde solution, namely actually measuring the stability of the emulsion under different HLB.
S3: screening the composite emulsifier and measuring the stability.
S4: selection of gel material and confirmation of optimal concentration.
S5: optimizing the preparation process conditions. A novel natural preservative based on perillaldehyde is prepared according to the RHLB value screened by the spreading method in the step S1, the HLB value measured by the emulsification method in the step S2, the optimal compound emulsifier measured in the step S3, the optimal gel material and the concentration determined in the step S4. Wherein, the concentration of the perillaldehyde is prepared to be 0.25 percent, the composite emulsifier is 48.2:51.8, the emulsifier is compounded to be 48.2 percent span80+51.8 percent tween20, and the concentration of the agar is 0.6 percent. Finally homogenizing and emulsifying at 50 deg.C.
Further, the step S1 specifically includes:
s1-1: selecting a pair of surfactants with larger HLB value difference to prepare a series of water solutions with HLB from high to low, dripping oil on the water surface, and preliminarily estimating the RHLB value of the perillaldehyde oil-water system by observing the spreading condition.
S1-2: when the HLB value is higher, oil drops can be spread completely, spreading becomes more and more difficult after HLB is reduced, and when the oil drops just do not spread and form one drop, the RHLB value can be obtained.
S1-3: this method is simple, but rough, and therefore only suitable for preliminary screening of RHLB values.
Further, the step S2 specifically includes:
s2-1: mixing emulsifiers with different HLB values, and adding the mixed emulsifiers into a perillaldehyde-water system.
S2-2: homogenizing and emulsifying the mixture in a high-speed disperser in a system, centrifuging, taking intermediate liquid, measuring the light absorption value of the intermediate liquid after gradient dilution, and determining the RHLB value according to the light absorption value.
Further, the step S3 specifically includes:
s3-1: different emulsifiers are selected to be compounded according to a certain formula and added into a perillaldehyde-water system for homogeneous emulsification.
S3-2: after centrifugation, the intermediate liquid is taken out, diluted and the light absorption value is measured. The formulation with the highest absorbance is the optimal mixed emulsifier formulation.
Further, the step S4 specifically includes:
s4-1: gel material of solid volatile agent is selected from carrageenan, carboxymethyl cellulose, agar, etc.
S4-2: the above materials were added to water.
S4-3: heating to form clear transparent liquid, cooling, observing the property after gelling, and determining the optimal concentration of the gel solution.
Further, the step S5 specifically includes:
s5-1: adding perillaldehyde into an emulsifier and distilled water, and homogenizing and emulsifying by using a homogenizer to obtain an oil/water type sample.
S5-2: selecting the composite emulsifier according to the main factors influencing the emulsion formation and stability of the emulsion, optimizing the experiment and determining the optimal preparation process.
Finally, canning and sealing to obtain the novel natural preservative finished product based on the perillaldehyde. The invention provides a novel natural preservative based on perillaldehyde prepared by the preparation method.
As a preferable technical scheme, before the RHLB is accurately measured, the perillaldehyde refined oil is dropped on the water surface, and the RHLB value of the perillaldehyde oil-water system is preliminarily estimated by observing the spreading condition.
TABLE 1 development of perillaldehyde on the surface of aqueous emulsifier solutions of different HLB values
Figure BDA0003010260240000031
As a preferable technical scheme, before the RHLB is accurately measured, the mixed reagent is homogenized and emulsified by a high-speed disperser, and gradient dilution is carried out.
TABLE 2 determination of the HLB value required for Perilla aldehyde solution by the emulsification method
Figure BDA0003010260240000032
As a preferred technical scheme, the steps of screening the composite emulsifier and determining the stability specifically comprise: adding the prepared composite emulsifier into a perillaldehyde-water system for homogeneous emulsification.
TABLE 3 formulation of the Complex emulsifiers
Figure BDA0003010260240000033
TABLE 4 screening of Complex emulsifiers and determination of stability
Figure BDA0003010260240000034
According to a preferable technical scheme, the gel material is heated on the basis of material selection to form clear and transparent liquid, the gel material is cooled, the property after gelling is observed, and the optimal gel solution concentration is determined.
As a preferred technical scheme, the preparation process is optimized.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the agar is used as a carrier, and the perillaldehyde essential oil is added into the agar to be fused, so that the effect of better slowly releasing the effective components of the plant essential oil can be achieved.
2. The novel natural preservatives prepared by the present invention not only improve food safety by eliminating fungal transmission, but also do not leave detectable residues after storage.
3. The novel natural preservative is developed by taking the plant essential oil perillaldehyde as a raw material for the first time, so that the development degree of the plant essential oil is improved, the application range of the plant essential oil is widened, and the prospect is good.
4. The invention enriches the variety of preservatives, solves the problems of residual toxicity to human body, great harm to environment, low nutrition value, difficult transportation and storage of liquid essential oil and the like of the traditional chemical preservatives after being used excessively, and is particularly suitable for people who have requirements on dispelling the effects of alcohol and protecting the liver.
Detailed Description
The following is a detailed description of specific embodiments.
A preparation method of a novel natural preservative based on perillaldehyde comprises the following steps:
1. initial screening RHLB value by spreading method
Calculating the HLB value after mixing the alternative perillaldehyde and the ingredients according to the proportion of various surfactants in the composition and the HLB value:
HLB blend ═ h (WA × HLBA + WB × HLBB + WC × HLBC + …)/(WA + WB + WC + …).
S1-1: selecting a pair of surfactants with larger HLB value difference to prepare a series of water solutions with HLB from high to low, dripping oil on the water surface, and preliminarily estimating the RHLB value of the perillaldehyde oil-water system by observing the spreading condition.
S1-2: when the HLB value is higher, oil drops can be spread completely, spreading becomes more and more difficult after HLB is reduced, and when the oil drops just do not spread and form one drop, the RHLB value can be obtained.
S1-3: this method is simple, but rough, and therefore only suitable for preliminary screening of RHLB values.
2. Emulsification method for determining required HLB (hydrophile-lipophile balance) value of perillaldehyde solution by emulsification method
S2-1: mixing emulsifiers with different HLB values, and adding the mixed emulsifiers into a perillaldehyde-water system.
S2-2: homogenizing and emulsifying the mixture in a high-speed disperser in a system, centrifuging, taking intermediate liquid, measuring the light absorption value of the intermediate liquid after gradient dilution, and determining the RHLB value according to the light absorption value.
3. Screening the composite emulsifier and measuring the stability.
S3-1: different emulsifiers are selected to be compounded according to a certain formula and added into a perillaldehyde-water system for homogeneous emulsification.
S3-2: after centrifugation, the intermediate liquid is taken out, diluted and the light absorption value is measured. The formulation with the highest absorbance is the optimal mixed emulsifier formulation.
4. Selection of gel material and confirmation of optimal concentration.
S4-1: gel material of solid volatile agent is selected from carrageenan, carboxymethyl cellulose, agar, etc.
S4-2: the above materials were added to water.
S4-3: heating to form clear transparent liquid, cooling, observing the property after gelling, and determining the optimal concentration of the gel solution.
5. Optimizing the preparation process conditions. The formula of the solid propellant is as follows: alternative perillaldehyde, emulsifier, gel, and distilled water. Then, the influence of the factors and the level thereof on the quality of the solid volatile agent is examined.
S5-1: adding perillaldehyde into an emulsifier and distilled water, and homogenizing and emulsifying by using a homogenizer to obtain an oil/water type sample.
S5-2: selecting the composite emulsifier according to the main factors influencing the emulsion formation and stability of the emulsion, optimizing the experiment and determining the optimal preparation process.
6. Finally, canning and sealing to obtain the novel natural preservative finished product based on the perillaldehyde.
The novel natural preservative product is prepared by the preparation scheme of the novel natural preservative based on perillaldehyde, and orthogonal experimental design is carried out on 4 factors and 3 levels (the temperature is 40 ℃, 50 ℃ and 60 ℃, the volatile oil content is 0.05%, 0.25% and 0.75%, the HLB value is 10.72, 10.816 and 10.934, and the emulsifier content is 2%, 2.5% and 3%).
TABLE 5 orthogonal test factor horizon
Figure BDA0003010260240000052
TABLE 6 results of orthogonal experiments
Figure BDA0003010260240000053
The results of orthogonal experiments show that:
the optimal HLB value of the compound emulsifier is 10.72, namely, the compound emulsifier is prepared by compounding 48.2 percent of Span80 (Span 80) and 51.8 percent of Tween20 (Tween 20). Then, the emulsifier with the perillaldehyde concentration of 0.25%, the emulsifier concentration of 3% and the water with the water content of 96.75% is preferably selected and is obtained by homogeneous emulsification at the temperature of 50 ℃. And mixing with 0.6% agar to obtain solid volatile agent of perillaldehyde. Any modification, equivalent replacement or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (6)

1. A preparation method of a novel natural preservative based on perillaldehyde is characterized by comprising the following steps:
mixing 0.05-0.75% of perillaldehyde, 2-3% of emulsifier and double distilled water at 40-60 deg.C, homogenizing and emulsifying to obtain perillaldehyde emulsion; then mixing with 0.12% -1.8% agar to obtain the novel natural preservative based on perillaldehyde.
2. The method for preparing the novel natural preservative based on the perillaldehyde according to claim 1, wherein the mass ratio of Span80 to Tween20 in the emulsifier is 1-15: 4-1.
3. The method for preparing the novel natural preservative based on the perillaldehyde according to claim 2, wherein the mass ratio of the Span80 to the Tween20 is 48.2: 51.8.
4. the method for preparing a novel natural preservative based on perillaldehyde according to claim 1, wherein the temperature of the homogeneous emulsification is 50 ℃.
5. The method of preparing a novel natural preservative based on perillaldehyde according to claim 1, wherein the mass percentage of agar is 0.6%.
6. A novel natural preservative prepared by the process of any one of the preceding claims.
CN202110373497.1A 2021-04-07 2021-04-07 Novel natural preservative based on perillaldehyde and preparation method thereof Pending CN113397084A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002097302A (en) * 2000-09-22 2002-04-02 Fumakilla Ltd Aqueous gel composition
CN101181266A (en) * 2007-11-26 2008-05-21 沈阳药科大学 Biphenyl benzyl azoles emulsion agent and preparation method thereof
CN102648922A (en) * 2011-02-23 2012-08-29 深圳市嘉轩医药科技发展有限公司 Gamuzhuer medicinal latex preparation and preparation method thereof
CN102860330A (en) * 2012-10-09 2013-01-09 武汉大学 Dill seed volatile-oil fragrant mildewcide and preparation method and application thereof
CN108546590A (en) * 2018-04-20 2018-09-18 湖南农业大学 Application process of Fructus Perillae quintessence oil during citrus storage at normal temperature

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002097302A (en) * 2000-09-22 2002-04-02 Fumakilla Ltd Aqueous gel composition
CN101181266A (en) * 2007-11-26 2008-05-21 沈阳药科大学 Biphenyl benzyl azoles emulsion agent and preparation method thereof
CN102648922A (en) * 2011-02-23 2012-08-29 深圳市嘉轩医药科技发展有限公司 Gamuzhuer medicinal latex preparation and preparation method thereof
CN102860330A (en) * 2012-10-09 2013-01-09 武汉大学 Dill seed volatile-oil fragrant mildewcide and preparation method and application thereof
CN108546590A (en) * 2018-04-20 2018-09-18 湖南农业大学 Application process of Fructus Perillae quintessence oil during citrus storage at normal temperature

Non-Patent Citations (2)

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Title
TAMER M. SHEHATA: "Curcumin Niosomes Prepared from Proniosomal Gels: In Vitro Skin Permeability, Kinetic and In Vivo Studies", POLYMERS, 4 April 2021 (2021-04-04), pages 1 - 14 *
章勇: "桂皮醛亚微乳的制备及抗关节炎作用研究", 优秀硕士学位论文数据库, 15 March 2021 (2021-03-15), pages 9 - 11 *

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