CN114410420A - Preparation method of mature vinegar containing spice essential oil nano emulsion - Google Patents
Preparation method of mature vinegar containing spice essential oil nano emulsion Download PDFInfo
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- CN114410420A CN114410420A CN202210048182.4A CN202210048182A CN114410420A CN 114410420 A CN114410420 A CN 114410420A CN 202210048182 A CN202210048182 A CN 202210048182A CN 114410420 A CN114410420 A CN 114410420A
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- C12J—VINEGAR; PREPARATION OR PURIFICATION THEREOF
- C12J1/00—Vinegar; Preparation or purification thereof
Abstract
The invention discloses a preparation method of mature vinegar containing spice essential oil nano emulsion, belonging to the technical field of seasoning processing. The invention prepares the spice essential oil into stable, clear and transparent O/W type nano emulsion by an efficient nano emulsification technology, then adds the nano emulsion into mature vinegar, uses a magnetic stirrer to stir uniformly to obtain a semi-finished product, fills and seals the prepared semi-finished product mature vinegar in an aseptic state, and performs ultraviolet irradiation sterilization to obtain a finished product. The invention solves the limitation of the application of the essential oil in water-soluble products, the spice essential oil nanoemulsion prepared by the method has safe preparation raw materials, simple and convenient preparation method, easy mass production and wide application in food bacteriostasis and corrosion prevention; the spice essential oil is prepared into the nano emulsion for mature vinegar, so that the quality change of the mature vinegar can be reduced, and the mature vinegar with specific flavor can be prepared.
Description
Technical Field
The invention belongs to the technical field of seasoning processing, and particularly relates to a preparation method of mature vinegar containing spice essential oil nano emulsion.
Background
Plant essential oil is a secondary metabolite of plants, and the application of the essential oil in the food industry is limited due to low water solubility, dense flavor and high volatility. A nanoemulsion is an isotropic, thermodynamically stable colloidal dispersion. Thus, nanoemulsions may be an alternative in order to enhance the dispersion of essential oils in water and to prevent degradation of the essential oils.
The food-grade nano emulsion can prevent functional nutrient components from being oxidized, and improve the water solubility and the bioavailability of the functional nutrient components. In addition, the emulsion embedding technology can reduce the inherent flavor of the essential oil to a certain extent, so that the essential oil is more easily accepted by consumers, and the unstable phenomena of sedimentation, flocculation and the like in the storage process can be greatly reduced in the application process, so that the essential oil is widely applied as a drug carrier. The formation of the nanoemulsion requires external supply of mechanical energy. At present, the preparation method of the nano emulsion comprises two main types of high-energy emulsification methods and low-energy emulsification methods, and a high-pressure homogeneous emulsification technology is taken as a commonly used high-energy method for preparing the nano emulsion.
The spice in the existing special flavor seasoning is easy to reduce the sensory quality of mature vinegar, and is easy to generate precipitation and flocculation in the shelf life to cause layering, thereby bringing bad consumption experience to consumers and shortening the shelf life. Therefore, the development of a preparation method of mature vinegar with specific flavor and long-term stability is of great significance.
In recent years, plant essential oils of natural origin have attracted much attention as antibacterial substances. The spice essential oil is mainly used for highlighting different tastes of various delicious foods in foods, and can also be used for preparing anesthetics, insecticides and bactericides and the like in the aspects of medicine and industry. The stability and water solubility of the essential oil are improved by preparing the essential oil into the oil-in-water type nano emulsion, so that the applicability of the essential oil in the flavoring is enhanced.
Disclosure of Invention
The invention aims to provide a preparation method of mature vinegar containing spice essential oil nano emulsion. Preparing the spice essential oil into stable, clear and transparent O/W type nano emulsion by a high-efficiency nano emulsification technology, then adding the nano emulsion into mature vinegar, uniformly stirring by using a magnetic stirrer to obtain a semi-finished product, filling and sealing the prepared semi-finished product mature vinegar in an aseptic state, and performing ultraviolet irradiation sterilization to obtain a finished product.
The technical scheme of the invention is as follows:
a preparation method of mature vinegar containing spice essential oil nano emulsion mainly comprises the following preparation steps:
(1) preparation of a crude emulsion: uniformly mixing the spice essential oil and the emulsifier by adopting an in-oil method, adding deionized water, and fully stirring to obtain a coarse emulsion;
(2) preparing the nano emulsion: treating the coarse emulsion obtained in the step (1) by a high-energy emulsification method, and finally cooling by an ice-water bath to obtain the spice essential oil nano emulsion;
(3) mature vinegar blending: adding the spice essential oil nano emulsion prepared in the step (2) into mature vinegar according to a proportion, wherein the addition amount of the spice essential oil nano emulsion is 1% -3% of the total volume of the product, and uniformly stirring by using a magnetic stirrer to obtain a semi-finished product;
(4) and (3) sterilization: and filling and sealing the prepared semi-finished mature vinegar in an aseptic state, and sterilizing for 1-2h by ultraviolet irradiation to obtain a finished product.
The emulsifier in the step (1) is composed of tween 60(T-60) and polyglycerol fatty acid ester (PGFE), wherein the weight ratio of T-60: PGFE ═ 2: 1.
the spice essential oil, the emulsifier and the deionized water respectively account for 3-5%, 2-15% and 80-95% of the total mass of the nano emulsion.
The high-energy emulsification method is an ultrahigh-pressure homogenization method, and the specific conditions are as follows: 50MPa pressure, cycle number 4.
And (3) in the step (2), the temperature of the ice water bath is 5 ℃, and the time is 30 min.
The spice essential oil is ginger essential oil, pepper essential oil and the like.
The invention has the beneficial effects that:
1. the invention adopts a high-energy emulsification method to prepare the spice essential oil nanoemulsion, so that spice essential oil is used as an oil phase, T-60 and PGFE are selected as emulsifiers, and the spice essential oil nanoemulsion is prepared by the high-energy emulsification method, so that the spice essential oil nanoemulsion has long-term storage stability, the grain size distribution, PDI (Poly-lactic acid) and Zeta potential and the like of the spice essential oil nanoemulsion are not obviously changed after being stored for 60 days, and the turbidity is not obviously changed; and secondly, the essential oil nano emulsion has higher stability in different application scenes. The system increases the water solubility of the spice essential oil, and is beneficial to inhibiting bacteria; meanwhile, the strong volatility and instability of the spice essential oil are avoided through high-energy emulsification.
2. The spice essential oil nano-emulsion prepared by the invention has safe preparation raw materials, does not relate to toxic materials, has simple and convenient preparation method, is easy for large-scale production, and can be widely used for food bacteriostasis and corrosion prevention.
3. The spice essential oil is prepared into the nano emulsion for mature vinegar, so that the quality change of the mature vinegar can be reduced, and the mature vinegar with specific flavor can be prepared.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below.
FIG. 1 is a graph showing the changes of the prepared pepper essential oil nanoemulsion before and after storage at different temperatures.
FIG. 2 is a graph showing the storage of mature vinegar at different temperatures before and after addition of the nanoemulsion.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention is further illustrated below with reference to specific examples.
Example 1: preparation method of mature vinegar containing ginger essential oil nano emulsion
The method mainly comprises the following steps:
(1) preparing an emulsifier: mixing T-60 and PGFE proportionally, and taking 15% of the total mass of the emulsion.
(2) Preparation of a crude emulsion: uniformly mixing 5% of ginger essential oil and 15% of emulsifier by adopting an in-oil method, adding 80% of deionized water, and fully stirring to obtain a coarse emulsion;
(3) and (3) treating the crude emulsion obtained in the step (2) by a high-energy emulsification method, homogenizing and circulating for 4 times under the pressure of 50MPa, and finally cooling by an ice-water bath (30min) to obtain the uniform, stable, clear and transparent ginger essential oil nano emulsion.
(4) Mature vinegar blending: adding the ginger essential oil nano emulsion according to a proportion, wherein the addition amount of the ginger essential oil nano emulsion is 1% of the total volume of the product, and uniformly stirring by a magnetic stirrer to obtain a semi-finished product.
(5) And filling and sealing the prepared semi-finished mature vinegar in an aseptic state, and sterilizing for 1h by ultraviolet irradiation to obtain a finished product.
Example 2: preparation method of mature vinegar containing pepper essential oil nano emulsion
The method mainly comprises the following steps:
(1) preparing an emulsifier: mixing T-60 and PGFE proportionally, and taking 12% of the total mass of the emulsion.
(2) Preparation of a crude emulsion: uniformly mixing 4% of pepper essential oil and 12% of emulsifier by adopting an in-oil method, adding 84% of deionized water, and fully stirring to obtain a coarse emulsion;
(3) and (3) treating the crude emulsion obtained in the step (2) by a high-energy emulsification method, homogenizing and circulating for 4 times under the pressure of 50MPa, and finally cooling by an ice water bath (30min) to obtain the uniform, stable, clear and transparent pepper essential oil nano emulsion.
(4) Mature vinegar blending: adding the obtained pepper essential oil nano emulsion according to a proportion, wherein the adding amount of the pepper essential oil nano emulsion is 1% of the total volume of the product, and uniformly stirring the mixture by using a magnetic stirrer to obtain a semi-finished product.
(5) And filling and sealing the prepared semi-finished mature vinegar in an aseptic state, and sterilizing for 1h by ultraviolet irradiation to obtain a finished product.
Example 3: preparation method of mature vinegar containing pepper essential oil nano emulsion
The method mainly comprises the following steps:
(1) preparing an emulsifier: mixing T-60 and PGFE at a ratio of 2:1, and collecting 8% of the total weight of the emulsion.
(2) Preparation of a crude emulsion: fully stirring 3% of pepper essential oil, 8% of compound emulsifier and 89% of deionized water by adopting a method of using a preparation in oil to obtain a coarse emulsion;
(3) and (3) treating the crude emulsion obtained in the step (2) by a high-energy emulsification method, homogenizing and circulating for 4 times under the pressure of 50MPa, and finally cooling by an ice water bath (30min) to obtain the uniform, stable, clear and transparent pepper essential oil nano emulsion.
(4) Mature vinegar blending: adding the obtained pepper essential oil nano emulsion according to a proportion, wherein the addition amount of the pepper essential oil nano emulsion is 1% of the total volume of the product, and uniformly stirring by a magnetic stirrer to obtain a semi-finished product.
(5) And filling and sealing the prepared semi-finished mature vinegar in an aseptic state, and sterilizing for 1h by ultraviolet irradiation to obtain a finished product.
Example 4: preparation method of mature vinegar containing pepper essential oil nano emulsion
(1) Selecting pepper essential oil as an oil phase, selecting T-60 and PGFE as emulsifiers, uniformly compounding the emulsifiers in proportion, adding spice essential oil, and uniformly stirring by a magnetic stirrer for later use;
(2) adding a certain amount of mature vinegar obtained in the step (1), and shearing at a high speed of 10000r/min for 3min to obtain a coarse emulsion;
(3) pouring the crude emulsion into an ultrahigh pressure homogenizer, and homogenizing under 40MPa and circulating for 3 times to obtain half-finished mature vinegar with pepper flavor;
(4) and (4) filling and sealing the obtained product in the step (3) in an aseptic state, and sterilizing by ultraviolet irradiation to obtain a finished product.
Control group: the purchased mature vinegar is used as a blank control group without adding the pepper essential oil nano emulsion and carrying out homogenization treatment, and other preparation methods are the same as the examples.
The stability and application stability of the pepper essential oil nanoemulsion in example 3 were examined:
the grain size, the centrifugal stability rate and the Zeta potential of the spice essential oil nano emulsion prepared in example 3 were measured by a Zeta potential and nano-particle size analyzer after being placed for 2 months at day 0 and normal temperature, and the results showed that the average grain size, the centrifugal stability rate, the Zeta potential and the polydispersity index (PDI) of the nano emulsion before and after being placed were not significantly different, and the emulsion was clear and transparent, i.e., the emulsion had better storage stability.
The prepared pepper essential oil nano emulsion is applied to mature vinegar, and storage acceleration experiments show that the storage property of the mature vinegar can be improved by adding the nano emulsion. The mature vinegar added with the nano emulsion has good storage stability, and the turbidity of the sample does not change obviously in the storage process, and the phenomena of flocculation, aggregation, precipitation and the like do not occur. The turbidity, color, eccentricity and oxidation resistance (reducing power and DPPH free radical clearance) of the vinegar are all superior to those of the mature vinegar without the nano emulsion.
And (3) measuring the turbidity of the sample: the sample was diluted 10 times and measured with an ultraviolet spectrophotometer at 600 nm. Table 1 is a comparison of turbidity of mature vinegar stored for 2 months before and after addition of nanoemulsion. The result shows that the turbidity of the sample increases along with the temperature increase, as shown in figure 1, the state of the pepper essential oil nanoemulsion stored for 60 days at different temperatures is shown, and the storage for 60 days at 25 ℃ has no significant difference from the fresh emulsion. At the same temperature, the turbidity change of the sample added with the nano emulsion is smaller than that of the sample without the nano emulsion, as shown in fig. 2, the difference of the clarity before and after the nano emulsion is added is shown, namely, the addition of the nano emulsion can reduce the quality change of the mature vinegar.
TABLE 1 comparison of turbidity at different storage temperatures and times of mature vinegar addition nanoemulsion
And (3) measuring the color of the sample: the sample was diluted 10-fold and measured using a colorimeter. As a result, as shown in Table 2, the color change of mature vinegar was suppressed by adding the nanoemulsion.
TABLE 2 comparison of color of mature vinegar with nano emulsion added at different storage temperatures and times
Sample eccentricity determination: the sample is diluted by 10 times, centrifuged for 30min at 2000g in a high-speed centrifuge, and the absorbance before and after centrifugation is measured at 500nm of an ultraviolet spectrophotometer. As shown in Table 3, the eccentricity of the mature vinegar with the added nanoemulsion after being stored for 60 days at room temperature is 29.32%, which is smaller than the eccentricity without the added nanoemulsion, i.e. the nanoemulsion enables the mature vinegar to be more stable in the storage process.
TABLE 3 comparison of the eccentricity of mature vinegar storage for 2 months before and after addition of nanoemulsion
Determination of antioxidant capacity: the change in DPPH clearance of mature vinegar stored for 60 days before and after addition of nanoemulsion was determined. DPPH free radical clearance is determined after dilution of the sample by a factor of 20. The results are shown in table 4, the antioxidant capacity of the mature vinegar can be remarkably improved by adding the nano emulsion, and the DPPH free radical clearance of the mature vinegar containing the nano emulsion is obviously higher than that of a sample without adding the nano emulsion under the same storage time and storage temperature.
TABLE 4 comparison of DPPH radical scavenging Rate of mature Vinegar storage for 2 months before and after addition of nanoemulsion
Claims (6)
1. A preparation method of mature vinegar containing spice essential oil nano emulsion is characterized by mainly comprising the following preparation steps:
(1) preparation of a crude emulsion: uniformly mixing the spice essential oil and the emulsifier by adopting an in-oil method, adding deionized water, and fully stirring to obtain a coarse emulsion;
(2) preparing the nano emulsion: treating the coarse emulsion obtained in the step (1) by a high-energy emulsification method, and finally cooling by an ice-water bath to obtain the spice essential oil nano emulsion;
(3) mature vinegar blending: adding the spice essential oil nano emulsion prepared in the step (2) into mature vinegar according to a proportion, wherein the addition amount of the spice essential oil nano emulsion is 1% -3% of the total volume of the product, and uniformly stirring by using a magnetic stirrer to obtain a semi-finished product;
(4) and (3) sterilization: and filling and sealing the prepared semi-finished mature vinegar in an aseptic state, and sterilizing for 1-2h by ultraviolet irradiation to obtain a finished product.
2. The method for preparing mature vinegar containing spice essential oil nano-emulsion according to claim 1, wherein the emulsifier in the step (1) is composed of tween 60(T-60) and polyglycerol fatty acid ester (PGFE), wherein the ratio of T-60: PGFE ═ 2: 1.
3. the method for preparing mature vinegar containing spice essential oil nano-emulsion according to claim 1, wherein the spice essential oil, the emulsifier and the deionized water respectively account for 3-5%, 2-15% and 80-95% of the total mass of the nano-emulsion.
4. The method for preparing the mature vinegar containing the spice essential oil nano-emulsion according to claim 1, wherein the high-energy emulsification method is an ultrahigh-pressure homogenization method, and the specific conditions are as follows: 50MPa pressure, cycle number 4.
5. The method for preparing mature vinegar containing spice essential oil nano-emulsion according to claim 1, wherein the temperature of the ice water bath in the step (2) is 5 ℃ and the time is 30 min.
6. The method for preparing mature vinegar containing spice essential oil nano-emulsion according to claim 1, wherein the spice essential oil is ginger essential oil, pepper essential oil and the like.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6077559A (en) * | 1998-04-27 | 2000-06-20 | Mccormick & Company, Incorporated | Flavored oil-in-vinegar microemulsion concentrates, method for preparing the same, and flavored vinegars prepared from the same |
| JP2005200393A (en) * | 2004-01-16 | 2005-07-28 | Polysis:Kk | Creamy composition of bamboo vinegar (chikusaku-eki) |
| US20130064954A1 (en) * | 2011-09-08 | 2013-03-14 | Maria Ochomogo | Microemulsion Concentrates and Nanoemulsion Flavorant Compositions For Food Applications |
| CN105053938A (en) * | 2015-09-07 | 2015-11-18 | 江南大学 | Preparation method for seasoning fragrance-enhanced cooking wine |
| CN109497497A (en) * | 2018-12-20 | 2019-03-22 | 四川大学 | A kind of Chinese prickly ash flavor soy sauce and preparation method thereof |
| CN112273433A (en) * | 2020-11-30 | 2021-01-29 | 吉林大学 | Preparation method and application of chitosan-based butyl essential oil nanoemulsion |
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- 2022-01-17 CN CN202210048182.4A patent/CN114410420A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6077559A (en) * | 1998-04-27 | 2000-06-20 | Mccormick & Company, Incorporated | Flavored oil-in-vinegar microemulsion concentrates, method for preparing the same, and flavored vinegars prepared from the same |
| JP2005200393A (en) * | 2004-01-16 | 2005-07-28 | Polysis:Kk | Creamy composition of bamboo vinegar (chikusaku-eki) |
| US20130064954A1 (en) * | 2011-09-08 | 2013-03-14 | Maria Ochomogo | Microemulsion Concentrates and Nanoemulsion Flavorant Compositions For Food Applications |
| CN105053938A (en) * | 2015-09-07 | 2015-11-18 | 江南大学 | Preparation method for seasoning fragrance-enhanced cooking wine |
| CN109497497A (en) * | 2018-12-20 | 2019-03-22 | 四川大学 | A kind of Chinese prickly ash flavor soy sauce and preparation method thereof |
| CN112273433A (en) * | 2020-11-30 | 2021-01-29 | 吉林大学 | Preparation method and application of chitosan-based butyl essential oil nanoemulsion |
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