CN111085142A

CN111085142A - Orange oil nano dispersion, preparation method thereof, transparent beverage and detergent

Info

Publication number: CN111085142A
Application number: CN201911298833.XA
Authority: CN
Inventors: 刘能; 黄宏军; 马银杰; 李靖娥
Original assignee: Dongguan Boton Flavors & Fragrances Co ltd
Current assignee: Botton Spices Co ltd
Priority date: 2019-12-16
Filing date: 2019-12-16
Publication date: 2020-05-01
Anticipated expiration: 2039-12-16
Also published as: CN111085142B

Abstract

The invention relates to a sweet orange oil nano dispersion, a preparation method thereof, a transparent beverage and a detergent. The preparation process of the sweet orange oil nano dispersion comprises the following steps: removing terpene from sweet orange oil to obtain de-terpened sweet orange oil; mixing the de-terpened sweet orange oil with a protein solution, homogenizing, and adjusting pH to be alkaline to obtain a mixed solution; and adding the propylene glycol alginate solution into the mixed solution for reaction to obtain the sweet orange oil nano dispersion. The preparation method of the sweet orange oil nano dispersion can be used for preparing the transparent, uniformly dispersed and good-stability sweet orange oil nano dispersion.

Description

Orange oil nano dispersion, preparation method thereof, transparent beverage and detergent

Technical Field

The invention relates to a sweet orange oil nano dispersion, a preparation method thereof, a transparent beverage and a detergent.

Background

The sweet orange oil is obtained by cold grinding, cold pressing, steam distillation, and CO₂The sweet orange juice is prepared from sweet orange fruits or sweet orange peels by processes such as a supercritical extraction method, contains various volatile components, is fresh and sweet, is fresh and natural, and is widely applied to food, daily chemicals and tobacco.

The traditional micron-sized sweet orange oil microcapsule solution is in a turbid state, is not suitable for transparent beverages, is unstable in application in detergents and is easy to have a poor layering phenomenon.

Disclosure of Invention

Based on this, there is a need for a method for preparing a sweet orange oil nano-dispersion which can make the prepared sweet orange oil nano-dispersion transparent and has good stability.

In addition, the sweet orange oil nano dispersant, transparent beverage and detergent are also provided.

A preparation method of a sweet orange oil nano dispersion comprises the following steps:

removing terpene from sweet orange oil to obtain de-terpened sweet orange oil;

mixing the de-terpened sweet orange oil with a protein solution, homogenizing, and adjusting the pH value to be alkaline to obtain a mixed solution; and

and adding the propylene glycol alginate solution into the mixed solution for reaction to obtain the sweet orange oil nano dispersion.

In one embodiment, the method further comprises the following steps: and centrifuging the sweet orange oil nano dispersion to remove micron-sized dispersion, and taking supernatant to obtain the purified sweet orange oil nano dispersion.

In one embodiment, in the step of centrifuging the sweet orange oil nano-dispersion, the centrifugation speed is 10000rpm to 15000rpm, and the centrifugation time is 30min to 50 min.

In one embodiment, the sweet orange oil is subjected to terpene removal by molecular distillation under the following conditions: the temperature of molecular distillation is 30-50 ℃, the distillation pressure is 120-350 Pa, the feeding speed is 1.0-3.5 mL/min, and the scraper rotating speed is 150-300 r/min.

In one embodiment, the protein solution comprises protein and water, the protein is selected from at least one of soy protein, whey protein, gelatin and wheat protein; and/or the presence of a catalyst in the reaction mixture,

the concentration of the protein solution is 0.5 mg/mL-3.0 mg/mL, and the volume ratio of the de-terpenoid sweet orange oil to the protein solution is 1: 180-1: 20.

In one embodiment, the homogenization treatment step is performed at a homogenization pressure of 10000 psi-20000 psi for 2-3 times of cyclic homogenization; and/or the presence of a catalyst in the reaction mixture,

and in the step of adjusting the pH to be alkaline, adjusting the pH to be 8.5-10.5.

In one embodiment, the esterification degree of the propylene glycol alginate is 88 to 99 percent; and/or the presence of a catalyst in the reaction mixture,

the concentration of the propylene glycol alginate solution is 0.1 mg/mL-0.5 mg/mL, and the volume ratio of the propylene glycol alginate solution to the mixed solution is 1: 120-1: 10; and/or the presence of a catalyst in the reaction mixture,

the time for adding the propylene glycol alginate solution into the mixed solution to react is 0.5 to 1.5 hours.

The sweet orange oil nano dispersion is prepared by the preparation method of the sweet orange oil nano dispersion.

A transparent beverage comprises the above sweet orange oil nano-dispersion.

In one embodiment, the transparent beverage further comprises 5-15% of sweetening agent and 0.08-0.50% of sour agent by mass percentage.

A detergent comprising the above sweet orange oil nanodispersion.

In one embodiment, the detergent further comprises 5-12% of fatty alcohol-polyoxyethylene ether, 15-25% of ethoxylated sodium alkyl sulfate and 3-8% of ethylene diamine tetraacetic acid disodium salt by mass percentage.

The terpene components in the sweet orange oil contribute little to the fragrance of the sweet orange oil and are easy to oxidize and deteriorate, so that the sweet orange oil is deteriorated, the water solubility of the terpene components is high, and if the content of the terpene components in the sweet orange oil is high, an emulsion prepared subsequently is easy to generate an austenite curing phenomenon, so that a stable emulsion is difficult to form, and the nano dispersion is not favorable to obtain. The preparation method of the sweet orange oil nano dispersion removes terpenes from the sweet orange oil, so that the sweet orange oil is not easy to deteriorate, and the subsequent formation of stable emulsion by the sweet orange oil and protein solution and the like is facilitated, thereby facilitating the preparation of the nano dispersion. And then mixing and homogenizing the de-terpened sweet orange oil and the protein solution to enable the sweet orange oil to be nanocrystallized, adjusting the pH value to be alkaline, enabling the protein to react with propylene glycol alginate under the alkaline condition to form gel and serve as a wall material to embed the sweet orange oil, and thus obtaining a nano dispersion body which is uniformly dispersed, and the nano dispersion body can not be layered after being placed for a long time. And the sweet orange oil nano dispersion is liquid and transparent, does not affect the appearance of the beverage or detergent when applied to the beverage or the detergent, and can be quickly and uniformly dispersed. Therefore, the preparation method of the sweet orange oil nano dispersion can prepare the transparent and high-stability sweet orange oil nano dispersion.

Drawings

FIG. 1 is a process flow diagram of one embodiment of a method for making a nano-dispersion of sweet orange oil;

fig. 2 is a particle size distribution diagram of the nano-dispersion of sweet orange oil prepared in example 1.

Detailed Description

In order that the invention may be more fully understood, reference will now be made to the following description taken in conjunction with the accompanying drawings. The detailed description sets forth the preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

Referring to fig. 1, a method for preparing a nano-dispersion of sweet orange oil according to an embodiment includes the following steps:

step S110: and (3) carrying out terpene removal on the sweet orange oil to obtain the de-terpened sweet orange oil.

In the present embodiment, the sweet orange oil is subjected to terpene removal by molecular distillation. Specifically, sweet orange oil is filled into a sample injection bottle of short-path molecular distillation equipment for molecular distillation, and distillate is collected to obtain the de-terpened sweet orange oil.

In one embodiment, the conditions of the molecular distillation are: the temperature of molecular distillation is 30-50 ℃, the distillation pressure is 120-350 Pa, the feeding speed is 1.0-3.5 mL/min, and the scraper rotating speed is 150-300 r/min. The content of terpenes in the sweet orange oil is as high as about 95 percent, the terpene contributes little to the fragrance of the sweet orange oil, and the sweet orange oil is easy to oxidize and deteriorate, so that the sweet orange oil is deteriorated. In the embodiment, the terpene content in the sweet orange oil can be effectively reduced through a molecular distillation process, the enrichment of the characteristic aroma components of the sweet orange oil is realized, the aroma of the sweet orange oil after the terpene removal is pure, the sweet orange oil is not easy to deteriorate, and the stability of the sweet orange oil is improved.

In addition, the terpene components have high water solubility, and if the content of the terpene components in the sweet orange oil is high, the subsequently prepared emulsion is easy to generate an austenite curing phenomenon, so that a stable emulsion is difficult to form, and the nano dispersion is not easy to obtain. The preparation method of the sweet orange oil nano dispersion removes terpenes from the sweet orange oil, so that the sweet orange oil is not easy to deteriorate, and the subsequent formation of stable emulsion by the sweet orange oil and protein solution and the like is facilitated, thereby facilitating the preparation of the nano dispersion.

Step S120: mixing the de-terpened sweet orange oil with the protein solution, homogenizing, and adjusting pH to alkalinity to obtain a mixed solution.

Wherein the protein solution comprises protein and water. The protein is at least one selected from soybean protein, whey protein, gelatin and wheat protein. Specifically, the concentration of the protein in the protein solution is 0.5mg/mL to 3.0 mg/mL. The volume ratio of the de-terpened sweet orange oil to the protein solution is 1: 180-1: 20.

Specifically, in the step of homogenizing, a microfluid ultrahigh pressure homogenizer is used for homogenizing. Further, in the step of homogenizing treatment, the homogenizing pressure is 10000 psi-20000 psi, and the number of times of circulating homogenization is 2-3 times. The ultra-high pressure homogenization treatment can ensure that the de-terpened sweet orange oil and the protein are uniformly dispersed.

Further, in the step of adjusting the pH to be alkaline, the pH is adjusted to be 8.5-10.5. The propylene glycol alginate and the protein have better binding capacity, and in a weakly alkaline environment, amino groups which are not charged in the protein and mannose residues generate a cross-linking reaction to generate amido bonds, so that a gel with a high melting point is quickly formed. Therefore, the orange oil nano-dispersion can be prepared by taking the propylene glycol alginate and the protein as wall materials.

Step S130: and adding the propylene glycol alginate solution into the mixed solution for reaction to obtain the sweet orange oil nano dispersion.

Wherein the propylene glycol alginate solution is an aqueous solution of propylene glycol alginate. The esterification degree of the propylene glycol alginate is 88 to 99 percent. Specifically, the concentration of the propylene glycol alginate solution is 0.1 mg/mL-0.5 mg/mL. The volume ratio of the propylene glycol alginate solution to the mixed solution is 1: 120-1: 10.

The propylene glycol alginate is a water-soluble high polymer material, and has two groups of hydrophilicity and lipophilicity in a molecular structure, so that the propylene glycol alginate has emulsifying property, acid resistance and stability. The propylene glycol alginate and the protein have better binding capacity, and in a weakly alkaline environment, amino groups which are not charged in the protein and mannose residues generate a cross-linking reaction to generate amido bonds, so that a gel with a high melting point is quickly formed. Because the reaction of the propylene glycol alginate and the protein is fast under the alkaline condition, the speed of adding the propylene glycol alginate into the mixed solution is slow, the reaction is carried out under the stirring condition, and the concentrations of the propylene glycol alginate solution and the protein solution are set to be lower, so that the reaction speed is reduced, the reaction is slow, and the formation of the terpene-removed orange oil dispersion is facilitated.

In one embodiment, the step of adding the propylene glycol alginate solution into the mixed solution is carried out in a dropwise manner at a speed of 0.5mL/min to 3.0 mL/min. Specifically, a peristaltic pump may be used for the dropwise addition.

Specifically, the time for adding the propylene glycol alginate solution into the mixed solution to react is 0.5 h-1.5 h.

Step S140: and centrifuging the sweet orange oil nano dispersion to remove micron-sized dispersion, and taking supernatant to obtain the purified sweet orange oil nano dispersion.

Specifically, in the step of centrifuging the sweet orange oil nano-dispersion, the process conditions are as follows: the centrifugal speed is 10000 rpm-15000 rpm. The centrifugation time is 30 min-50 min. The centrifugation temperature was 4 ℃.

The transparent, uniformly dispersed and stable sweet orange oil nano dispersion can be prepared through the steps S110 to S140, and the particle size of the sweet orange oil nano dispersion is 15nm to 90 nm. And the problem of slow release of the sweet orange oil fragrance can be effectively solved by nanocrystallizing the sweet orange oil, so that the sweet orange oil fragrance can be slowly released outwards and can be emitted for a long time.

The preparation method of the sweet orange oil nano dispersion has at least the following advantages:

(1) the invention adopts the molecular distillation technology to effectively reduce the content of terpenes in the sweet orange oil, realizes the enrichment of the characteristic aroma components of the sweet orange oil, ensures pure flavor and improves the stability of the sweet orange oil.

(2) The invention successfully prepares the de-terpenoid sweet orange oil nano-dispersion by utilizing the crosslinking characteristic between the sodium alginate propylene glycol ester and the protein, and no relevant research report is found at home at present.

(3) The prepared sweet orange oil nano dispersion has small dispersed particle size (15-90 nm), good stability, no toxicity and safety, is not layered after being placed for a long time, can stably exist in boiling water, can be slowly released outwards, and can permanently emit fragrance.

(4) The sweet orange oil nano-dispersion prepared by the invention is in a liquid appearance and a transparent state, is convenient to use in beverages and detergents, can be rapidly and uniformly dispersed, does not have a layering phenomenon, does not influence the original appearance of the beverages and the detergents, and does not influence the functional characteristics of the beverages and the detergents.

The transparent beverage of an embodiment comprises the sweet orange oil nano-dispersion prepared by the preparation method of the sweet orange oil nano-dispersion. Specifically, the transparent beverage further includes: sweeteners and acidulants. In this embodiment, the sweetener and sour agent may be those commonly used in the art. For example, the sweetener may be white sugar, xylitol, sucrose, sodium cyclamate, aspartame, acesulfame, AK sugar, stevioside, sucralose, etc. The sour agent can be citric acid, sodium citrate, lactic acid, tartaric acid, malic acid, etc.

In one embodiment, the transparent beverage consists of 5-15% of sweetening agent, 0.08-0.50% of sour agent and the balance of orange oil nano dispersion by mass percentage. It is understood that in other embodiments, the formulation of the transparent beverage is not limited to the above formulation, and may be other formulations commonly used in the art.

In one embodiment, the method for preparing the transparent beverage comprises the following steps: and (3) uniformly mixing the sweetening agent, the sour agent and the sweet orange oil nano dispersion to obtain the transparent beverage.

The transparent beverage has the advantages of transparent appearance, moderate sour and sweet taste, pure and strong fragrance, and no layering phenomenon after being stored for more than 6 months.

The detergent of an embodiment comprises the sweet orange oil nano-dispersion prepared by the preparation method of the sweet orange oil nano-dispersion of the above embodiment. Specifically, the detergent also comprises fatty alcohol-polyoxyethylene ether, ethoxylated sodium alkyl sulfate and ethylene diamine tetraacetic acid disodium salt.

In one embodiment, the detergent comprises, by mass, 5% to 12% of fatty alcohol-polyoxyethylene ether, 15% to 25% of ethoxylated sodium alkyl sulfate, 3% to 8% of ethylenediaminetetraacetic acid disodium salt, and the balance of a sweet orange oil nano-dispersion. It is understood that in other embodiments, the formulation of the detergent is not limited to the above-mentioned formulation ratio, and may be other formulation ratios commonly used in the art.

In one embodiment, the detergent is prepared by a method comprising: and uniformly mixing the fatty alcohol-polyoxyethylene ether, the ethoxylated alkyl sodium sulfate, the ethylene diamine tetraacetic acid disodium salt and the sweet orange oil nano dispersion to obtain the detergent.

The detergent of the embodiment has good stability, does not generate layering phenomenon after being stored for a long time, and can be effectively adsorbed on clothes, so that the fabric has lasting fragrance.

The following are specific examples:

it is noted that in the following examples, the particle size of the orange oil nanodispersion was measured using a particle size analyzer model malvern S90.

Example 1

The procedure for the preparation of the orange oil nanodispersion of this example is as follows:

(1) the sweet orange oil is filled into a sample injection bottle of short-path molecular distillation equipment for molecular distillation, the molecular distillation temperature is 30 ℃, the distillation pressure is 150Pa, the feeding speed is 1.8mL/min, and the scraper plate rotating speed is 200 r/min. Collecting the distillate to obtain the de-terpened sweet orange oil.

(2) Adding 1mL of de-terpened sweet orange oil into 80mL of gelatin solution with the concentration of 1.5mg/mL, treating by a micro-jet ultrahigh-pressure homogenizer with the homogenizing pressure of 12000psi, circularly homogenizing for 3 times, and then adjusting the pH value of the solution to 9.3 to obtain a mixed solution.

(3) Slowly and dropwise adding 0.7mL of propylene glycol alginate solution with the concentration of 0.3mg/mL and the esterification degree of 90% into the mixed solution, and reacting for 0.8h to obtain the sweet orange oil dispersoid.

(4) Centrifuging the sweet orange oil dispersion at 12000rpm and 4 deg.C for 40min to remove micrometer-sized dispersion, and collecting supernatant to obtain sweet orange oil nanometer dispersion with particle diameter of 18.03 nm.

The particle size distribution of the orange oil nanodispersion of this example is shown in figure 2.

Example 2

(1) the sweet orange oil is filled into a sample injection bottle of short-path molecular distillation equipment for molecular distillation, the molecular distillation temperature is 50 ℃, the distillation pressure is 120Pa, the feeding speed is 3.5mL/min, and the scraper rotating speed is 300 r/min. Collecting the distillate to obtain the de-terpened sweet orange oil.

(2) Adding 2.5mL of de-terpened sweet orange oil into 100mL of whey protein solution with the concentration of 2.6mg/mL, treating by a micro-jet ultra-high pressure homogenizer with the homogenizing pressure of 20000psi, circularly homogenizing for 2 times, and adjusting the pH value of the solution to 9.6 to obtain a mixed solution.

(3) Slowly and dropwise adding 6.0mL of propylene glycol alginate solution with the concentration of 0.45mg/mL and the esterification degree of 90% into the mixed solution, and reacting for 1.0h to obtain the sweet orange oil dispersoid.

(4) Centrifuging the sweet orange oil dispersion at 15000rpm and 4 deg.C for 30min, removing micrometer dispersion, and collecting supernatant to obtain 35.18nm sweet orange oil nanometer dispersion.

Example 3

(1) the sweet orange oil is filled into a sample injection bottle of short-path molecular distillation equipment for molecular distillation, the molecular distillation temperature is 35 ℃, the distillation pressure is 180Pa, the feeding speed is 1.5mL/min, and the scraper plate rotating speed is 160 r/min. Collecting the distillate to obtain the de-terpened sweet orange oil.

(2) Adding 5mL of de-terpened sweet orange oil into 200mL of gelatin solution with the concentration of 0.8mg/mL, treating by a micro-jet ultrahigh-pressure homogenizer with the homogenizing pressure of 12000psi, circularly homogenizing for 3 times, and adjusting the pH value of the solution to 10.2 to obtain a mixed solution.

(3) And slowly dropwise adding 13mL of propylene glycol alginate solution with the concentration of 0.1mg/mL and the esterification degree of 95% into the mixed solution, and reacting for 1.2h to obtain the de-terpenic sweet orange oil dispersion.

(4) Centrifuging the sweet orange oil dispersion at 10000rpm and 4 deg.C for 50min, removing micrometer dispersion, and collecting supernatant to obtain 81.59nm sweet orange oil nanometer dispersion.

Example 4

(1) the sweet orange oil is filled into a sample injection bottle of short-path molecular distillation equipment for molecular distillation, the molecular distillation temperature is 40 ℃, the distillation pressure is 350Pa, the feeding speed is 2.5mL/min, and the scraper rotating speed is 200 r/min. Collecting the distillate to obtain the de-terpened sweet orange oil.

(2) Adding 1mL of de-terpenized sweet orange oil into 180mL of gelatin solution with the concentration of 1.0mg/mL, treating by a micro-jet ultra-high pressure homogenizer with the homogenizing pressure of 15000psi, circularly homogenizing for 3 times, and then adjusting the pH value of the solution to 8.5 to obtain a mixed solution.

(3) Slowly and dropwise adding 3mL of propylene glycol alginate solution with the concentration of 0.3mg/mL and the esterification degree of 92% into the mixed solution, and reacting for 0.8h to obtain the sweet orange oil dispersoid.

(4) Centrifuging the sweet orange oil dispersion at 13000rpm and 4 deg.C for 40min, removing micrometer-sized dispersion, and collecting supernatant to obtain sweet orange oil nanometer dispersion with particle diameter of 23.74 nm.

Example 5

(1) the sweet orange oil is filled into a sample injection bottle of short-path molecular distillation equipment for molecular distillation, the molecular distillation temperature is 45 ℃, the distillation pressure is 200Pa, the feeding speed is 2mL/min, and the scraper rotating speed is 250 r/min. Collecting the distillate to obtain the de-terpened sweet orange oil.

(2) Adding 1mL of de-terpened sweet orange oil into 100mL of gelatin solution with the concentration of 2mg/mL, treating by a micro-jet ultra-high pressure homogenizer with the homogenizing pressure of 10000psi, circularly homogenizing for 3 times, and then adjusting the pH value of the solution to 10.0 to obtain a mixed solution.

(3) Slowly and dropwise adding 1.3mL of propylene glycol alginate solution with the concentration of 0.4mg/mL and the esterification degree of 96% into the mixed solution, and reacting for 0.6h to obtain the sweet orange oil dispersoid.

(4) Centrifuging the sweet orange oil dispersion at 14000rpm and 4 deg.C for 35min to remove micrometer-sized dispersion, and collecting supernatant to obtain sweet orange oil nanometer dispersion with particle diameter of 42.68 nm.

Example 6

The preparation process of the transparent beverage of this example is as follows:

(1) weighing the following raw materials in proportion: 4g of white granulated sugar, 5g of xylitol, 0.16g of citric acid, 0.28g of sodium citrate and 90.56g of the sweet orange oil nano-dispersion prepared in the example 1.

(2) Mixing the above materials uniformly to obtain transparent beverage.

Example 7

The preparation process of the transparent type beverage of example 7 is similar to that of example 6 except that: the transparent beverage of example 7 comprises the following raw materials: 14g of white granulated sugar, 0.08g of citric acid, 0.21g of sodium citrate and 85.71g of the sweet orange oil nano-dispersion prepared in example 2.

Example 8

The preparation process of the transparent type beverage of example 8 is similar to that of example 6 except that: the transparent beverage of example 8 comprises the following raw materials: 10g of sucrose, 0.23g of citric acid, 0.18g of sodium citrate and 89.59g of the sweet orange oil nano-dispersion prepared in example 3.

Experiments prove that the transparent beverages prepared in the embodiments 6 to 8 have the advantages of transparent appearance, proper sour and sweet taste, pure and rich fragrance, and no layering phenomenon after being stored for more than 6 months.

Example 9

The preparation process of the detergent of this example is as follows:

(1) weighing the following raw materials in proportion: 6g of fatty alcohol-polyoxyethylene ether, 20g of ethoxylated sodium alkyl sulfate, 7g of ethylene diamine tetraacetic acid disodium salt and 67g of the sweet orange oil nano dispersion prepared in example 1.

(2) And uniformly mixing the raw materials to obtain the detergent.

Example 10

The procedure for the preparation of the detergent of example 10 was similar to that of example 9, except that: the proportion of each raw material of the detergent of the embodiment 10 is as follows: 12g of fatty alcohol-polyoxyethylene ether, 15g of ethoxylated sodium alkyl sulfate, 3g of ethylenediamine tetraacetic acid disodium salt and 70g of the sweet orange oil nano dispersion prepared in the example 2.

Example 11

The procedure for the preparation of the detergent of example 11 was similar to that of example 9, except that: the formulation of the detergent of example 11 was as follows: 10g of fatty alcohol-polyoxyethylene ether, 25g of ethoxylated sodium alkyl sulfate, 6g of ethylene diamine tetraacetic acid disodium salt and 59g of the sweet orange oil nano dispersion prepared in example 3.

Experiments prove that the detergents prepared in the examples 9 to 11 have good stability and do not generate layering phenomenon after being stored for a long time. And the detergent can be effectively adsorbed on clothes, so that the fragrance of the fabric is kept for a long time.

Comparative example 1

The procedure for the preparation of the sweet orange oil nanodispersion of comparative example 1 was similar to that of example 1 except that: in comparative example 1, step (1) was not included, i.e. the sweet orange oil was not subjected to a terpenoid removal step during the preparation of the sweet orange oil nanodispersion of comparative example 1.

Comparative example 2

The procedure for the preparation of the sweet orange oil nanodispersion of comparative example 2 was similar to that of example 1 except that: in step (2) of comparative example 2, the pH was not adjusted.

Comparative example 3

The procedure for the preparation of the sweet orange oil nanodispersion of comparative example 3 was similar to that of example 1 except that: in step (2) of comparative example 3, the homogenization pressure was 5000 psi.

Comparative example 4

The procedure for the preparation of the sweet orange oil nanodispersion of comparative example 4 was similar to that of example 1 except that: in step (2) of comparative example 4, the concentration of the protein solution was 5.0 mg/mL.

Comparative example 5

The procedure for the preparation of the sweet orange oil nanodispersion of comparative example 5 was similar to that of example 1 except that: in step (3) of comparative example 5, the concentration of propylene glycol alginate was 1.5 mg/mL.

After the orange oil nano-dispersions prepared in examples 1 to 5 and comparative examples 1 to 5 were allowed to stand at room temperature for 1 month, 2 months, 4 months, 5 months and 6 months, the appearance state of the orange oil nano-dispersions at different periods was observed, and data as shown in table 1 below were obtained.

Table 1 stability data of the sweet orange oil nanodispersions of the examples and comparative examples

As can be seen from table 1 above, the orange oil nanodispersions prepared in examples 1 to 5 remained transparent after being placed for a long time, and did not delaminate and have good stability. The sweet orange oil nano dispersions prepared in comparative examples 1 to 5 are opaque and easy to delaminate.

The orange oil nanodispersions obtained in the above examples 1 to 5 and comparative examples 1 to 5 were tested for retention after a certain period of time, and data as shown in the following table 2 were obtained.

The method for calculating the sweet orange oil retention rate comprises the following steps:

50g of the sweet orange oil nano dispersion is accurately weighed and placed in a round bottom flask with glass beads, 500mL of deionized water is added, and after shaking and mixing, a volatile oil tester and a reflux condenser tube are connected. Adding water from the upper end of the condensation tube to make the water fill the scale part of the volatile oil detector and overflow to the flask. And (3) placing the flask in an electric heating jacket, slowly heating to boil, keeping slightly boiling for about 5 hours until the oil amount in the volatile oil detector is not increased any more, stopping heating, placing for a moment, starting a piston at the lower end of the volatile oil detector, and slowly discharging water until the upper end of the oil layer reaches a position 5mm above the 0 line of the scale mark. Standing for more than 1h, starting the piston at the lower end of the volatile oil tester, lowering the oil layer until the upper end of the oil layer is just level with the 0-line scale, and reading the volatile oil amount.

The retention K of essential oil in the orange oil nanodispersion was calculated as follows: and K is M/M multiplied by 100 percent, wherein M is the content of essential oil in the nano dispersion after being placed for a period of time, and M is the content of essential oil in the untreated sweet orange oil nano dispersion.

Table 2 retention data for the sweet orange oil nanodispersions of the examples and comparative examples

As can be seen from table 2, the sweet orange oil nano-dispersions prepared in examples 1 to 5 still maintain high retention rate after being placed for a long time, and have lasting fragrance.

The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.

The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims

1. A preparation method of the sweet orange oil nano dispersion is characterized by comprising the following steps:

removing terpene from sweet orange oil to obtain de-terpened sweet orange oil;

2. The method of preparing a nano-dispersion of sweet orange oil according to claim 1, further comprising: and centrifuging the sweet orange oil nano dispersion to remove micron-sized dispersion, and taking supernatant to obtain the purified sweet orange oil nano dispersion.

3. The method for preparing the sweet orange oil nano-dispersion according to claim 2, wherein in the step of centrifuging the sweet orange oil nano-dispersion, the centrifugation speed is 10000rpm to 15000rpm, and the centrifugation time is 30min to 50 min.

4. The method for preparing the sweet orange oil nano dispersion as claimed in claim 1, wherein the sweet orange oil is subjected to terpene removal by molecular distillation under the following conditions: the temperature of molecular distillation is 30-50 ℃, the distillation pressure is 120-350 Pa, the feeding speed is 1.0-3.5 mL/min, and the scraper rotating speed is 150-300 r/min.

5. The method of claim 1, wherein the protein solution comprises a protein and water, wherein the protein is at least one selected from the group consisting of soy protein, whey protein, gelatin, and wheat protein; and/or the presence of a catalyst in the reaction mixture,

6. The method for preparing the nano-dispersion of sweet orange oil according to claim 1, wherein in the step of homogenizing, the homogenizing pressure is 10000 psi-20000 psi, and the number of times of circulating homogenization is 2-3 times; and/or the presence of a catalyst in the reaction mixture,

7. The preparation method of the sweet orange oil nano-dispersion according to claim 1, wherein the degree of esterification of the propylene glycol alginate is 88% to 99%; and/or the presence of a catalyst in the reaction mixture,

8. The sweet orange oil nano dispersion prepared by the preparation method of the sweet orange oil nano dispersion as claimed in any one of claims 1 to 7.

9. A clear beverage comprising the nano-dispersion of sweet orange oil of claim 8.

10. The transparent beverage as claimed in claim 9, further comprising 5-15% sweetener and 0.08-0.50% sour agent by weight.

11. A detergent comprising the sweet orange oil nanodispersion of claim 8.

12. The detergent according to claim 11, wherein the detergent further comprises 5-12% by mass of fatty alcohol-polyoxyethylene ether, 15-25% by mass of sodium ethoxylated alkyl sulfate, and 3-8% by mass of disodium ethylenediamine tetraacetic acid.