CN114163836B - Acid-resistant annatto as well as preparation method and application thereof - Google Patents
Acid-resistant annatto as well as preparation method and application thereof Download PDFInfo
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- CN114163836B CN114163836B CN202111387762.8A CN202111387762A CN114163836B CN 114163836 B CN114163836 B CN 114163836B CN 202111387762 A CN202111387762 A CN 202111387762A CN 114163836 B CN114163836 B CN 114163836B
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- annatto
- preparation
- resistant
- acid
- temperature
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0084—Dispersions of dyes
- C09B67/0091—Process features in the making of dispersions, e.g. ultrasonics
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, 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
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- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
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Abstract
The invention belongs to the field of natural pigment preparation, and particularly relates to an acid-resistant annatto as well as a preparation method and application thereof. The invention adopts the technical means of pipeline emulsification high-speed shearing mixing, low-temperature degassing and positive pressure inert gas protection, wet grinding, high-pressure homogenization, UHT sterilization and the like to prepare the acid-resistant annatto with different color tones. The preparation process does not use organic solvent for dissolution or organic solvent for dissolution, has no harm to the dissolution residue and safety risk of products, and the particle size D90 of the prepared acid-resistant annatto is less than 400nm, which is favorable for improving the stability and bioavailability, and does not precipitate under the acidic condition, so that the stability is high, the color tone of annatto is enriched, the practical application problems of precipitation, low stability, single color tone and the like of the prior market annatto under the acidic condition are changed, the requirements of different markets can be met, the domestic blank is filled, and the application field of annatto is further expanded.
Description
Technical Field
The invention belongs to the field of natural pigment preparation, and particularly relates to an acid-resistant annatto as well as a preparation method and application thereof.
Background
The annatto is a nontoxic and harmless natural pigment extracted from seed coats of the tropical plant annatto, and can be used for coloring food and has functional nutritive value. The functional natural pigment is widely used internationally in European and American areas for thousands of years through FAO/WHO and JECFA reviews. The food additive has been put into the national standard for use in the health standard (GB 2760) in China for a long time, and has been widely applied.
At present, the development and application of the annatto pigment in China are still in a starting stage, and because of the limitations of resources, technology and the like, the annatto pigment product used in China is mostly dissolved and applied in an alkaline environment, and the problems of precipitation, poor stability and the like often appear when the annatto pigment is applied in an acidic environment, so that the actual requirements of a plurality of food categories in GB2760 can not be met; meanwhile, the current annatto products used in China are yellow in color, and the requirements of rich and colorful foods are not met.
Therefore, the preparation process of the annatto is studied deeply, fills the blank of the annatto products with different color tones of acid resistance in China, and becomes urgent.
Disclosure of Invention
In order to overcome the defects and the shortcomings of the prior art, the primary aim of the invention is to provide a preparation method of acid-resistant annatto, which does not use organic solvent for dissolution or organic solvent for dissolution assistance in the preparation process, has no harm to the residual dissolution and safety risk on products, and has the particle size D90 of less than 400nm, thereby being beneficial to improving the stability and bioavailability.
The invention also aims to provide the acid-resistant annatto prepared by the preparation method, which is free from precipitation under the acid condition, has high stability, can be used for preparing different colors, further meets the requirements of different markets, and further expands the application field.
It is a further object of the present invention to provide the use of the acid resistant annatto described above.
The aim of the invention is achieved by the following technical scheme:
a method for preparing acid-resistant annatto, comprising the following steps:
(1) Preparation of annatto preparation: uniformly stirring and mixing the annatto and the diluent in low-temperature vacuum to obtain annatto preparation materials, wherein the conditions of low-temperature vacuum stirring are as follows: the temperature is 0-50 ℃, the vacuum degree is-0.005 to-0.1 Mpa, the stirring rotating speed is 5-500r/min, and the time is 5-60min;
(2) Preparing an aqueous solution of annatto: mixing at least one of a dispersing agent and a filler with water uniformly by low-temperature vacuum stirring and emulsification to obtain a annatto aqueous phase solution, wherein the conditions of the low-temperature vacuum stirring and emulsification are as follows: the temperature is 0-50 ℃, the vacuum degree is-0.005 to-0.1 Mpa, the stirring and emulsifying speed is 5-5000r/min, and the time is 5-60min;
(3) Pipeline emulsification high-speed shear mixing: synchronously conveying the annatto preparation material prepared in the step (1) and the annatto aqueous solution prepared in the step (2) into a pipeline emulsifying machine on line according to the mass ratio of 1 (8-20), and carrying out pipeline emulsification high-speed shearing and mixing to ensure that materials are uniformly and finely dispersed to obtain annatto preparation liquid, wherein the pipeline emulsification high-speed shearing and mixing conditions are as follows: the temperature is 0-50 ℃, the rotating speed is 500-3000r/min, and the time is 0.5-30min;
(4) Low temperature vacuum degassing and positive pressure inert gas protection: carrying out low-temperature vacuum degassing on the annatto preparation liquid prepared in the step (3) in a storage tank, wherein the low-temperature vacuum degassing condition is that the temperature is 0-50 ℃, the vacuum degree is-0.005 to-0.1 Mpa, and the stirring rotating speed is 5-500r/min for 5-30min; then filling inert gas to replace the vacuum state, so that the pressure of the inert gas in the storage tank is 0.005-3.0Mpa, the loss of materials is reduced through the protection of the inert gas by positive pressure, and the materials are combined more tightly;
(5) Wet grinding: delivering the annatto preparation solution treated in the step (4) into a wet grinder for wet grinding, wherein the conditions of the wet grinding are as follows: the rotating speed is 500-8000r/min, and the time is 5-120min;
(6) Homogenizing under high pressure: homogenizing the annatto preparation liquid obtained by wet crushing in the step (5) at least one high pressure, so that the annatto preparation liquid enters a more stable and fine state;
(7) UHT sterilization: carrying out UHT sterilization on the annatto preparation liquid after high-pressure homogenization in the step (6) to obtain acid-resistant annatto;
the diluent in the step (1) is at least one of grease, an emulsifying agent, an antioxidant and the like;
the oil is at least one of safflower seed oil, MCT oil (medium chain triacylglycerol), corn oil, olive oil, sunflower seed oil, peanut oil, soybean oil, coconut oil, palm oil and other oils;
the emulsifier is at least one of span, tween, sucrose fatty acid ester, polyglycerol fatty acid ester, citric acid fatty acid glyceride, propylene glycol fatty acid ester, phospholipid, enzymolysis soybean phospholipid, modified soybean phospholipid, mono-diglycerol fatty acid ester, lactic acid fatty acid glyceride, sodium caseinate and other emulsifiers;
the antioxidant is at least one of polyphenols and its derivatives/extracts, flavonoids and its derivatives/extracts, and antioxidant esters/salts;
the polyphenols and their derivatives/extracts are preferably at least one of rosemary extract, carnosol and tocopherol;
the flavonoid and its derivative/extract are preferably at least one of tea polyphenols and folium Bambusae extract;
the antioxidant esters/salts are preferably at least one of lecithin, ascorbyl palmitate, ascorbic acid and salts thereof;
the low-temperature vacuum stirring in the step (1) is preferably performed in a vacuum stirring and mixing tank;
the low-temperature vacuum stirring emulsification in the step (2) is preferably performed in a vacuum stirring emulsification tank, wherein the vacuum stirring emulsification tank is provided with a stirrer device and an emulsifying device, and the two devices are not operated in the same direction, one device is anticlockwise, the other device is clockwise, stirring force, emulsifying shearing force, collision force and the like are formed on materials, and the efficiency is higher than that of single stirring or single emulsification;
the dispersing agent in the step (2) is at least one of water, tween, polyglycerol fatty acid ester, sucrose fatty acid ester, propylene glycol, glycerol and other dispersing agents;
the filler in the step (2) is at least one of maltitol, sorbitol, glucose syrup, erythritol, xylitol, maltitol, glucose, white granulated sugar, trehalose, maltodextrin, xanthan gum, pectin, acacia, cellulose, dietary fiber, microcrystalline cellulose, carboxymethyl cellulose, cyclodextrin, starch, modified starch and other fillers;
the aqueous annatto solution described in step (2) preferably further comprises: at least one of water-soluble emulsifiers, preservatives, stabilizers, acids and salts thereof, moisture retention agents, protective colloids, fragrances, fillers, pH buffers and other common components;
the preservative is preferably at least one of sorbic acid and salts thereof;
the acid is preferably at least one of citric acid and acetic acid;
the water retention agent is preferably at least one of glycerol, sorbitol and polyethylene glycol;
the inert gas in the step (4) can be nitrogen, argon or the like;
the conveying in the step (5) is preferably carried out by adopting a peristaltic pump or a screw pump, the working speed of the pump is preferably 5-500r/min, and the flow speed of conveying materials is low when the pump speed is low; the rotating speed is high, and the flow speed of the conveying material is high;
the pressure of the high-pressure homogenization in the step (6) is preferably 10-200Mpa;
the pressure of the high-pressure homogenization in the step (6) is further preferably 65-200Mpa;
the UHT sterilization conditions in step (7) are as follows: the temperature is 80-135 ℃ and the time is 3-15s;
the acid-resistant annatto in the step (7) can be further filled to obtain an acid-resistant annatto emulsion or spray-dried to obtain acid-resistant annatto powder;
the acid-resistant annatto is prepared by the preparation method;
the acid-resistant annatto is applied to the fields of food, cosmetics and medicine preparation;
the principle of the invention is as follows:
in order to solve the problems of narrow application field, poor stability, single color tone and the like of the annatto in the prior art, the invention prepares the acid-resistant annatto with different color tones through the optimized combination of a plurality of processes, and specifically comprises the following steps:
(1) According to the invention, the annatto preparation material is prepared by low-temperature vacuum stirring, so that the oxidation loss of the material is reduced, and the annatto and the diluent are combined more tightly.
(2) According to the invention, the annatto aqueous phase solution is prepared by low-temperature vacuum stirring and emulsification, so that oxygen and bubble residues in the aqueous phase solution are reduced, further, on one hand, the subsequent oxidation loss is reduced, and on the other hand, the bonding compactness of annatto in the later-stage working procedure is increased, so that the annatto is emulsified and bonded in a molecular state, and the annatto is more stable.
(3) According to the invention, the high-speed shearing mixing of the annatto preparation material and the annatto aqueous solution is performed through pipeline emulsification, so that the emulsifying shearing capability is stronger, and an emulsion system with uniform dispersion and tight combination stability is formed; and the pipeline emulsifying machine can be operated continuously on line, so that the operation is more convenient and the efficiency is higher.
(4) The invention further achieves the purposes of reducing the oxidation loss of materials and improving the bonding compactness of the materials through low-temperature vacuum degassing and positive pressure inert gas protection, so that an emulsion system is more stable; wherein, the air in the removable emulsion is deaerated in vacuum at low temperature (air bubbles can be generated during emulsification and gas is involved), so that on one hand, oxidation is avoided, and on the other hand, the problems of untight material combination, agglomeration and the like in the three-phase mixing process of annatto, water phase and gas are avoided; the material loss is further reduced through the protection of inert gas positive pressure, and the material combination is tighter.
(5) The invention further ensures that the annatto preparation liquid is finer and more uniform through wet grinding, and the annatto preparation material and the water are combined more firmly.
(6) The invention further ensures that the annatto emulsion is finer and more uniform and has D90 less than 400nm through high-pressure homogenization, and the annatto preparation material and the water phase are combined very firmly.
(7) The invention makes the annatto preparation liquid in a sterile state through UHT sterilization, and has higher application quality and safety.
Compared with the prior art, the invention has the following advantages and effects:
(1) The invention adopts five technologies (figure 1) of pipeline emulsification high-speed shearing mixing, low-temperature degassing and positive pressure inert gas protection, wet grinding, high-pressure homogenization and UHT sterilization to prepare the acid-resistant annatto with different colors.
(2) The preparation process of the preparation method provided by the invention does not use organic solvent for dissolution or organic solvent for dissolution assistance, and has no residual solvent hazard and safety risk to products.
(3) The invention solves the practical application problems of precipitation and precipitation under the acidic condition, poor stability, single color tone and the like of the prior market annatto, and the prepared acid-resistant annatto product does not precipitate under the acidic condition, and the annatto particle size D90 is less than 400nm, thereby being beneficial to improving the stability and bioavailability and improving the stability.
(4) The acid-resistant annatto product prepared by the invention can be manufactured into different color tones, so that the color tone of annatto is enriched, the demands of different markets are met, the domestic blank is filled, and the application field is further expanded.
Drawings
Fig. 1 is a process flow diagram of the present invention.
Fig. 2 is an external appearance display view of an aqueous solution (ABS 453 nm=1.0) prepared from the annatto samples prepared in examples 1-2 and comparative example 1, wherein a: example 1 sample (red), B: example 2 sample (orange), C: comparative example 1 sample (yellow in color).
FIG. 3 is an external view showing the appearance of an acidic juice beverage prepared from the annatto emulsion prepared in examples 1 and 2; wherein A: example 1 sample (red), B: example 2 sample (orange yellow).
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
The annatto and the deodorized rosemary extract, etc. are provided by Henan Hemsl Biotech Co.
Example 1
(1) Preparation of annatto preparation: 2.15Kg of annatto (the content is 95 wt.%), 0.1Kg of tocopherol, 0.1Kg of deodorized rosemary extract and 0.15Kg of sunflower seed oil are added into a vacuum stirring and mixing tank, and the mixture is uniformly stirred and mixed at a low temperature under vacuum to obtain annatto preparation materials, wherein the conditions of low temperature vacuum stirring are as follows: the temperature is 25 ℃, the vacuum degree is-0.05 Mpa, the stirring rotating speed is 150r/min, and the time is 20min;
(2) Preparing an aqueous solution of annatto: adding 6.0Kg of modified starch, 1.5Kg of maltodextrin and 30.0Kg of reverse osmosis membrane water into a vacuum stirring emulsifying tank, and uniformly mixing by low-temperature vacuum stirring, wherein the conditions of the low-temperature vacuum stirring and emulsifying are as follows: the temperature is 30 ℃, the vacuum degree is-0.06 MPa, the stirring and emulsifying rotational speed is 2000r/min, and the time is 40min; after standing, the aqueous phase solution is transparent, has no bubbles and no floating foam, namely the annatto aqueous phase solution;
(3) Pipeline emulsification high-speed shear mixing: synchronously conveying the annatto preparation material prepared in the step (1) and the annatto aqueous solution prepared in the step (2) into a pipeline emulsifying machine on line according to the mass ratio of 1:15, and carrying out pipeline emulsification high-speed shearing mixing, wherein the conditions of the pipeline emulsification high-speed shearing mixing are as follows: the temperature is 35 ℃, the rotating speed is 2500r/min, and the time is 20min, so that the materials are dispersed uniformly and finely, and the annatto preparation liquid is obtained;
(4) Low temperature vacuum degassing and positive pressure inert gas protection: carrying out low-temperature vacuum degassing on the annatto preparation liquid prepared in the step (3) in a storage tank, wherein the conditions of the low-temperature vacuum degassing are as follows: the temperature is 35 ℃, the vacuum degree is-0.08 Mpa, the stirring rotating speed is 100r/min, and the time is 10min; then, nitrogen is started, the nitrogen is filled, the vacuum state is replaced, the storage tank presents nitrogen pressure of 0.8Mpa, material loss can be reduced through positive pressure protection of the nitrogen, and the materials are combined more tightly;
(5) Wet grinding: after the nitrogen reaches the preset pressure, conveying the annatto preparation liquid treated in the step (4) into a wet grinder for wet grinding through a peristaltic pump (the rotating speed is 60 r/min), wherein the conditions of the wet grinding are as follows: the rotating speed is 5000r/min, and the time is 80min;
(6) Homogenizing under high pressure: homogenizing the annatto preparation liquid obtained by wet grinding in the step (5) for 1 time under 150Mpa to make the annatto preparation liquid enter a more stable and fine state;
(7) UHT sterilization: carrying out UHT high-temperature instantaneous sterilization on the annatto preparation liquid after the high-pressure homogenization in the step (6), wherein the sterilization conditions are as follows: and (3) conveying the mixture to a sterile storage tank at the temperature of 121 ℃ for 3 seconds, and spray-drying to obtain sterile acid-resistant annatto powder.
Example 2
(1) Preparation of annatto preparation: adding 0.25Kg of annatto (content of 95 wt.%), 0.05Kg of tocopherol, 0.05Kg of lecithin and 0.65Kg of MCT oil into a vacuum stirring and mixing tank, and uniformly stirring and mixing at a low temperature under vacuum to obtain annatto preparation materials, wherein the conditions of low temperature vacuum stirring are as follows: the temperature is 20 ℃, the vacuum degree is-0.08 Mpa, the stirring rotating speed is 300r/min, and the time is 35min;
(2) Preparing an aqueous solution of annatto: adding 4Kg of glycerin, 1.5Kg of sucrose fatty acid ester, 2.5Kg of polyglycerol fatty acid ester and 1Kg of reverse osmosis membrane water into a vacuum stirring emulsifying tank, and uniformly mixing by low-temperature vacuum stirring, wherein the conditions of the low-temperature vacuum stirring and emulsifying are as follows: the temperature is 20 ℃, the vacuum degree is-0.09 MPa, the emulsifying stirring rotating speed is 1000r/min, and the time is 30min; after standing, the aqueous phase solution is transparent, has no bubbles and no floating foam, namely the annatto aqueous phase solution;
(3) Pipeline emulsification high-speed shear mixing: synchronously conveying the annatto preparation material prepared in the step (1) and the annatto aqueous solution prepared in the step (2) into a pipeline emulsifying machine on line according to the mass ratio of 1:9, and carrying out pipeline emulsification high-speed shearing mixing, wherein the conditions of the pipeline emulsification high-speed shearing mixing are as follows: the temperature is 25 ℃, the rotating speed is 2000r/min, and the time is 15min, so that the materials are dispersed uniformly and finely, and the annatto preparation liquid is obtained;
(4) Low temperature vacuum degassing and positive pressure inert gas protection: carrying out low-temperature vacuum degassing on the annatto preparation liquid prepared in the step (3) in a storage tank, wherein the conditions of the low-temperature vacuum degassing are as follows: the temperature is 25 ℃, the vacuum degree is-0.09 Mpa, the stirring rotating speed is 50r/min, and the time is 20min; then, nitrogen is started, the nitrogen is filled in to replace the vacuum state, the storage tank presents nitrogen pressure of 1.5Mpa, material loss can be reduced through positive pressure protection of the nitrogen, and the materials are combined more tightly;
(5) Wet grinding: after the nitrogen reaches the preset pressure, conveying the annatto preparation liquid processed in the step (4) into a wet grinder for wet grinding through a peristaltic pump (the rotating speed is 120 r/min), wherein the conditions of the wet grinding are as follows: the rotating speed is 3500r/min, and the time is 50min;
(6) Homogenizing under high pressure: homogenizing the annatto preparation liquid obtained by wet grinding in the step (5) for 2 times under 65Mpa to make the annatto preparation liquid enter a more stable and fine state;
(7) UHT sterilization: carrying out UHT high-temperature instantaneous sterilization on the annatto preparation liquid after the high-pressure homogenization in the step (6), wherein the sterilization conditions are as follows: and (3) conveying the mixture to a sterile storage tank at the temperature of 105 ℃ for 5 seconds, and filling to obtain the sterile acid-resistant annatto emulsion.
Comparative example 1
(1) Preparation of annatto preparation: mixing annatto (95 wt.%) 0.5Kg and sodium hydroxide 0.2Kg, and pulverizing by conventional dry method;
(2) Preparing an aqueous solution of annatto: emulsifying and mixing 1.3Kg of maltodextrin and 3.5Kg of reverse osmosis membrane water uniformly in an emulsifying tank to obtain a annatto aqueous phase solution, wherein the emulsifying conditions are as follows: the emulsification temperature is 85 ℃, the emulsification rotating speed is 2000r/min, and the time is 40min;
(3) Common emulsification and mixing: adding the annatto preparation material prepared in the step (1) into the annatto aqueous phase solution prepared in the step (2), and emulsifying and mixing uniformly in an emulsifying tank to obtain annatto preparation liquid, wherein the emulsifying conditions are as follows: the temperature is 85 ℃, the emulsifying rotating speed is 3500r/min, and the time is 90min;
(4) Homogenizing under high pressure: homogenizing the annatto preparation solution prepared in the step (3) under 40Mpa for 1 time;
(5) And (3) carrying out spray drying on the annatto preparation liquid subjected to high-pressure homogenization in the step (4) to obtain annatto powder.
Comparative example 2
(1) Preparation of annatto preparation: 2.15Kg of annatto (content of 95 wt.%), 0.1Kg of tocopherol, 0.1Kg of deodorized rosemary extract and 0.15Kg of sunflower seed oil are mixed and stirred uniformly under the following stirring conditions: stirring at a rotation speed of 150r/min for 20min; then crushing the mixture by a dry method for standby;
(2) Preparing an aqueous solution of annatto: emulsifying and mixing 6.0Kg of modified starch, 1.5Kg of maltodextrin and 30.0Kg of reverse osmosis membrane water uniformly in an emulsifying tank to obtain a annatto aqueous phase solution, wherein the emulsifying conditions are as follows: the temperature is 85 ℃, the emulsifying rotating speed is 2000r/min, and the time is 40min;
(3) Common emulsification and mixing: adding the annatto preparation material prepared in the step (1) into the annatto aqueous phase solution prepared in the step (2), and emulsifying and mixing uniformly in an emulsifying tank to obtain annatto preparation liquid, wherein the emulsifying conditions are as follows: the temperature is 85 ℃, the emulsifying rotating speed is 3500r/min, the time is 90min, and the materials are dispersed uniformly and finely to form the annatto preparation liquid;
(4) Homogenizing the annatto preparation solution prepared in the step (3) under 40Mpa for 1 time;
(5) And (3) carrying out spray drying on the homogenized annatto preparation liquid in the step (4) to obtain annatto powder.
Comparative example 3
(1) Preparation of annatto preparation: as in example 1;
(2) Preparing an aqueous solution of annatto: adding 6.0Kg of modified starch, 1.5Kg of maltodextrin and 30.0Kg of reverse osmosis membrane water into a vacuum stirring emulsifying tank, and uniformly stirring, emulsifying and mixing under the following conditions: the temperature is 85 ℃, the vacuum degree is-0.06 MPa, the emulsifying time is 2000r/min, and the emulsifying time is 40min; after standing, the aqueous phase solution is transparent, has no bubbles and no floating foam, namely the annatto aqueous phase solution;
(3) Vacuum stirring, emulsifying and mixing: adding the annatto preparation material prepared in the step (1) into the annatto aqueous phase solution prepared in the step (2), and uniformly mixing in a vacuum stirring and emulsifying tank by vacuum stirring, wherein the conditions of vacuum stirring and emulsifying are as follows: emulsifying 3500r/min for 90min at 85 ℃ under vacuum degree-0.06 MPa to disperse the materials uniformly and fine to form annatto preparation liquid;
(4) Homogenizing the annatto preparation solution prepared in the step (3) under 40Mpa for 1 time;
(5) And (3) carrying out spray drying on the homogenized annatto preparation liquid in the step (4) to obtain annatto powder.
Comparative example 4
(1) Preparation of annatto preparation: as in example 1;
(2) Preparing an aqueous solution of annatto: as in example 1;
(3) Low-temperature vacuum stirring, emulsifying and mixing: adding the annatto preparation material prepared in the step (1) into the annatto aqueous phase solution prepared in the step (2), and uniformly mixing in a vacuum stirring and emulsifying tank under the conditions of low-temperature vacuum stirring and emulsifying: emulsifying 3500r/min for 90min at 30 ℃ under vacuum degree-0.06 MPa to disperse the materials uniformly and fine to form annatto preparation liquid;
(4) Homogenizing the annatto preparation solution prepared in the step (3) under 40Mpa for 1 time;
(5) Carrying out UHT high-temperature instantaneous sterilization on the homogenized annatto preparation solution in the step (4), wherein the sterilization conditions are as follows: the temperature is 121 ℃ for 3s, then the mixture is conveyed to a sterile storage tank, and spray drying is carried out to obtain annatto powder.
Comparative example 5
(1) Preparation of annatto preparation: as in example 1;
(2) Preparing an aqueous solution of annatto: as in example 1;
(3) Low-temperature vacuum stirring, emulsifying and mixing: same as comparative example 4;
(4) Wet grinding: conveying the annatto preparation liquid prepared in the step (3) into a wet grinder for wet grinding through a peristaltic pump (rotating speed 60 r/min), wherein the wet grinding conditions are as follows: the rotating speed is 5000r/min, and the time is 80min;
(5) Homogenizing the annatto preparation solution subjected to wet grinding in the step (4) under 40Mpa for 1 time;
(6) Carrying out UHT high-temperature instantaneous sterilization on the homogenized annatto preparation solution in the step (5), wherein the sterilization conditions are as follows: the temperature is 121 ℃ for 3s, then the mixture is conveyed to a sterile storage tank, and spray drying is carried out to obtain annatto powder.
Comparative example 6
(1) Preparation of annatto preparation: as in example 1;
(2) Preparing an aqueous solution of annatto: as in example 1;
(3) Pipeline emulsification high-speed shear mixing: as in example 1;
(4) Wet grinding: conveying the annatto preparation liquid prepared in the step (3) into a wet grinder for wet grinding through a peristaltic pump (rotating speed 60 r/min), wherein the wet grinding conditions are as follows: the rotating speed is 5000r/min, and the time is 80min;
(5) Homogenizing the annatto preparation solution subjected to wet grinding in the step (4) under 40Mpa for 1 time;
(6) Carrying out UHT high-temperature instantaneous sterilization on the homogenized annatto preparation solution in the step (5), wherein the sterilization conditions are as follows: the temperature is 121 ℃ for 3s, then the mixture is conveyed to a sterile storage tank, and spray drying is carried out to obtain annatto powder.
Example 3
(1) Preparation of annatto preparation: as in example 1;
(2) Preparing an aqueous solution of annatto: as in example 1;
(3) Pipeline emulsification high-speed shear mixing: as in example 1;
(4) Low temperature vacuum degassing and positive pressure inert gas protection: as in example 1;
(5) Wet grinding: as in example 1;
(6) Homogenizing under high pressure: homogenizing the annatto preparation liquid obtained by wet grinding in the step (5) under 40Mpa for 1 time to make the annatto preparation liquid enter a more stable and fine state;
(7) UHT sterilization: as in example 1.
Effect examples
Comparative example 1 is a preparation process of a common annatto preparation on the market at present, the preparation process is used for preparing annatto under neutral and alkaline conditions, the emulsification temperature is high, and the prepared annatto powder is a yellow color product and has the defects of poor stability, incapability of meeting the requirements of acidic conditions and the like. In order to overcome the defects and shortcomings of the traditional preparation process, the inventor of the invention intensively researches the preparation process of the annatto in practical work and explores the selection of different process means and the influence of combination on the effect of the annatto preparation. Wherein:
comparative example 2 differs from comparative example 1 in the formulation of annatto formulations;
comparative example 3 was based on comparative example 2, but the treatment temperature was still conventional high (85 ℃) in order to ensure that the microbiological indicator of the subsequent product reached the standard;
in the comparative example 4, in order to overcome the influence of high-temperature emulsification on materials based on the comparative example 3, low-temperature vacuum stirring emulsification is adopted, namely, the whole process is low in temperature, on one hand, the loss of materials is reduced, on the other hand, the stability of an emulsion stabilizing system is greatly improved, and meanwhile, UHT sterilization is introduced in order to ensure that the microbial index reaches the standard;
comparative example 5 wet milling was added on the basis of comparative example 4;
in the comparative example 6, on the basis of the comparative example 5, the emulsification of the lead-in pipeline has strong emulsifying and shearing capability, continuous online operation, more convenient operation and higher efficiency;
example 3 was based on comparative example 6 by introducing a low temperature vacuum degassing and a positive pressure inert gas blanket.
The process differences for comparative examples 1-6 and example 3 are shown in Table 1.
Table 1 comparative examples 1-6 and example 3 process comparative example
(1) Annatto content detection
(1) Accurately weighing 0.1-0.5g (accurate to 0.0001 g) of the annatto samples prepared in examples 1-3 and comparative examples 1-6, putting the annatto samples into a 50mL clean and dry small beaker, adding a small amount of distilled water, carefully stirring with a glass rod until the annatto samples are completely dissolved, transferring the annatto samples to a 100mL volumetric flask, and shaking the annatto samples uniformly.
(2) Accurately sucking the solution by a 1mL suction pipe, injecting 1mL into a 100mL volumetric flask, fixing the volume to a scale by using acetone, and shaking uniformly to obtain the test solution.
(3) The absorbance A of the test solution was measured at 453nm in a 1cm cuvette using acetone as reference solution.
W＝A/(m*30)*100
W: the content is as follows; a: absorbance at 453 nm; m: sample mass g;30: content coefficient; 100: dilution factor.
(2) Particle size detection
The annatto samples prepared in examples 1 to 3 and comparative examples 1 to 6 were formulated into aqueous solutions, and the particle size was measured by adding a laser particle size distribution instrument.
(3) Microorganism detection
The annatto samples prepared in examples 1-3 and comparative examples 1-6 were tested for relevant microbial indicators according to national standards, wherein the total number of colonies: GB 4789.2, coliform: GB 4789.3, pathogenic bacteria (salmonella): GB 4789.4.
(4) Water soluble tone detection
The annatto samples prepared in examples 1-3 and comparative examples 1-6 were prepared as an aqueous solution with ABS 453 nm=1.0, and the values of L, a, b were measured on a color difference meter.
The annatto samples prepared in examples 1-3 and comparative examples 1-6 were shown in Table 2 for loss rate, particle size, and microorganism detection results, and it can be seen from the table that the annatto samples prepared in the present invention were low in loss rate and small in particle size compared with the conventional annatto preparation process.
The appearance color and chromaticity values of the annatto samples prepared in examples 1-3 and comparative examples 1-6 are shown in fig. 2 and table 3, from which it can be seen that annatto samples of different hues can be prepared according to the present invention.
TABLE 2 relevant Performance index of the annatto samples prepared in examples 1-3 and comparative examples 1-6
TABLE 3 color and color values of appearance of annatto samples prepared in examples 1-3 and comparative examples 1-6
| Examples | Appearance color | Chromaticity value |
| Example 1 | Red color | L：65.66，a：29.20，b：25.72 |
| Example 2 | Orange yellow | L：77.56，a：23.18，b：65.73 |
| Comparative example 1 | Yellow colour | L：80.30，a：-0.65，b：65.07 |
| Comparative example 2 | Dark red | L：60.46，a：21.67，b：16.5 |
| Comparative example 3 | Dark red | L：62.43，a：25.38，b：20.40 |
| Comparative example 4 | Dark red | L：62.96，a：26.28，b：22.27 |
| Comparative example 5 | Red color | L：64.32，a：27.36，b：25.80 |
| Comparative example 6 | Red color | L：65.09，a：28.25，b：26.17 |
| Example 3 | Red color | L：65.23，a：28.63，b：25.92 |
Application examples
(1) An acidic juice beverage was prepared from the annatto powder prepared in examples 1, 3 and comparative examples 1-6, and comprises the following components in mass fraction: 76.1% of water, 10% of grapefruit juice concentrate, 3% of lemon juice concentrate, 10% of erythritol, 0.5% of stevioside, 0.2% of mogroside, 0.05% of malic acid, 0.05% of citric acid, 0.06% of sodium citrate, 0.002% of annatto powder and 0.038% of essence for food, wherein the pH of the acidic juice beverage is 2.8-4.5, and then observing whether the appearance color of the beverage is precipitated or not.
(2) An acidic juice beverage is prepared by taking the annatto emulsion prepared in example 2 as a raw material, and comprises the following components in mass percent: 76.4% of water, 8% of blood orange concentrated juice, 3% of apple concentrated juice, 2% of lemon concentrated juice, 10% of erythritol, 0.3% of stevioside, 0.1% of mogroside, 0.1% of citric acid, 0.04% of sodium citrate, 0.03% of annatto emulsion and 0.03% of essence for food; the pH of the acidic juice beverage is 2.8-4.5, and then the appearance color of the beverage is observed to see whether precipitation occurs.
The results are shown in Table 4, and it can be seen from the tables that the annatto powder or emulsion prepared in examples 1-3 has the characteristics of rich color, high stability, applicability under acidic conditions, and the like. FIG. 2 is an external view showing the appearance of an acidic juice beverage prepared from the annatto emulsion prepared in examples 1 and 2, wherein the acidic juice beverage prepared from the annatto emulsion prepared in example 1 is red in color and has no precipitation; the acidic juice beverage prepared by taking the annatto emulsion prepared in the example 1 as a raw material is orange in color and has no precipitation, and both the two components meet the requirements of the acidic beverage.
Table 4 evaluation results of acidic juice beverages
| Examples | Beverage tone | Whether or not there is precipitation | Whether or not to meet the acidic application |
| Example 1 | The color tone is red | No precipitation and precipitation | Meets the requirements of acidic beverage |
| Example 2 | The color tone is orange yellow | No precipitation and precipitation | Meets the requirements of acidic beverage |
| Comparative example 1 | Is yellow in color | More precipitate is separated out | Can not meet the requirements of acidic beverages |
| Comparative example 2 | Has dark red color, dark color and no appetite | More precipitate is separated out | Can not meet the requirements of acidic beverages |
| Comparative example 3 | Has dark red color, dark color and no appetite | More precipitate is separated out | Can not meet the requirements of acidic beverages |
| Comparative example 4 | Is dark red and has a slightly dark tone | More precipitate is separated out | Can not meet the requirements of acidic beverages |
| Comparative example 5 | Is red in color | With a small amount of precipitate | Substantially meets the requirements of acidic beverages |
| Comparative example 6 | Is red in color | No precipitation | Meets the requirements of acidic beverage |
| Example 3 | Is red in color | No precipitation | Meets the requirements of acidic beverage |
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the acid-resistant annatto is characterized by comprising the following steps of:
(1) Preparation of annatto preparation: uniformly stirring and mixing the annatto and the diluent in low-temperature vacuum to obtain annatto preparation materials, wherein the conditions of low-temperature vacuum stirring are as follows: the temperature is 0-50 ℃, the vacuum degree is-0.005 to-0.1 Mpa, the stirring speed is 5-500r/min, and the time is 5-60min;
(2) Preparing an aqueous solution of annatto: mixing at least one of a dispersing agent and a filler with water uniformly by low-temperature vacuum stirring and emulsification to obtain a annatto aqueous phase solution, wherein the conditions of the low-temperature vacuum stirring and emulsification are as follows: the temperature is 0-50 ℃, the vacuum degree is 0.005-0.1 Mpa, the stirring and emulsifying speed is 5-5000r/min, and the time is 5-60min;
(3) Pipeline emulsification high-speed shear mixing: synchronously conveying the annatto preparation material prepared in the step (1) and the annatto aqueous solution prepared in the step (2) to a pipeline emulsifying machine on line according to the mass ratio of 1 (8-20), and carrying out pipeline emulsification high-speed shearing mixing to obtain annatto preparation liquid, wherein the pipeline emulsification high-speed shearing mixing conditions are as follows: the temperature is 0-50 ℃, the rotating speed is 500-3000r/min, and the time is 0.5-30min;
(4) Low temperature vacuum degassing and positive pressure inert gas protection: carrying out low-temperature vacuum degassing on the annatto preparation liquid prepared in the step (3) in a storage tank, wherein the low-temperature vacuum degassing condition is that the temperature is 0-50 ℃, the vacuum degree is-0.005 to-0.1 Mpa, and the stirring rotating speed is 5-500r/min for 5-30min; then filling inert gas to replace the vacuum state, so that the pressure of the inert gas in the storage tank is 0.005-3.0Mpa;
(5) Wet grinding: delivering the annatto preparation solution treated in the step (4) into a wet grinder for wet grinding, wherein the conditions of the wet grinding are as follows: the rotating speed is 500-8000r/min, and the time is 5-120min;
(6) Homogenizing under high pressure: homogenizing the annatto preparation liquid obtained by wet grinding in the step (5) at least one high pressure;
(7) UHT sterilization: carrying out UHT sterilization on the annatto preparation liquid after high-pressure homogenization in the step (6) to obtain acid-resistant annatto;
the diluent in the step (1) is a mixture of grease, an emulsifying agent and an antioxidant;
the emulsifier is at least one of span, tween, sucrose fatty acid ester, polyglycerol fatty acid ester, citric acid fatty acid glyceride, propylene glycol fatty acid ester, phospholipid, enzymatic hydrolysis soybean phospholipid, modified soybean phospholipid, mono-diglycerol fatty acid ester, lactic acid fatty acid glyceride and sodium caseinate.
2. The method for preparing acid-resistant annatto of claim 1, wherein:
the filler in the step (2) is at least one of maltitol, sorbitol, glucose syrup, erythritol, xylitol, glucose, white granulated sugar, trehalose, maltodextrin, xanthan gum, pectin, acacia, cellulose, dietary fiber, carboxymethyl cellulose, cyclodextrin, starch and modified starch.
3. The method for preparing acid-resistant annatto of claim 1, wherein:
the dispersing agent in the step (2) is at least one of tween, polyglycerol fatty acid ester, sucrose fatty acid ester, propylene glycol and glycerin.
4. The method for preparing acid-resistant annatto of claim 1, wherein:
the aqueous annatto solution described in step (2) further comprises at least one of a water-soluble emulsifier, a preservative, a stabilizer, an acid, a salt thereof, a moisture-retaining agent, a protective colloid, a fragrance, a filler, and a pH buffer.
5. The method for preparing acid-resistant annatto of claim 1, wherein:
the inert gas in the step (4) is nitrogen or argon.
6. The method for preparing acid-resistant annatto of claim 1, wherein:
the high-pressure homogenization pressure in the step (6) is 10-200Mpa.
7. The method for preparing acid-resistant annatto of claim 1, wherein:
the UHT sterilization conditions in step (7) are as follows: the temperature is 80-135 ℃ and the time is 3-15s.
8. The method for preparing acid-resistant annatto of claim 1, wherein:
and (3) further filling the acid-resistant annatto in the step (7) to obtain an acid-resistant annatto emulsion or spray-drying to obtain acid-resistant annatto powder.
9. An acid resistant annatto prepared by the method of any one of claims 1-8.
10. Use of the acid resistant annatto of claim 9 in the field of food, cosmetic and pharmaceutical preparation.
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