CN116508979A

CN116508979A - Preparation method of high-ester pectin composition

Info

Publication number: CN116508979A
Application number: CN202310510227.XA
Authority: CN
Inventors: 李海秦; 李祥印
Original assignee: Qinhuangdao Jizhong Food Co ltd
Current assignee: Qinhuangdao Jizhong Food Co ltd
Priority date: 2023-05-08
Filing date: 2023-05-08
Publication date: 2023-08-01

Abstract

The invention provides a preparation method of a high-ester pectin composition applied to the field of high-ester pectin, wherein most of 3, 6-D-galacturonate groups of a pectin main chain in the high-ester pectin composition are methyl esterified, and meanwhile, part of groups are acetylated, so that the pectin forms a stable system in a yogurt system through electrostatic interaction between carboxyl groups and proteins, and acetyl can prevent the carboxyl groups of the pectin from forming a network structure through calcium bridges, thereby realizing no flocculation risk even under the condition of high addition amount, and enabling the mouthfeel to be fresh and smooth.

Description

Preparation method of high-ester pectin composition

Technical Field

The application relates to the field of high-ester pectin, in particular to a preparation method of a high-ester pectin composition.

Background

Pectin is a high molecular polysaccharide widely distributed in the primary cell wall and cell gap of the roots, stems, leaves, fruits and the like of higher plants. Commercial pectin is a food additive prepared by extracting and refining pericarps or pomace of pomelo, lemon, orange, apple and the like as raw materials.

Pectin is widely applied in the fields of fermented milk-containing beverages, formulated milk-containing beverages, lactobacillus beverages, vegetable protein beverages, compound protein beverages and the like. The pH value range of the fermented milk beverage, the prepared milk beverage, the lactobacillus beverage, the acidic plant protein beverage and the acidic compound protein beverage, which have good flavor, is 4.0-4.8, and the fermented milk beverage is just in the isoelectric point range of protein, so that protein flocculation is easy to occur, and precipitation layering phenomenon is caused.

In the acidification process of milk, as the protein carries positive charges under acidic conditions, and galacturonic acid of pectic polysaccharide carries negative charges, pectin and protein are adsorbed by electrostatic action to form pectin casein/protein composite colloidal particles, and the colloidal particles can exist stably in a system, so that the stability of the protein is maintained. Meanwhile, only part of pectin and protein interact in an acidic milk system to form pectin/casein composite colloidal particles, and the rest of unadsorbed pectin and pectin/protein composite colloidal particles form a self-supporting weak network structure through calcium bridges.

Application number CN99815310.9 provides a pectin having: a Degree of Esterification (DE) of 60 to 95%; (ii) a calcium sensitivity (Δcs) below 25 cP; and (iii) a weight ratio of Calcium Sensitive Pectin (CSP) to the sum of CSP and non-calcium sensitive pectin (NCSP) (hereinafter referred to as Calcium Sensitive Pectin Ratio (CSPR)) of 0.7 or more. Such pectins are useful as stabilizing components in aqueous acidic beverages such as drinking yoghurt, which contain suspensions of protein particles formed from e.g. casein.

Application number CN201480068608.6 describes a process for extracting calcium sensitive pectin from pectin containing starting materials, as well as pectin products obtained by said process and the use of said products for stabilizing beverages and/or structuring acidified dairy products.

If the addition amount of the calcium-sensitive high-ester pectin in an acidic protein system is low, the calcium-sensitive high-ester pectin is unfavorable for the formation of a weak gel network structure, so that the stabilizing effect of the system is poor; however, if the addition amount is too high, the weak gel network structure can cause obvious increase of the viscosity of the system, so that the taste is thick, the smoothness is insufficient, and even the gel phenomenon occurs.

In summary, in sour milk beverage systems, the requirements for pectin ingredients are higher due to the low protein content and low pH, both the stability of the protein is maintained and too high viscosity cannot be produced, resulting in poor freshness of the product. How to produce a yoghurt drink with not only good protein stability but also a fresh mouthfeel is a problem faced in the art. This places higher demands on the thickening properties, protein stability and flavour release of pectin, which is not met by the common high ester pectins on the market.

Disclosure of Invention

The application aims to provide a preparation method of a high-ester pectin composition, which is characterized in that the high-ester pectin composition comprises a high-ester pectin mixture, buffer salt and sugar, and the preparation method of the high-ester pectin composition comprises the following steps:

s1, squeezing underground tubers of plant raw materials to obtain pomace;

s2, adding 10-40 times of water into the pomace, and regulating pH to 1.5-4.5 by using acid to obtain acidic pomace water;

s3, heating the acidic fruit residue water to 65-95 ℃ for 0.5-5 hours;

s4, sequentially filtering and concentrating the acidic fruit residue water after heating, precipitating with ethanol, and finally drying and crushing to obtain a high-fat pectin mixture, wherein the drying step is performed by adopting a drying device which rotates longitudinally, and the material to be dried is subjected to the processes of continuous dispersion and breaking by the longitudinal rotation of the whole drying device, so that the drying is accelerated, the particle size of the material to be dried is reduced, and the primary crushing of the material is realized;

s5, uniformly mixing the high-fat pectin mixture, the buffer salt and the sugar in a dry mixing mode to obtain the high-ester pectin composition.

In the high-fat pectin composition, most of 3, 6-D-galacturonic acid groups of a pectin main chain are methyl esterified, and at the same time, part of groups are acetylated, so that a stable system is formed between carboxyl groups and proteins in a yogurt system through electrostatic action, and acetyl groups can prevent the carboxyl groups of pectin from forming a network structure through calcium bridges, so that flocculation risk is avoided even under the condition of high addition amount, and the taste is fresh and smooth.

Further, the degree of esterification of the high ester pectin mixture is not less than 55% to 95%, preferably 60% to 90%, and the degree of acetylation of the high ester pectin mixture is not less than 1% to 25%, preferably 5% to 20%.

Further, the viscosity of the high ester pectin composition measured at 23 ℃ in a 2% by weight aqueous solution ranges from 100 to 400 mPa-s, preferably from 150 to 300 mPa-s, and the SAG value (gel degree) of the high ester pectin composition is less than 100, preferably less than 50.

Further, the plant material in the step S1 is one or more of chicory, jerusalem artichoke and beet, and the sugar in the step S5 is at least one of glucose, sucrose, fructose, maltose or trehalose.

Further, the weight ratio of the high ester pectin mixture to the buffer salt to the sugar is 1:1-50%:1-50% buffer salt and sugar, preferably 5-40% of the high ester pectin mixture.

Further, the buffer salt is one or more of sodium gluconate, sodium oxalate, sodium tartrate, sodium citrate, sodium acetate, potassium gluconate, potassium oxalate, potassium tartrate, potassium citrate, potassium acetate, trisodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate and combinations thereof.

Optionally, drying equipment includes the barrel, and barrel inner wall installs heating element, barrel middle part outer end fixedly connected with two relative connecting rods, connecting rod outer end fixedly connected with center pin, two center pins are installed on rotating assembly, barrel bottom fixedly connected with ventilative board, ventilative board upper end middle part fixedly connected with plummer, plummer upper end fixedly connected with fall bulk cargo umbrella, barrel's bung middle part lower extreme fixedly connected with rubber piece, fall bulk cargo umbrella's upper end and rubber piece are contradicted each other.

Further, the falling bulk cargo umbrella includes the random pocket of fixed connection in the plummer upper end, fixed connection is at the electromagnetism bundle club of random pocket upper end and movable sleeve establish the iron ball of pounding on the electromagnetism bundle club, ventilation board upper end fixed mounting has two electric putter, electric putter extension end and random pocket edge fixed connection, when needs are dry, the whole vertical rotation of accessible rotating assembly control barrel, in this in-process, the material is constantly thrown vertically in the barrel, make the material be in the process that developments and constantly dispersed, effectively avoid the material to appear piling up, effectively guarantee its drying efficiency, simultaneously, when random pocket orientation below, control electric putter extension, make random pocket present the umbrella form structure of inversion, be convenient for gather together the material to the center, the iron pound the ball simultaneously under the action of gravity, can fall along the electromagnetism bundle club fast, and pound on the material, can realize the preliminary breakage to the material, make its particle diameter diminish gradually in the drying process, compare with prior art, can reduce the particle diameter in a wide margin and break the initial narrow degree, and then reduce required time and high-input preparation fat.

Further, the variable pocket comprises a variable pocket ring fixedly connected with the bearing table and attached to the inner wall of the cylinder body, and a material gathering layer fixedly connected between the variable pocket ring and the stressed bottom plate, and the connecting part of the electric push rod and the variable pocket is positioned on the variable pocket ring.

Further, the atress bottom plate is the stereoplasm cambered surface structure of undercut, gathers the material layer and is made for flexible ventilative nylon cloth, when the pocket leaves the bottom with becoming, steerable electric putter shortens, drives to become the pocket ring and moves down, and flexible gathers material layer can be deformed along with it this moment, makes the falling bulk cargo umbrella bottom tend to be even, makes at the material along with rotating the dispersion in-process, falls on the material of pocket part along with becoming, is difficult for concentrating towards center department gathering, effectively avoids piling up of material, makes drying uniformity and efficiency higher.

Compared with the prior art, the advantage of this application lies in:

Drawings

FIG. 1 is a main flow block diagram of the present application;

fig. 2 is a perspective view of a drying apparatus according to the present application rotated longitudinally;

FIG. 3 is a schematic view of the drying apparatus of the present application when rotated longitudinally;

FIG. 4 is a perspective view, in semi-section, of a portion of the drying apparatus of the present application;

FIG. 5 is a cross-sectional view of the drying apparatus of the present application;

FIG. 6 is a perspective view of the inverted bulk umbrella of the present application;

FIG. 7 is a front view of the inverted bulk umbrella of the present application;

FIG. 8 is a schematic view of the bottom portion of the inverted bulk umbrella of the present application;

FIG. 9 is a perspective view of the bottom of the inverted bulk umbrella of the present application as it tends to be flat;

fig. 10 is a main flow chart of embodiment 2 of the present application.

The reference numerals in the figures illustrate:

1 barrel, 21 center shaft, 22 connecting rod, 3 ventilative board, 4 electric putter, 51 electromagnetism beam club, 52 iron pound ball, 53 along with becoming pocket, 531 gathers the material layer, 532 atress bottom plate, 533 become the pocket ring, 6 plummer, 7 rubber blocks.

Detailed Description

The embodiments will be described in detail and throughout the specification with reference to the drawings, wherein, based on the embodiments in the application, all other embodiments obtained by persons skilled in the art without making creative efforts are within the scope of protection of the application.

Example 1:

the invention provides a preparation method of a high-ester pectin composition, which comprises a high-ester pectin mixture, buffer salt and sugar, and comprises the following steps:

s1, squeezing underground tubers of plant raw materials to obtain fruit residues, wherein the plant raw materials are one or more of chicory, jerusalem artichoke and beet, the chicory raw materials are chicory residues, the jerusalem artichoke raw materials are jerusalem artichoke residues, and the beet raw materials are beet residues;

s3, heating the acidic fruit residue water to 65-95 ℃ for 0.5-5 hours;

s4, sequentially filtering and concentrating the acidic fruit residue water after heating, precipitating with ethanol, and finally drying and crushing to obtain a high-fat pectin mixture;

s5, uniformly mixing the high-fat pectin mixture with buffer salt and sugar in a dry mixing manner to obtain a high-ester pectin composition;

wherein the sugar is at least one of glucose, sucrose, fructose, maltose or trehalose;

the buffer salt is one or more of sodium gluconate, sodium oxalate, sodium tartrate, sodium citrate, sodium acetate, potassium gluconate, potassium oxalate, potassium tartrate, potassium citrate, potassium acetate, trisodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate and combinations thereof.

The high ester pectin mixture has a degree of esterification of not less than 55% -95%, preferably 60-90%, for example not less than 60%, not less than 61%, not less than 62%.

It is noted that "high-ester pectin" generally refers to pectin having a degree of esterification (e.g., methyl esterification, degree of methoxylation) of not less than 50%, such as 50-80%. In the pectin field, the degree of esterification generally refers to the degree of substitution by esterification.

The high ester pectin mixture has a Degree of Acetylation (DA) of not less than 1-25%, preferably 5-20%, for example not less than 5%, not less than 6%, not less than 7%.

The high ester pectin composition has a viscosity in the range of 100-400 mPa-s, preferably 150-300 mPa-s, e.g. 150 mPa-s, 160 mPa-s, 170 mPa-s, 300 mPa-s, measured at 23 ℃ in a 2% by weight aqueous solution.

The high ester pectin composition has a SAG value (gel degree) of less than 100, preferably less than 50, e.g. less than 50, less than 40.

In the case where the above is satisfied, the protein stability factor of the high-ester pectin composition in this example is not less than 90, preferably not less than 120, i.e., the stability of the protein is good.

The weight ratio of the high-ester pectin mixture to the buffer salt to the sugar is 1:1-50%:1-50%, the buffer salt and sugar preferably comprise 5-40% of the high ester pectin mixture, e.g. in a ratio of 1:10%:10%.

The pectin from different plant sources is used as a raw material to develop a high-ester pectin composition for fermentation type milk-containing beverage, preparation type milk-containing beverage, lactobacillus beverage, vegetable protein beverage, compound protein beverage and the like, wherein most of 3, 6-D-galactoaldehyde acid groups of a pectin main chain in the high-ester pectin composition are methyl esterified, and part of groups are acetylated at the same time, so that the pectin forms a stable system between carboxyl groups and proteins through electrostatic action in a yogurt system, and acetyl groups can prevent the carboxyl groups of the pectin from forming a network structure through calcium bridges, thereby realizing no flocculation risk and fresh and smooth mouthfeel even under the condition of high addition amount.

The following is the application and detection of the high-performance pectin product in sour milk beverage, wherein the esterification degree and the acetylation degree of the pectin sample are measured by high performance liquid chromatography.

Pectin preparation is first performed:

product index and detection result table:

application experiment: a yogurt drink product was prepared from the pectin products in samples 1-9 above.

1. Yoghurt base material and process (fat content 0%, protein content 4.0%)

Adding skimmed milk powder and glucose powder into 50deg.C water, stirring, and keeping warm for 30min; heating to 65deg.C, homogenizing at 50/200 bar; preserving heat for about 2.5 hours at the temperature of 90-95 ℃ and browning; cooling to 42 ℃ for fermentation for 20 hours; and after the fermentation is finished by 100-120OT, demulsification and refrigeration are carried out for standby.

2. Brown milk formula and process: (fat content 0%, protein content 1%)

Wherein sample 10 is commercially available pectin product YM150H.

Uniformly mixing a stabilizer and white granulated sugar; adding into purified water at 85deg.C, stirring for 15min, and checking dispersity; cooling the feed liquid to below 30deg.C, adding yogurt, and mixing; adjusting pH to 3.6+ -0.05 with acid liquor, and fixing volume to total amount; heating the material to a temperature of 65 ℃ and homogenizing at 200bar (200/50 bar); canning, sterilizing in water bath at 90deg.C for 25 min, and cooling.

And (3) detecting the characteristics of the yogurt drink:

the detection items are as follows:

centrifugal sedimentation rate: taking 15 ml of sour milk beverage, and centrifuging: 4000rpm X10 min, room temperature.

Viscosity of yogurt beverage: a viscometer: model Brookfield DV-II, 64# rotor 60r/min, pH 4.20 measured at 23 ℃.

Mouthfeel: the products were evaluated for freshness and smoothness (in 5 points) by 12 professional sensory panelists.

Product application evaluation table:

numbering device	Centrifugal sedimentation rate	Viscosity of the mixture	Fresh and cool degree	Smoothness degree of smoothness
					1	0.68	6.95	3	4
2	0.53	8.15	2	3
					3	0.36	5.71	4	5
4	0.64	6.60	4	4
					5	0.72	4.45	2	4
6	0.80	5.63	4	3
					7	0.40	6.55	4	5
8	0.65	8.30	3	3
					9	0.67	13.43	1	2
10	1.53	3.38	4	2

The results in the above table can be seen:

the high-fat pectin composition can be used as a food additive to obtain a sour milk beverage which is moderate in thickness, fresh and smooth in taste and high in stability, has no gel risk especially under high addition amount, and is suitable for fermentation type milk-containing beverages, preparation type milk-containing beverages, lactobacillus beverages, vegetable protein beverages, compound protein beverages and the like.

Example 2:

in this example, the following was added to the example 1, and the rest was the same as in example 1.

Referring to fig. 9, in step S4, as shown in fig. 2-3, the drying step is performed by using a drying device that rotates longitudinally, and the material to be dried is continuously dispersed and crashed through the longitudinal rotation of the whole drying device, so as to accelerate the drying, and simultaneously reduce the particle size of the material to be dried, thereby realizing the primary crushing of the material.

Referring to fig. 4-5, the drying apparatus includes a barrel 1, a heating assembly is installed on the inner wall of the barrel 1, two opposite connecting rods 22 are fixedly connected to the outer end of the middle part of the barrel 1, a central shaft 21 is fixedly connected to the outer end of each connecting rod 22, the two central shafts 21 are installed on the rotating assembly, an air permeable plate 3 is fixedly connected to the bottom of the barrel 1, a bearing table 6 is fixedly connected to the middle part of the upper end of the air permeable plate 3, an inverted bulk material umbrella is fixedly connected to the upper end of the bearing table 6, a rubber block 7 is fixedly connected to the lower end of the middle part of a barrel cover of the barrel 1, and the upper end of the inverted bulk material umbrella is mutually abutted to the rubber block 7.

As shown in figure 6, the inverted bulk material umbrella comprises a random pocket 53 fixedly connected to the upper end of a bearing table 6, an electromagnetic beam ball 51 fixedly connected to the upper end of the random pocket 53, and an iron smashing ball 52 movably sleeved on the electromagnetic beam ball 51, wherein two electric push rods 4 are fixedly arranged at the upper end of the air permeable plate 3, the extending ends of the electric push rods 4 are fixedly connected with the edges of the random pocket 53, when drying is needed, the whole longitudinal rotation of the barrel 1 can be controlled through a rotating assembly, in the process, materials are continuously and longitudinally thrown in the barrel 1, the materials are in a dynamic and continuously dispersed process, accumulation of the materials is effectively avoided, drying efficiency is effectively guaranteed, meanwhile, when the random pocket 53 faces downwards, the electric push rods 4 are controlled to extend, the random pocket 53 is in an inverted umbrella-shaped structure, the materials are conveniently gathered to the center, the iron smashing ball 52 can rapidly drop along the electromagnetic beam ball 51 under the action of gravity, and can be initially smashed on the materials, the primary smashing of the materials is achieved, the primary smashing of the materials in the drying process is gradually reduced, and the particle size is greatly reduced compared with the prior art, and the primary smashing efficiency is greatly reduced, and the required primary smashing time is greatly reduced.

The variable pocket 53 comprises a force-bearing bottom plate 532 fixedly connected with the bearing table 6, a variable pocket ring 533 attached to the inner wall of the cylinder body 1 and a material gathering layer 531 fixedly connected between the variable pocket ring 533 and the force-bearing bottom plate 532, wherein the connecting part of the electric push rod 4 and the variable pocket 53 is positioned on the variable pocket ring 533, the force-bearing bottom plate 532 is of a hard cambered surface structure which is concave downwards, the material gathering layer 531 is made of flexible breathable nylon cloth, as shown in fig. 9, when the variable pocket 53 leaves the bottom, the electric push rod 4 can be controlled to shorten to drive the variable pocket ring 533 to move downwards, at the moment, the flexible material gathering layer 531 can deform along with the variable pocket ring, so that the bottom of the inverted bulk material umbrella tends to be flat, materials falling on the variable pocket 53 part are difficult to gather towards the center in the process of rotating and dispersing along with the rotation, the accumulation of materials is effectively avoided, and the drying uniformity and the efficiency are higher.

It is worth noting that, the electromagnetism beam ball 51 runs through the random pocket 53 and is electrically connected with the plummer 6, when the random pocket 53 faces upwards, the iron ball smashing 52 is located at one end of the electromagnetism beam ball 51 far away from the random pocket 53 under the action of gravity, at this time, the iron ball smashing 52 is controlled to be electrified, magnetism is generated, the iron ball smashing 52 is adsorbed, the position of the iron ball smashing 52 can be limited, when the random pocket 53 rotates to the right below, the power is cut off again, the material falls behind the random pocket 53, and the smashing and crushing effects of the iron ball smashing 52 on the material are effectively guaranteed.

The foregoing is merely a preferred embodiment of the present application, which is used in connection with the actual requirement, but the scope of the present application is not limited thereto.

Claims

1. A method of preparing a high ester pectin composition comprising a high ester pectin mixture, a buffer salt and a sugar, the method comprising the steps of:

s1, squeezing underground tubers of plant raw materials to obtain pomace;

s3, heating the acidic fruit residue water to 65-95 ℃ for 0.5-5 hours;

2. A method of preparing a high ester pectin composition according to claim 1 wherein the high ester pectin mixture has a degree of esterification of not less than 55% to 95% and the high ester pectin mixture has a degree of acetylation of not less than 1% to 25%.

3. A method of preparing a high ester pectin composition according to claim 1 wherein the high ester pectin composition has a viscosity in the range of 100-400 mPa-s when tested in a 2% by weight aqueous solution at 23 ℃ and the high ester pectin composition has a gel degree of less than 100.

4. The method for preparing a high ester pectin composition according to claim 1, wherein the plant material in the step S1 is one or more of chicory, jerusalem artichoke and beet, and the sugar in the step S5 is at least one of glucose, sucrose, fructose, maltose or trehalose.

5. The method of preparing a high ester pectin composition of claim 4 wherein the high ester pectin mixture, the buffer salt and the sugar are present in a weight ratio of 1:1-50%:1-50%.

6. The method of claim 5, wherein the buffer salt is one or more of sodium gluconate, sodium oxalate, sodium tartrate, sodium citrate, sodium acetate, potassium gluconate, potassium oxalate, potassium tartrate, potassium citrate, potassium acetate, trisodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, and combinations thereof.

7. The preparation method of the high-ester pectin composition according to claim 6, wherein the drying equipment comprises a barrel (1), a heating assembly is installed on the inner wall of the barrel (1), two opposite connecting rods (22) are fixedly connected to the outer end of the middle part of the barrel (1), a central shaft (21) is fixedly connected to the outer end of each connecting rod (22), the two central shafts (21) are installed on the rotating assembly, a ventilation plate (3) is fixedly connected to the bottom of the barrel (1), a bearing table (6) is fixedly connected to the middle part of the upper end of the ventilation plate (3), an inverted bulk material umbrella is fixedly connected to the upper end of the bearing table (6), a rubber block (7) is fixedly connected to the lower end of the middle part of a barrel cover of the barrel (1), and the upper end of the inverted bulk material umbrella is mutually abutted to the rubber block (7).

8. The preparation method of the high-ester pectin composition according to claim 7, wherein the inverted bulk umbrella comprises a variable pocket (53) fixedly connected to the upper end of a bearing table (6), an electromagnetic beam ball (51) fixedly connected to the upper end of the variable pocket (53) and an iron smashing ball (52) movably sleeved on the electromagnetic beam ball (51), two electric push rods (4) are fixedly arranged at the upper end of the ventilation plate (3), and the extension end of each electric push rod (4) is fixedly connected with the edge of the variable pocket (53).

9. The method for preparing the high-ester pectin composition according to claim 8, wherein the variable pocket (53) comprises a variable pocket ring (533) fixedly connected with the bearing table (6) and attached to the inner wall of the barrel (1), and a polymeric layer (531) fixedly connected between the variable pocket ring (533) and the stressed bottom plate (532), and the connection part of the electric push rod (4) and the variable pocket (53) is positioned on the variable pocket ring (533).

10. The method for preparing the high-ester pectin composition according to claim 9, wherein the stress bottom plate (532) is a hard cambered surface structure recessed downwards, and the polymer layer (531) is made of flexible and breathable nylon cloth.