Purification treatment method for soluble sugar in fruits and vegetables

文档序号:527260 发布日期:2021-06-01 浏览:10次 中文

阅读说明:本技术 一种果蔬中可溶性糖的净化处理方法 (Purification treatment method for soluble sugar in fruits and vegetables ) 是由 赵江丽 关军锋 程玉豆 于 2020-12-28 设计创作,主要内容包括:本发明涉及一种果蔬中可溶性糖的净化处理方法,包括:制备样品溶液,以得到含有杂质的可溶糖原液,提取可溶糖原液,并对所述可溶糖原液进行净化或富集,以分离可溶糖原液中的可溶性糖和杂质,并得到待测滤液。通过加入某一种或几种对有机酸、多酚、黄酮、叶绿素等有吸附作用,而对单糖不吸附的固体粉末吸附材料,实现了果糖测定样品的除杂,保证了可溶性糖测定样品的纯度,提高了后续测定准确性。(The invention relates to a purification treatment method of soluble sugar in fruits and vegetables, which comprises the following steps: preparing a sample solution to obtain soluble sugar stock solution containing impurities, extracting the soluble sugar stock solution, purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution, and obtaining a filtrate to be detected. By adding one or more solid powder adsorbing materials which have an adsorbing effect on organic acids, polyphenols, flavones, chlorophyll and the like and do not adsorb monosaccharides, impurity removal of a fructose determination sample is realized, the purity of a soluble sugar determination sample is ensured, and the subsequent determination accuracy is improved.)

1. A purification treatment method for soluble sugar in fruits and vegetables is characterized by comprising the following steps:

preparing a sample solution to obtain a soluble sugar stock solution containing impurities;

extracting soluble sugar stock solution, and purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution and obtain a filtrate to be detected.

2. The purification treatment method according to claim 1, wherein the preparing of the sample solution to obtain the soluble sugar stock solution containing impurities specifically comprises:

taking 1.0g of fruit and vegetable pulp, peel or kernel, adding 10mL of 80% ethanol solution, carrying out ultrasonic extraction in a water bath at 40 ℃ for 30min, carrying out centrifugation at 4 ℃ and 10000prm for 10min, taking supernatant, re-extracting the residue with 5mL of 80% ethanol solution once, combining the supernatant, and carrying out constant volume to 25mL with 80% acetonitrile to obtain the soluble sugar stock solution.

3. The purification treatment method according to claim 1, wherein the extracting and purifying the soluble sugar raw solution specifically comprises:

and taking the soluble sugar stock solution, sequentially adding an organic acid adsorption material, a polyphenol adsorption material, a flavone adsorption material and a chlorophyll adsorption material, carrying out vortex adsorption and centrifugation, and filtering the supernatant through a 0.45-micrometer filter membrane to obtain the filtrate to be detected.

4. The purification treatment method according to claim 3, wherein the organic acid adsorbent is a strongly basic anion exchange resin having a polystyrene skeleton.

5. The purification treatment method according to claim 3, wherein the organic acid adsorption process comprises:

introducing 25mL of strong-base anion exchange resin with polystyrene as a basic skeleton into soluble sugar stock solution with the concentration of 1-50 g.L < -1 > and the pH value of 8.3-5.1 to obtain mixed solution, placing the mixed solution in a constant-temperature water bath shaking table at the temperature of 20-60 ℃ to shake and adsorb for 1-3 h, and filtering to obtain filtrate after organic acid is removed.

6. The purification treatment method according to claim 3, wherein the polyphenol adsorbent material is a lignocellulose composite material.

7. The purification process of claim 6, wherein the preparation of the lignocellulosic composite material comprises the steps of:

weighing 1-5 parts by mass of chitosan, adding water according to the proportion that 1 part of chitosan is matched with 9-11 ml of water, and then dripping glacial acetic acid until the chitosan is dissolved to obtain a chitosan solution;

weighing 1-2 times of gelatin by weight of chitosan, adding distilled water into the gelatin, and heating until the gelatin is melted to obtain a gelatin solution, wherein the dosage ratio of the distilled water to the gelatin is 3.6-20 ml: 1g of a compound;

pouring the gelatin solution into the chitosan solution, adding 1 part by weight of lignocellulose, uniformly stirring, freeze-drying, dispersing, and performing heat treatment at 80-140 ℃ for 1.5-2.5 h;

obtaining the lignocellulose composite material.

8. The purification treatment method according to claim 3, wherein the flavone adsorption material is flavonoid glycoside adsorption resin APBA/pGMA/macroporous resin.

9. The purification treatment method according to claim 6, wherein the preparation method of the macroporous resin comprises the following steps:

pretreating macroporous resin;

taking glycidyl methacrylate as a functional monomer, and grafting an organic long-chain polymer on the surface of the macroporous resin through a free radical chain reaction to obtain a grafting material pGMA/macroporous resin;

3-aminophenylboronic acid is taken as a ring-opening reaction substance, and a boronic acid group is introduced into a chain link of the organic long-chain polymer through an epoxy ring-opening reaction to obtain the flavonoid glycoside adsorption resin APBA/pGMA/macroporous resin.

10. The purification treatment method according to claim 3, wherein the chlorophyll-adsorbing material is silica powder.

Technical Field

The invention relates to the technical field of fructose purification, in particular to a purification treatment method of soluble sugar in fruits and vegetables.

Background

The chemical components of fruits and vegetables are very complex: the chromatographic column comprises chlorophyll, fatty acid, terpenes, flavonoids, nucleosides, polyphenols, organic acid, water-soluble vitamins, amino acids, monosaccharides, disaccharides, polysaccharides, proteins and the like, and a plurality of components can interfere with different types of liquid phase analysis or form dead adsorption on the chromatographic column to shorten the service life of the chromatographic column, thereby increasing the instability and cost of detection.

At present, monosaccharide and disaccharide are mainly measured by pre-column derivatization gas (gas) chromatography, pre-column derivatization liquid chromatography, ion chromatography and liquid chromatography. Various derivatization methods have the characteristics of complex operation, reagent toxicity and the like; the cation chromatographic column, the anion chromatographic column and the special sugar column have the problem of poor separation performance. At present, the column separation effect is better by an amino column and an amide column, but the two chromatographic columns have strong adsorbability on strong-polarity organic acid, Vc and other acidic components, and are easy to form dead adsorption to reduce the column effect; in addition, the polysaccharide and the protein with lower polymerization degree have good retention performance on the two chromatographic columns, are not easy to wash out, and can be accumulated in the chromatographic columns to reduce the column efficiency.

Therefore, the method for purifying soluble sugar in fruits and vegetables is provided, so that the impurity removal of a fructose determination sample is realized, the purity of the soluble sugar determination sample is ensured, and the subsequent determination accuracy is improved, and the method becomes a problem to be solved by the technical staff in the field.

Disclosure of Invention

The invention aims to provide a purification treatment method of soluble sugar in fruits and vegetables, which is used for removing impurities from a fructose determination sample, ensuring the purity of the soluble sugar determination sample and improving the accuracy of subsequent determination.

In order to achieve the purpose, the technical scheme provided by the invention is as follows:

a purification treatment method for soluble sugar in fruits and vegetables comprises the following steps:

preparing a sample solution to obtain a soluble sugar stock solution containing impurities;

extracting soluble sugar stock solution, and purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution and obtain a filtrate to be detected.

Further, the preparing the sample solution to obtain the soluble sugar stock solution containing impurities specifically comprises:

taking 1.0g of fruit and vegetable pulp, peel or kernel, adding 10mL of 80% ethanol solution, carrying out ultrasonic extraction in a water bath at 40 ℃ for 30min, carrying out centrifugation at 4 ℃ and 10000prm for 10min, taking supernatant, re-extracting the residue with 5mL of 80% ethanol solution once, combining the supernatant, and carrying out constant volume to 25mL with 80% acetonitrile to obtain the soluble sugar stock solution.

Further, the extracting the soluble sugar stock solution and purifying the soluble sugar stock solution specifically comprise:

and taking the soluble sugar stock solution, sequentially adding an organic acid adsorption material, a polyphenol adsorption material, a flavone adsorption material and a chlorophyll adsorption material, carrying out vortex adsorption and centrifugation, and filtering the supernatant through a 0.45-micrometer filter membrane to obtain the filtrate to be detected.

Further, the organic acid adsorption material is strongly basic anion exchange resin with polystyrene as a basic skeleton.

Further, the organic acid adsorption process comprises:

introducing 25mL of strong-base anion exchange resin with polystyrene as a basic skeleton into soluble sugar stock solution with the concentration of 1-50 g.L < -1 > and the pH value of 8.3-5.1 to obtain mixed solution, placing the mixed solution in a constant-temperature water bath shaking table at the temperature of 20-60 ℃ to shake and adsorb for 1-3 h, and filtering to obtain filtrate after organic acid is removed.

Further, the polyphenol adsorbing material is a lignocellulose composite material.

Further, the preparation of the lignocellulose composite material comprises the following steps:

weighing 1-5 parts by mass of chitosan, adding water according to the proportion that 1 part of chitosan is matched with 9-11 ml of water, and then dripping glacial acetic acid until the chitosan is dissolved to obtain a chitosan solution;

weighing 1-2 times of gelatin by weight of chitosan, adding distilled water into the gelatin, and heating until the gelatin is melted to obtain a gelatin solution, wherein the dosage ratio of the distilled water to the gelatin is 3.6-20 ml: 1g of a compound;

pouring the gelatin solution into the chitosan solution, adding 1 part by weight of lignocellulose, uniformly stirring, freeze-drying, dispersing, and performing heat treatment at 80-140 ℃ for 1.5-2.5 h;

obtaining the lignocellulose composite material.

Further, the flavone adsorption material is flavonoid glycoside adsorption resin APBA/pGMA/macroporous resin.

Further, the preparation method of the macroporous resin comprises the following steps:

pretreating macroporous resin;

taking glycidyl methacrylate as a functional monomer, and grafting an organic long-chain polymer on the surface of the macroporous resin through a free radical chain reaction to obtain a grafting material pGMA/macroporous resin;

3-aminophenylboronic acid is taken as a ring-opening reaction substance, and a boronic acid group is introduced into a chain link of the organic long-chain polymer through an epoxy ring-opening reaction to obtain the flavonoid glycoside adsorption resin APBA/pGMA/macroporous resin.

Further, the chlorophyll adsorbing material is silicon dioxide powder.

The technical scheme provided by the invention has the following beneficial effects: the invention provides a purification treatment method of soluble sugar in fruits and vegetables, which comprises the steps of preparing a sample solution to obtain a soluble sugar stock solution containing impurities, extracting the soluble sugar stock solution, purifying or enriching the soluble sugar stock solution to separate the soluble sugar and the impurities in the soluble sugar stock solution, and obtaining a filtrate to be detected. By adding one or more solid powder adsorbing materials which have an adsorbing effect on organic acids, polyphenols, flavones, chlorophyll and the like and do not adsorb monosaccharides, impurity removal of a fructose determination sample is realized, the purity of a soluble sugar determination sample is ensured, and the subsequent determination accuracy is improved.

Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.

Detailed Description

The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.

The experimental procedures in the following examples are conventional unless otherwise specified. The test materials used in the following examples were purchased from a conventional reagent store unless otherwise specified. In the quantitative tests in the following examples, three replicates were set, and the data are the mean or the mean ± standard deviation of the three replicates.

The raw material components for preparing the chemical root-resisting agent are used as proportioning according to parts by weight, and can be increased or reduced according to corresponding proportion during production, for example, the weight can be increased or reduced by taking kilogram or ton as a unit during large-scale production and taking gram as a unit during small-scale production, but the mass proportioning proportion among the components is not changed.

The invention provides a purification treatment method of soluble sugar in fruits and vegetables, which comprises the following steps:

preparing a sample solution to obtain a soluble sugar stock solution containing impurities; specifically, 1.0g of fruit and vegetable pulp, peel or kernel is taken, 10mL of 80% ethanol solution is added, ultrasonic extraction is carried out in water bath at 40 ℃ for 30min, centrifugation is carried out at 4 ℃ and 10000prm for 10min, supernatant is taken, residues are re-extracted once by 5mL of 80% ethanol solution, supernatant is combined, 80% acetonitrile is used for fixing the volume to 25mL, and the soluble sugar stock solution is obtained.

Extracting soluble sugar stock solution, and purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution and obtain a filtrate to be detected. Specifically, adding an organic acid adsorption material, a polyphenol adsorption material, a flavone adsorption material and a chlorophyll adsorption material into soluble sugar stock solution in sequence, carrying out vortex adsorption and centrifugation, and filtering supernate through a 0.45-micrometer filter membrane to obtain a filtrate to be detected. Wherein the chlorophyll adsorbing material is conventional silicon dioxide powder.

Preferably, the organic acid adsorbing material is strong-base anion exchange resin with polystyrene as basic skeleton, specifically can be one of D201, D290, Amberlite IRA-401, Dower 1X 4, Amberlite IRA-900 and Diaion SA-161, and is preferably macroporous adsorbing resin D201. Wherein, the organic acid adsorption process comprises the following steps: introducing 25mL of strong-base anion exchange resin with polystyrene as a basic skeleton into soluble sugar stock solution with the concentration of 1-50 g.L < -1 > and the pH value of 8.3-5.1 to obtain mixed solution, placing the mixed solution in a constant-temperature water bath shaking table at the temperature of 20-60 ℃ to shake and adsorb for 1-3 h, and filtering to obtain filtrate after organic acid is removed.

The polyphenol adsorption material is a lignocellulose composite material, and in order to ensure the polyphenol adsorption effect, the preparation of the lignocellulose composite material comprises the following steps:

weighing 1-5 parts by mass of chitosan, adding water according to the proportion that 1 part of chitosan is matched with 9-11 ml of water, and then dripping glacial acetic acid until the chitosan is dissolved to obtain a chitosan solution;

weighing 1-2 times of gelatin by weight of chitosan, adding distilled water into the gelatin, and heating until the gelatin is melted to obtain a gelatin solution, wherein the dosage ratio of the distilled water to the gelatin is 3.6-20 ml: 1g of a compound;

pouring the gelatin solution into the chitosan solution, adding 1 part by weight of lignocellulose, uniformly stirring, freeze-drying, dispersing, and performing heat treatment at 80-140 ℃ for 1.5-2.5 h;

obtaining the lignocellulose composite material.

Further, the flavone adsorption material is flavonoid glycoside adsorption resin APBA/pGMA/macroporous resin. In order to ensure the adsorption effect of flavone, the preparation method of the macroporous resin comprises the following steps:

pretreating macroporous resin;

taking glycidyl methacrylate as a functional monomer, and grafting an organic long-chain polymer on the surface of the macroporous resin through a free radical chain reaction to obtain a grafting material pGMA/macroporous resin;

3-aminophenylboronic acid is taken as a ring-opening reaction substance, and a boronic acid group is introduced into a chain link of the organic long-chain polymer through an epoxy ring-opening reaction to obtain the flavonoid glycoside adsorption resin APBA/pGMA/macroporous resin.

The technical solution provided by the present invention is further illustrated below with reference to specific examples.

Example 1

In this example 1, the method provided by the present invention comprises the steps of:

s101: preparing a sample solution to obtain a soluble sugar stock solution containing impurities; specifically, 1.0g of fruit and vegetable pulp is taken, 10mL of 80% ethanol solution is added, ultrasonic extraction is carried out in water bath at 40 ℃ for 30min, centrifugation is carried out at 4 ℃ and 10000prm for 10min, supernate is taken, 5mL of 80% ethanol solution is used for re-extracting residues once, the supernate is combined, 80% acetonitrile is used for fixing the volume to 25mL, and the soluble sugar stock solution is obtained.

S102: extracting soluble sugar stock solution, and purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution and obtain a filtrate to be detected. Specifically, adding an organic acid adsorption material, a polyphenol adsorption material, a flavone adsorption material and a chlorophyll adsorption material into soluble sugar stock solution in sequence, carrying out vortex adsorption and centrifugation, and filtering supernate through a 0.45-micrometer filter membrane to obtain a filtrate to be detected.

Wherein the chlorophyll adsorbing material is conventional silicon dioxide powder; the organic acid adsorbing material is macroporous adsorption resin D201. The organic acid adsorption process comprises the following steps: introducing strongly basic anion exchange resin with polystyrene as basic skeleton into 25mL soluble sugar stock solution with concentration of 30 g.L < -1 > and pH of about 7 to obtain mixed solution, placing the mixed solution in a constant-temperature water bath shaking table at 40 ℃ to shake and adsorb for 2h, and filtering to obtain filtrate after organic acid is removed with impurities.

In step S102, the polyphenol adsorption material is a lignocellulose composite material, and in order to ensure the polyphenol adsorption effect, the preparation of the lignocellulose composite material includes the following steps:

weighing 3 parts by mass of chitosan, adding water according to the proportion that 1 part of chitosan is matched with 10ml of water, and then dripping glacial acetic acid until the chitosan is dissolved to obtain a chitosan solution;

weighing 1 weight time of gelatin of chitosan, adding distilled water into the gelatin, and heating until the gelatin is melted to obtain a gelatin solution, wherein the dosage ratio of the distilled water to the gelatin is 10 ml: 1g of a compound;

pouring the gelatin solution into the chitosan solution, adding 1 part by weight of lignocellulose, uniformly stirring, freeze-drying, dispersing, and performing heat treatment at 100 ℃ for 2 hours;

obtaining the lignocellulose composite material.

Example 2

In this example 2, the method provided by the present invention comprises the steps of:

s201: preparing a sample solution to obtain a soluble sugar stock solution containing impurities; specifically, 1.0g of fruit and vegetable pulp is taken, 10mL of 80% ethanol solution is added, ultrasonic extraction is carried out in water bath at 40 ℃ for 30min, centrifugation is carried out at 4 ℃ and 10000prm for 10min, supernate is taken, 5mL of 80% ethanol solution is used for re-extracting residues once, the supernate is combined, 80% acetonitrile is used for fixing the volume to 25mL, and the soluble sugar stock solution is obtained.

S202: extracting soluble sugar stock solution, and purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution and obtain a filtrate to be detected. Specifically, adding an organic acid adsorption material, a polyphenol adsorption material, a flavone adsorption material and a chlorophyll adsorption material into soluble sugar stock solution in sequence, carrying out vortex adsorption and centrifugation, and filtering supernate through a 0.45-micrometer filter membrane to obtain a filtrate to be detected.

Wherein the chlorophyll adsorbing material is conventional silicon dioxide powder; the organic acid adsorption material is macroporous adsorption resin D290. The organic acid adsorption process comprises the following steps: introducing strongly basic anion exchange resin with polystyrene as basic skeleton into 25mL soluble sugar stock solution with concentration of 15 g.L < -1 > and pH of about 8 to obtain mixed solution, placing the mixed solution in a 35 ℃ constant temperature water bath shaking table for shaking adsorption for 2h, and filtering to obtain filtrate after organic acid is removed with impurities.

In step S202, the polyphenol adsorption material is a lignocellulose composite material, and in order to ensure the polyphenol adsorption effect, the preparation of the lignocellulose composite material includes the following steps:

weighing 2 parts by mass of chitosan, adding water according to the proportion that 1 part of chitosan is matched with 9ml of water, and then dripping glacial acetic acid until the chitosan is dissolved to obtain a chitosan solution;

weighing 1 weight time of gelatin of chitosan, adding distilled water into the gelatin, and heating until the gelatin is melted to obtain a gelatin solution, wherein the dosage ratio of the distilled water to the gelatin is 12 ml: 1g of a compound;

pouring the gelatin solution into the chitosan solution, adding 1 part by weight of lignocellulose, uniformly stirring, freeze-drying, dispersing, and performing heat treatment at 120 ℃ for 2.2 hours;

obtaining the lignocellulose composite material.

Example 3

In this example 3, the method provided by the present invention comprises the steps of:

s301: preparing a sample solution to obtain a soluble sugar stock solution containing impurities; specifically, 1.0g of fruit and vegetable kernels are taken, 10mL of 80% ethanol solution is added, ultrasonic extraction is carried out in water bath at 40 ℃ for 30min, centrifugation is carried out at 4 ℃ and 10000prm for 10min, supernate is taken, 5mL of 80% ethanol solution is used for re-extracting residues once, the supernate is combined, 80% acetonitrile is used for fixing the volume to 25mL, and the soluble sugar stock solution is obtained.

S302: extracting soluble sugar stock solution, and purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution and obtain a filtrate to be detected. Specifically, adding an organic acid adsorption material, a polyphenol adsorption material, a flavone adsorption material and a chlorophyll adsorption material into soluble sugar stock solution in sequence, carrying out vortex adsorption and centrifugation, and filtering supernate through a 0.45-micrometer filter membrane to obtain a filtrate to be detected.

Wherein the chlorophyll adsorbing material is conventional silicon dioxide powder; the organic acid adsorption material is macroporous adsorption resin Amberlite eIRA-401. The organic acid adsorption process comprises the following steps: introducing strongly basic anion exchange resin with polystyrene as basic skeleton into 25mL of soluble sugar stock solution with the concentration of 35 g.L < -1 > and the pH value of about 6 to obtain a mixed solution, placing the mixed solution in a constant-temperature water bath shaking table at 38 ℃, vibrating and adsorbing for 2h, and filtering to obtain a filtrate after organic acid is removed with impurities.

In step S302, the polyphenol adsorption material is a lignocellulose composite material, and in order to ensure the polyphenol adsorption effect, the preparation of the lignocellulose composite material includes the following steps:

weighing 4 parts by mass of chitosan, adding water according to the proportion relationship of 1 part of chitosan and 10.5ml of water, and then dripping glacial acetic acid until the chitosan is dissolved to obtain a chitosan solution;

weighing 1.5 times of gelatin by weight of chitosan, adding distilled water into the gelatin, and heating until the gelatin is melted to obtain a gelatin solution, wherein the dosage ratio of the distilled water to the gelatin is 15 ml: 1g of a compound;

pouring the gelatin solution into the chitosan solution, adding 1 part by weight of lignocellulose, uniformly stirring, freeze-drying, dispersing, and performing heat treatment at 120 ℃ for 1.8 hours;

obtaining the lignocellulose composite material.

Example 4

In this example 4, the method provided by the present invention comprises the steps of:

s401: preparing a sample solution to obtain a soluble sugar stock solution containing impurities; specifically, 1.0g of fruit and vegetable peel is taken, 10mL of 80% ethanol solution is added, ultrasonic extraction is carried out in water bath at 40 ℃ for 30min, centrifugation is carried out at 4 ℃ and 10000prm for 10min, the supernatant is taken, 5mL of 80% ethanol solution is used for re-extracting the residue once, the supernatants are combined, and the volume is determined to be 25mL by 80% acetonitrile, so as to obtain the soluble sugar stock solution.

S402: extracting soluble sugar stock solution, and purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution and obtain a filtrate to be detected. Specifically, adding an organic acid adsorption material, a polyphenol adsorption material, a flavone adsorption material and a chlorophyll adsorption material into soluble sugar stock solution in sequence, carrying out vortex adsorption and centrifugation, and filtering supernate through a 0.45-micrometer filter membrane to obtain a filtrate to be detected.

Wherein the chlorophyll adsorbing material is conventional silicon dioxide powder; the organic acid adsorbing material is macroporous adsorbent resin Dower1 × 4. The organic acid adsorption process comprises the following steps: introducing strongly basic anion exchange resin with polystyrene as basic skeleton into 25mL soluble sugar stock solution with concentration of 40 g.L < -1 > and pH of about 5.5 to obtain mixed solution, placing the mixed solution in a 43 ℃ constant temperature water bath shaking table for vibration adsorption for 2h, and filtering to obtain filtrate after organic acid is removed with impurities.

In step S402, the polyphenol adsorption material is a lignocellulose composite material, and to ensure the polyphenol adsorption effect, the preparation of the lignocellulose composite material includes the following steps:

weighing 2 parts by mass of chitosan, adding water according to the proportion of 1 part of chitosan and 9.5ml of water, and then dripping glacial acetic acid until the chitosan is dissolved to obtain a chitosan solution;

weighing 1.5 times of gelatin by weight of chitosan, adding distilled water into the gelatin, and heating until the gelatin is melted to obtain a gelatin solution, wherein the dosage ratio of the distilled water to the gelatin is 16 ml: 1g of a compound;

pouring the gelatin solution into the chitosan solution, adding 1 part by weight of lignocellulose, uniformly stirring, freeze-drying, dispersing, and performing heat treatment at 110 ℃ for 2 hours;

obtaining the lignocellulose composite material.

Example 5

In this example 5, the method provided by the present invention comprises the steps of:

s501: preparing a sample solution to obtain a soluble sugar stock solution containing impurities; specifically, 1.0g of fruit and vegetable pulp is taken, 10mL of 80% ethanol solution is added, ultrasonic extraction is carried out in water bath at 40 ℃ for 30min, centrifugation is carried out at 4 ℃ and 10000prm for 10min, supernate is taken, 5mL of 80% ethanol solution is used for re-extracting residues once, the supernate is combined, 80% acetonitrile is used for fixing the volume to 25mL, and the soluble sugar stock solution is obtained.

S502: extracting soluble sugar stock solution, and purifying or enriching the soluble sugar stock solution to separate soluble sugar and impurities in the soluble sugar stock solution and obtain a filtrate to be detected. Specifically, adding an organic acid adsorption material, a polyphenol adsorption material, a flavone adsorption material and a chlorophyll adsorption material into soluble sugar stock solution in sequence, carrying out vortex adsorption and centrifugation, and filtering supernate through a 0.45-micrometer filter membrane to obtain a filtrate to be detected.

Wherein the chlorophyll adsorbing material is conventional silicon dioxide powder; the organic acid adsorption material is macroporous adsorption resin Amberlite IRA-900. The organic acid adsorption process comprises the following steps: introducing strongly basic anion exchange resin with polystyrene as basic skeleton into 25mL soluble sugar stock solution with concentration of 15 g.L < -1 > and pH of about 6.5 to obtain mixed solution, placing the mixed solution in a constant-temperature water bath shaking table at 30 ℃ to shake and adsorb for 1.5h, and filtering to obtain filtrate after organic acid is removed with impurities.

In step S502, the polyphenol adsorption material is a lignocellulose composite material, and in order to ensure the polyphenol adsorption effect, the preparation of the lignocellulose composite material includes the following steps:

weighing 3.5 parts by mass of chitosan, adding water according to the proportion relationship of 1 part of chitosan and 9.8ml of water, and then dripping glacial acetic acid until the chitosan is dissolved to obtain a chitosan solution;

weighing 1 weight time of gelatin of chitosan, adding distilled water into the gelatin, and heating until the gelatin is melted to obtain a gelatin solution, wherein the dosage ratio of the distilled water to the gelatin is 18 ml: 1g of a compound;

pouring the gelatin solution into the chitosan solution, adding 1 part by weight of lignocellulose, uniformly stirring, freeze-drying, dispersing, and performing heat treatment at 140 ℃ for 2 hours;

obtaining the lignocellulose composite material.

Comparative example 1

Taking 1.0g of fruit and vegetable pulp, adding 10mL of 80% ethanol solution, carrying out ultrasonic extraction in a water bath at 40 ℃ for 30min, carrying out centrifugal treatment at 4 ℃ and 10000prm for 10min, taking supernatant, re-extracting the residue once by using 5mL of 80% ethanol solution, combining the supernatant, carrying out constant volume treatment to 25mL by using 80% acetonitrile to obtain soluble sugar stock solution, and introducing the soluble sugar stock solution into a cation chromatographic column to complete the separation of organic acid, polyphenol, flavone, chlorophyll and fructose.

Comparative example 2

Taking 1.0g of fruit and vegetable pulp, adding 10mL of 80% ethanol solution, carrying out ultrasonic extraction in a water bath at 40 ℃ for 30min, carrying out centrifugal treatment at 4 ℃ and 10000prm for 10min, taking supernatant, re-extracting the residue once by using 5mL of 80% ethanol solution, combining the supernatant, carrying out constant volume treatment to 25mL by using 80% acetonitrile to obtain soluble sugar stock solution, and introducing the soluble sugar stock solution into an anion chromatographic column to complete the separation of organic acid, polyphenol, flavone, chlorophyll and fructose.

Comparative example 3

Taking 1.0g of fruit and vegetable pulp, adding 10mL of 80% ethanol solution, carrying out ultrasonic extraction in a water bath at 40 ℃ for 30min, carrying out centrifugal treatment at 4 ℃ and 10000prm for 10min, taking supernatant, re-extracting the residue once by using 5mL of 80% ethanol solution, combining the supernatant, carrying out constant volume treatment to 25mL by using 80% acetonitrile to obtain soluble sugar stock solution, and introducing the soluble sugar stock solution into a sugar special column to complete the separation of organic acid, polyphenol, flavone, chlorophyll and fructose.

The separated liquids obtained in examples 1 to 5 of the present invention were systematically evaluated for their effects by experiments, and the separated liquids obtained in comparative examples 1 to 3 were used as performance controls.

1. The fruit acid concentration in the separated liquid was measured, and the higher the fruit acid concentration, the smaller the loss of the fruit acid component during the separation, and the fruit acid concentrations at the completion of the separation and at the time of standing for 60 minutes were measured, respectively, and the results of the other groups of tests were relative to those of example 1, assuming that the test result of example 1 was 100%, and the results are shown in table 1 below.

TABLE 1 test results of fruit acid concentration in the separation liquid

Therefore, the separation method provided by the invention has the advantages that the concentration loss of the fruit acid is less, the fruit acid component in the separation liquid can be better reserved, the stability of the separation liquid is better, and the measurement liquid with better performance can be provided for subsequent measurement.

2. And (3) measuring the concentration of the organic acid in the separation liquid, wherein the lower the concentration of the organic acid is, the more thorough the removal of the organic acid is in the separation process, and the better the impurity removal effect of the fruit acid is. The organic acid concentrations at the completion of the separation and at the time of standing for 60 minutes were measured, and the results of the other tests were relative proportions to those of example 1, assuming that the test result of example 1 was 0%, and the results are shown in table 1 below.

TABLE 1 test results of organic acid concentration in separation liquid

Therefore, the separation method provided by the invention has a good organic acid removal effect, can better realize impurity removal of the separation liquid, has good acid stability after separation, and can provide a determination liquid with good performance for subsequent determination.

3. And (3) measuring the concentration of the polyphenol in the separation liquid, wherein the lower the concentration of the polyphenol is, the more thorough the removal of the polyphenol is in the separation process, and the better the impurity removal effect of the tartaric acid is. The polyphenol concentration at the completion of the separation and at the time of standing for 60 minutes were measured, and the results of the other groups were calculated as 0% in the test result of example 1 and the relative ratio to example 1, and the results are shown in table 1 below.

TABLE 1 measurement of the concentration of polyphenols in the separation liquid

Therefore, the separation method provided by the invention has a good polyphenol removal effect, can better realize impurity removal of the separation liquid, has good acid stability after separation, and can provide a determination liquid with good performance for subsequent determination.

4. And (3) measuring the concentration of the flavone in the separation liquid, wherein the lower the concentration of the flavone is, the more thorough the flavone is removed in the separation process, and the better the impurity removal effect of the tartaric acid is. The flavone concentration at the completion of the separation and at the time of standing for 60 minutes were measured, and the results of the other groups were expressed in the following table 1, assuming that the test result of example 1 was 0% and the relative ratio to example 1 was measured.

TABLE 1 results of measuring the concentration of flavone in the separation liquid

Therefore, the separation method provided by the invention has a good flavone removal effect, can better realize impurity removal of the separation liquid, has good acid stability of the separation result, and can provide a determination liquid with good performance for subsequent determination.

5. And measuring the concentration of chlorophyll in the separation liquid, wherein the lower the concentration of chlorophyll is, the more thorough the chlorophyll is removed in the separation process, and the better the impurity removal effect of the tartaric acid is. The chlorophyll concentration at the completion of the separation and at the time of standing for 60 minutes were measured, and the results of the other groups were expressed in the following table 1, assuming that the test result of example 1 was 0% and the relative ratio to example 1 was obtained.

TABLE 1 chlorophyll concentration test results in the separation liquid

Therefore, the separation method provided by the invention has the advantages that the chlorophyll removal effect is good, the impurity removal of the separation liquid can be better realized, the acid stability of the separation liquid is good, and the determination liquid with good performance can be provided for the subsequent determination.

The embodiment shows that the technical scheme provided by the invention has the following beneficial effects: the technical scheme provided by the invention has the following beneficial effects: the invention provides a purification treatment method of soluble sugar in fruits and vegetables, which comprises the steps of preparing a sample solution to obtain a soluble sugar stock solution containing impurities, extracting the soluble sugar stock solution, purifying or enriching the soluble sugar stock solution to separate the soluble sugar and the impurities in the soluble sugar stock solution, and obtaining a filtrate to be detected. By adding one or more solid powder adsorbing materials which have an adsorbing effect on organic acids, polyphenols, flavones, chlorophyll and the like and do not adsorb monosaccharides, impurity removal of a fructose determination sample is realized, the purity of a soluble sugar determination sample is ensured, and the subsequent determination accuracy is improved.

It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains. Unless specifically stated otherwise, the relative steps, numerical expressions, and values of the components and steps set forth in these embodiments do not limit the scope of the present invention. In all examples shown and described herein, unless otherwise specified, any particular value should be construed as merely illustrative, and not restrictive, and thus other examples of example embodiments may have different values.

In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.

Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention, and all of the technical solutions are covered in the protective scope of the present invention.

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