Method for removing metal ions in opuntia ficus-indica pomace extract

Abstract

The invention discloses a method for removing metal ions in a prickly pear pomace extract, which comprises the following steps: selecting prickly pear pomace, and carrying out freeze-drying treatment to obtain a freeze-dried prickly pear pomace raw material; adding distilled water for twice extraction, and combining the two extracting solutions to obtain a cactus pomace water extract; selecting resin for pretreatment; carrying out ultrasonic stirring on the cactus pomace water extract, and loading the water extract into the pretreated resin column, so that metal ions in the water extract are fully combined with the resin; and performing elution treatment to obtain the cactus pomace extract with low metal ion content. The result shows that calcium ions in the raw material puree are 6.77 * 10 mg / kg, iron ions in the raw material puree are 241 mg / kg, the calcium ions and the iron ions are not detected after being treated by 0017, D001 and T-42H resin, and the calcium ions are only 54.3 mg / kg after being treated by D401 resin. The process is clear in parameters, simple to operate, capable of efficiently removing metal ions and suitable for purification treatment of the prickly pear pomace extract.

Description

Technical Field

[0001] This invention relates to the field of natural plant extract purification technology, and in particular to a method for removing metal ions from cactus pomace extract. Background Technology

[0002] The processing of cactus fruit generates a large amount of pomace, which contains abundant active ingredients but also naturally carries metal ions such as calcium and iron ions. If these metal ions remain in the subsequently prepared extracts, they may not only affect the stability of the extracts (such as causing oxidation and precipitation of active ingredients) but may also fail to meet the quality standards of downstream applications, thus limiting the high-value utilization of cactus pomace resources.

[0003] Current methods for removing metal ions from plant extracts have certain limitations:

[0004] Some methods require the introduction of chemical reagents, which can easily cause secondary pollution;

[0005] Some process parameters are unclear, and the metal ion removal effect is unstable.

[0006] Therefore, in order to solve the problem of metal ion residue in cactus pomace extract in the prior art, an adsorption-water elution method with a specific resin as the core is provided to effectively remove calcium and iron ions, obtain cactus pomace extract with low metal ion content, and promote the rational utilization of cactus pomace resources. This is a technical problem that urgently needs to be solved by those skilled in the art. Summary of the Invention

[0007] In view of this, the present invention provides a method for removing metal ions from cactus pomace extract.

[0008] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0009] A method for removing metal ions from cactus fruit pomace extract includes the following steps:

[0010] Step 1: Raw material pretreatment

[0011] Select cactus pomace and freeze-dry it to obtain freeze-dried cactus pomace raw material for later use;

[0012] Step 2: Extract preparation

[0013] Weigh the freeze-dried cactus pomace raw material, add distilled water for the first reflux extraction, and start the reflux device; after the extraction is completed, filter and collect the first extract; add distilled water to the filtered residue for the second reflux extraction, and start the reflux device again; filter and collect the second extract, and combine the two extracts; place the combined extract in a vacuum concentration device and concentrate it to the preset volume to obtain the cactus pomace water extract;

[0014] Step 3: Resin Pretreatment

[0015] Select the resin and strictly follow the product instructions for the corresponding resin to complete the pretreatment to ensure that the resin has stable adsorption activity for later use.

[0016] Step 4: Resin Adsorption

[0017] The cactus fruit residue water extract prepared in step 2 is transferred to a container and subjected to ultrasonic stirring to ensure that the components in the extract are fully dissolved and evenly dispersed. The evenly dissolved water extract is then slowly loaded into a pre-treated resin column. The adsorption time is controlled to ensure that the metal ions in the water extract are fully combined with the resin.

[0018] Step 5: Water elution and concentration

[0019] After adsorption is complete, distilled water is introduced into the resin column for elution. All eluent is collected and transferred to a vacuum concentration device to concentrate to a preset concentration, thus obtaining cactus pomace extract with low metal ion content.

[0020] Preferably, in step 1, the freeze-drying conditions are as follows:

[0021] The temperature during the pre-freezing stage is -40℃ to -55℃, which is 10-20℃ below the eutectic point;

[0022] The temperature for sublimation drying is -20℃ to -10℃, with slow heating until it approaches the eutectic point but does not melt.

[0023] The drying temperature is 20℃~40℃ to remove residual bound water;

[0024] The freeze-drying process takes 24 to 48 hours.

[0025] Preferably, in step 2, the first reflux extraction conditions are as follows: distilled water is added at a ratio of 12 times the mass of the raw material, and reflux extraction is performed for 1 hour.

[0026] Preferably, in step 2, the conditions for refluxing and extracting are as follows: add 10 times the mass of distilled water to the filter residue and reflux for 1 hour.

[0027] Preferably, in step 2, the reduced pressure concentration conditions are: temperature 60-70℃, vacuum degree -0.08-0.1MPa.

[0028] Preferably, in step 3, the resin is any one of 001*7 resin, D401 resin, D001 resin or T-42H resin.

[0029] Preferably, in step 3, the pretreatment includes acid washing, alkali washing, and rinsing with distilled water until neutral.

[0030] Preferably, in step 4, the sample is slowly loaded into the pretreated resin column at a flow rate of 1 column volume / hour; the adsorption time is controlled to be 2 hours.

[0031] Preferably, in step 5, the elution conditions are: the elution flow rate of distilled water is controlled at 1.5 BV / h, and the elution volume is 3 BV.

[0032] The present invention achieves the following technical effects compared to the prior art:

[0033] (1) High metal ion removal efficiency: Compared with raw fruit puree (calcium ions 6.77×10 4 After treatment with this invention, the water extract showed an initial reduction in metal ions (calcium ions 310 mg / kg, iron ions 4.87 mg / kg). Further resin adsorption followed by water elution resulted in "undetectable" calcium and iron ions with 001*7, D001, and T-42H resins, while D401 resin reduced calcium ions to 54.3 mg / kg, demonstrating a significant removal effect.

[0034] (2) Flexible resin selection: This invention provides four types of resins that are effective in removing metal ions (001*7, D401, D001, T-42H). The appropriate resin can be selected according to the cost budget and processing volume requirements in actual production, which makes it highly applicable.

[0035] (3) No risk of secondary pollution: The present invention uses distilled water as the extraction and elution solvent throughout the process, without the need to introduce chemical reagents, thus avoiding contamination of the extract, ensuring the purity and safety of the extract, and meeting the requirements of downstream applications;

[0036] (4) Clear and controllable process parameters: This invention strictly limits the key parameters such as the amount of extraction solvent (12 times, 10 times), extraction time (1 hour / time), adsorption flow rate (1 BV / h), adsorption time (2 hours), elution flow rate (1.5 BV / h), and elution volume (3 BV) to ensure that the metal ion removal effect is stable and has good repeatability in different batches of production;

[0037] (5) Simple operation and easy to implement: The method steps of this invention only involve water extraction, resin adsorption, water washing and concentration, which are all routine operations in the production of natural extracts. No special equipment is required, which makes it easy for enterprises to quickly put into production and application. Attached Figure Description

[0038] Figure 1 This is a flowchart of the present invention. Detailed Implementation

[0039] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0040] This invention discloses a method for removing metal ions from cactus fruit pomace extract, comprising the following steps:

[0041] Step 1: Raw material pretreatment

[0042] Select cactus pomace and freeze-dry it to obtain freeze-dried cactus pomace raw material for later use;

[0043] Step 2: Extract preparation

[0044] Weigh the freeze-dried cactus pomace raw material, add distilled water for the first reflux extraction, and start the reflux device; after the extraction is completed, filter and collect the first extract; add distilled water to the filtered residue for the second reflux extraction, and start the reflux device again; filter and collect the second extract, and combine the two extracts; place the combined extract in a vacuum concentration device and concentrate it to the preset volume to obtain the cactus pomace water extract;

[0045] Step 3: Resin Pretreatment

[0046] Select the resin and strictly follow the product instructions for the corresponding resin to complete the pretreatment to ensure that the resin has stable adsorption activity for later use.

[0047] Step 4: Resin Adsorption

[0048] The cactus fruit residue water extract prepared in step 2 is transferred to a container and subjected to ultrasonic stirring to ensure that the components in the extract are fully dissolved and evenly dispersed. The evenly dissolved water extract is then slowly loaded into a pre-treated resin column. The adsorption time is controlled to ensure that the metal ions in the water extract are fully combined with the resin.

[0049] Step 5: Water elution and concentration

[0050] After adsorption is complete, distilled water is introduced into the resin column for elution. All eluent is collected and transferred to a vacuum concentration device to concentrate to a preset concentration, thus obtaining cactus pomace extract with low metal ion content.

[0051] In step 1, the freeze-drying conditions are as follows:

[0052] The temperature during the pre-freezing stage is -40℃ to -55℃, which is 10-20℃ below the eutectic point;

[0053] The temperature for sublimation drying is -20℃ to -10℃, with slow heating until it approaches the eutectic point but does not melt.

[0054] The drying temperature is 20℃~40℃ to remove residual bound water;

[0055] The freeze-drying process takes 24 to 48 hours.

[0056] In step 2, the conditions for the first reflux extraction are as follows: add distilled water at a ratio of 12 times the mass of the raw material and reflux for 1 hour.

[0057] In step 2, the conditions for refluxing and extraction are as follows: add 10 times the mass of distilled water to the filter residue and reflux for 1 hour.

[0058] In step 2, the reduced pressure concentration conditions are: temperature 60-70℃, vacuum degree -0.08-0.1MPa.

[0059] In step 3, the resin is any one of 001*7 resin, D401 resin, D001 resin or T-42H resin.

[0060] In step 3, the pretreatment includes acid washing, alkali washing, and rinsing with distilled water until neutral.

[0061] In step 4, the sample is slowly loaded into the pretreated resin column at a flow rate of 1 column volume / hour; the adsorption time is controlled to be 2 hours.

[0062] In step 5, the elution conditions are as follows: the elution flow rate of distilled water is controlled at 1.5 BV / h, and the elution volume is 3 BV.

[0063] Example 1:

[0064] 1. Experimental Materials

[0065] Raw material: Freeze-dried cactus pomace (corresponding to a calcium ion content of 6.77 × 10⁻⁶ in the pomace) 4 mg / kg, iron ion content 241 mg / kg);

[0066] Reagent: Distilled water (used for extraction and elution);

[0067] Instruments and equipment: reflux extraction device, vacuum concentrator, ultrasonic stirrer, resin column (specification compatible with the selected resin), atomic absorption spectrophotometer (for the detection of calcium ion and iron ion content);

[0068] Resins: 001*7 resin, D401 resin, D001 resin, T-42H resin (all pretreated according to their respective product instructions).

[0069] 2. Experimental Procedure

[0070] Preparation of water extract of cactus pomace: Weigh 100g of freeze-dried cactus pomace raw material, add 1200mL of distilled water (12 times the amount of solvent), start the reflux extraction device, and extract for 1 hour; filter and collect the first extract; add 1000mL of distilled water (10 times the amount of solvent) to the filter residue, and reflux extract again for 1 hour; filter and collect the second extract; combine the two extracts, concentrate under reduced pressure to 100mL, and obtain the water extract of cactus pomace; the calcium ion content in the water extract is 310mg / kg and the iron ion content is 4.87mg / kg.

[0071] Preparation of 60% alcohol extract (control experiment): Take the combined extract above, add ethanol to adjust the alcohol content of the system to 60%, and obtain 60% alcohol extract; the calcium ion content in the alcohol extract is 144 mg / kg, and iron ions are not detected, verifying that alcohol extraction can help reduce the content of metal ions.

[0072] Resin adsorption-water elution treatment (parallel experiments):

[0073] 001*7 Resin Group: Pretreated 001*7 resin was packed into a resin column (column volume 100mL); 100mL of water extract was dissolved by sonication and loaded at a flow rate of 1BV / h (100mL / h) for 2 hours; 300mL of distilled water (3BV) was added at a flow rate of 1.5BV / h (150mL / h) for elution, and the eluent was collected; the eluent was concentrated under reduced pressure to 50mL, and calcium ions and iron ions were not detected.

[0074] D401 Resin Group: Except for replacing the resin with pretreated D401 resin, all other operations (sample loading flow rate, adsorption time, elution flow rate, elution volume, concentration conditions) were completely consistent with the 001*7 resin group; the final concentrate was found to contain 54.3 mg / kg of calcium ions and no iron ions were detected.

[0075] D001 Resin Group: Except for replacing the resin with pretreated D001 resin, the other operations are completely the same as those for 001*7 resin group; no calcium ions and no iron ions were detected in the final concentrate.

[0076] T-42H resin group: Except for replacing the resin with pretreated T-42H resin, the other operations are completely the same as those of the 001*7 resin group; the final concentrate was tested and found to contain neither calcium nor iron ions.

[0077] 3. Test Results and Analysis

[0078] The test results are shown in Table 1.

[0079] Table 1:

[0080] As shown in Table 1, water extraction and alcohol extraction can initially reduce the metal ion content in cactus pomace; while the resin adsorption-water washing treatment in this process can further and efficiently remove metal ions. Among them, 001*7, D001, and T-42H resins have the best removal effect on calcium ions and iron ions, and can completely remove both, meeting the requirements for the preparation of low metal ion extracts.

[0081] The above description is merely a preferred embodiment of the present invention and does not constitute any limitation on the technical scope of the present invention. Therefore, any minor modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention shall still fall within the scope of the technical solution of the present invention.

Claims

1. A method for removing metal ions from cactus fruit pomace extract, characterized in that, Includes the following steps: Step 1: Raw material pretreatment Select cactus pomace and freeze-dry it to obtain freeze-dried cactus pomace raw material for later use; Step 2: Extract preparation Weigh the freeze-dried cactus pomace, add distilled water for the first reflux extraction, and start the reflux device; after the extraction is completed, filter and collect the first extract; add distilled water to the filtered residue for the second reflux extraction, and start the reflux device again. The second extract was collected by filtration, and the two extracts were combined. The combined extract was placed in a vacuum concentration device and concentrated to a preset volume to obtain the cactus fruit residue water extract. Step 3: Resin Pretreatment Select the resin and strictly follow the product instructions for the corresponding resin to complete the pretreatment to ensure that the resin has stable adsorption activity for later use. Step 4: Resin Adsorption The cactus fruit residue water extract prepared in step 2 is transferred to a container and subjected to ultrasonic stirring to ensure that the components in the extract are fully dissolved and evenly dispersed. The evenly dissolved water extract is then slowly loaded into a pre-treated resin column. The adsorption time is controlled to ensure that the metal ions in the water extract are fully combined with the resin. Step 5: Water elution and concentration After adsorption is complete, distilled water is introduced into the resin column for elution. All eluent is collected and transferred to a vacuum concentration device to concentrate to a preset concentration, thus obtaining cactus pomace extract with low metal ion content.

2. The method for removing metal ions from cactus fruit pomace extract according to claim 1, characterized in that, In step 1, the freeze-drying conditions are as follows: The temperature during the pre-freezing stage is -40℃ to -55℃, which is 10-20℃ below the eutectic point; The temperature for sublimation drying is -20℃ to -10℃, with slow heating until it approaches the eutectic point but does not melt. The drying temperature is 20℃~40℃ to remove residual bound water; The freeze-drying process takes 24 to 48 hours.

3. The method for removing metal ions from cactus fruit pomace extract according to claim 1, characterized in that, In step 2, the conditions for the first reflux extraction are as follows: add distilled water at a ratio of 12 times the mass of the raw material, and reflux for 1 hour.

4. The method for removing metal ions from cactus fruit pomace extract according to claim 1, characterized in that, In step 2, the conditions for refluxing and extraction are as follows: add 10 times the mass of distilled water to the filter residue and reflux for 1 hour.

5. The method for removing metal ions from cactus fruit pomace extract according to claim 1, characterized in that, In step 2, the vacuum concentration conditions are: temperature 60-70℃, vacuum degree -0.08--0.1MPa.

6. The method for removing metal ions from cactus fruit pomace extract according to claim 1, characterized in that, In step 3, the resin is any one of 001*7 resin, D401 resin, D001 resin or T-42H resin.

7. The method for removing metal ions from cactus fruit pomace extract according to claim 1, characterized in that, In step 3, the pretreatment includes acid washing, alkali washing, and rinsing with distilled water until neutral.

8. The method for removing metal ions from cactus fruit pomace extract according to claim 1, characterized in that, In step 4, the sample is slowly loaded into the pretreated resin column at a flow rate of 1 column volume / hour; the adsorption time is controlled to be 2 hours.

9. The method for removing metal ions from cactus fruit pomace extract according to claim 1, characterized in that, In step 5, the elution conditions are as follows: the elution flow rate of distilled water is controlled at 1.5 BV / h, and the elution volume is 3 BV.

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