CN114681495B

CN114681495B - A method for preparing seaweed extract capable of removing heavy metals with high efficiency, and seaweed extract and preparation prepared from the same

Info

Publication number: CN114681495B
Application number: CN202011593640.XA
Authority: CN
Inventors: 周厚成; 胡昌江; 黄美华; 张开元; 陈蓉; 梅国荣; 黄宇; 孙纪元
Original assignee: Jiangxi New Green Pharmaceutical Technology Development Co ltd; Sichuan New Green Pharmaceutical Technology Development Co ltd
Current assignee: Jiangxi New Green Pharmaceutical Technology Development Co ltd; Sichuan New Green Pharmaceutical Technology Development Co ltd
Priority date: 2020-12-29
Filing date: 2020-12-29
Publication date: 2023-07-14
Anticipated expiration: 2040-12-29
Also published as: CN114681495A

Abstract

The invention discloses a preparation method of a seaweed extract capable of efficiently removing heavy metals, the seaweed extract prepared by the seaweed extract and a preparation, which are prepared by the seaweed extract, firstly adopt a combination mode, are soaked by acetic acid in a medicinal material treatment stage, and are adsorbed by resin in an extraction stage, so that the heavy metals in the seaweed extract are efficiently, simply, conveniently and rapidly removed in the preparation process of the seaweed extract, the safety of the extract and the preparation of the seaweed extract is ensured, the content of active ingredients of the seaweed extract is effectively ensured, and the quality standard of the seaweed extract is met.

Description

A method for preparing seaweed extract capable of removing heavy metals with high efficiency, and seaweed extract and preparation prepared from the same

Technical Field

The invention belongs to the field of traditional Chinese medicine preparations, and particularly relates to a preparation method of a seaweed extract capable of efficiently removing heavy metals, and the seaweed extract and a preparation prepared by the seaweed extract.

Background

The seaweed is Sargassum pallidum of SargassaceaeSargassumpallidum(Turn.) C.Ag. Or Sargassum fusiformeSargassumfusiforme(Harv.) Setch. Dried algae has effects of resolving phlegm, softening and resolving hard mass, inducing diuresis for removing edema, can be used for treating goiter, scrofula,symptoms such as swelling and pain of testis, phlegm-fluid edema, etc. The history of the medicine is long, the dietetic therapy efficacy is recorded as early as in Shennong Ben Cao Jing, and the pharmaceutical value is recorded in Ben Cao gang mu: can be used for treating running pig qi, tinea pedis, edema, indigestion, and goiter. The seaweed contains rich nutrition and various chemical components, has higher health care value and unique biological activity, and has remarkable potential in the aspects of resisting virus, bacteria, oxidization, tumor, senile dementia and the like.

The prior researches show that the seaweed has a large surface area, viscosity and high selectivity of cell membranes, the capacity of adsorbing heavy metals is far higher than that of general marine plants, and the adsorption and concentration capacities of the seaweed are tens times higher than those of terrestrial plants. Heavy metals are difficult to biodegrade, but can be enriched in organisms by thousands of times through food chains, and the heavy metals enter human bodies to cause different degrees of damage to physiological functions and metabolic functions. Therefore, seaweed is used as a bulk medicinal material, and one of the main factors influencing the safe use of seaweed at present is the content of heavy metals.

The removal of heavy metals in traditional Chinese medicine extracts at present mainly comprises centrifugation, precipitation, ultrafiltration, ion exchange, membrane separation and the like, and is the treatment of the traditional Chinese medicine extracts and the preparation thereof, for example: wu Congjun in the research of the method for removing heavy metal ions from traditional Chinese medicine extract (modern food science, 2011, vol.27, no.10, 1268-1275), crude traditional Chinese medicine extract is taken as an experimental sample, and the adsorption of harmful heavy metal cations by using strong acid ion exchange resin shows that 10ml of wet resin can adsorb Pb ²⁺ 58.7mg, or Cu ²⁺ 19.04mg, or Cd ²⁺ 33.68mg, the removing effect is good, and the recovery rate of the active ingredient flavone of the traditional Chinese medicine extract reaches 95.3-97.9% after the ion exchange treatment.

In research of removing seaweed heavy metals, the prior patent document CN101579071a discloses a method for removing arsenic from seaweed extract, which utilizes sulfated polysaccharide and chitosan to prepare a polymer with a net structure and a large surface area and adsorption capacity, and adds the polymer into seaweed extract to adsorb arsenic compounds in aqueous solution, so that original functional components in the seaweed extract are greatly reserved, and the removal rate of the arsenic compounds can reach 95% along with the continuous increase of the usage of the polymer. In addition, the prior patent document CN102356892A also discloses a method for removing heavy metal lead and cadmium from gracilaria algae, which comprises the steps of cleaning the gracilaria algae, removing impurities, putting the gracilaria algae into an organic acid solution with a certain concentration to remove the metal lead and the cadmium, and enabling the gracilaria algae to reach the edible safety standard, wherein the removal rate of the lead is 93.4%, and the removal rate of the cadmium is 85%.

From the above prior art it is known that the following problems also exist in the removal of heavy metals from seaweed extracts and their preparations:

(1) In the conventional method for removing heavy metals from traditional Chinese medicine extract, although Pb ²⁺ 、Cu ²⁺ And Cd ²⁺ The method has the advantages that the effective removal effect is achieved, but the recovery rate of the flavone serving as an effective component is used as a reference basis, the reference standard of the effective component in the seaweed extract and the preparation thereof is not met, and the quality standard of traditional Chinese medicine of the seaweed extract and the preparation thereof cannot be met, so that a special heavy metal removal method for the seaweed extract and the preparation thereof still needs to be established.

(2) Heavy metals are more, and Pb, cd, hg, as, cu and the like are involved in heavy metals with larger enrichment in seaweed, but in the prior patent literature, the removal rate of CN101579071A only for arsenic compounds can reach 95%, the removal rate of CN102356892A only for lead and cadmium reaches 93.4% and 85%, and the comprehensive removal rate of heavy metals does not reach the standard.

Based on the above situation, in order to realize the effective removal of heavy metals in seaweed extract and its preparation, we need to find a specific method for removing heavy metals in seaweed extract and its preparation, so as to effectively ensure the content of effective extraction components, meet the requirements of quality standards, and establish a method with the highest comprehensive removal rate of heavy metals and the highest removal efficiency.

Disclosure of Invention

The invention aims to provide a preparation method of a seaweed extract capable of efficiently removing heavy metals, which adopts a combination mode for the first time, is soaked by acetic acid in a medicinal material treatment stage, and is used for adsorbing an extracting solution by resin in an extraction stage, so that the heavy metals in the seaweed extract can be efficiently, simply, conveniently and rapidly removed in the preparation process of the seaweed extract, the safety of the extract and a preparation thereof can be ensured, the content of active ingredients of the extract can be effectively ensured, and the quality standard of the extract can be met.

The invention is realized by the following technical scheme: a preparation method of seaweed extract capable of efficiently removing heavy metals comprises the following steps:

A. soaking seaweed material in acid solution, washing with water to neutrality, and drying to obtain seaweed decoction pieces;

B. preparing seaweed decoction pieces into seaweed extract;

C. adding resin into seaweed extract, stirring for adsorption, collecting adsorption solution, and drying to obtain seaweed extract.

In the step A, the soaking time is 2-6 hours.

In step a, the acid solution includes, but is not limited to, acetic acid, hydrochloric acid, or citric acid.

The acid solution is acetic acid with the mass concentration of 1-5%, and the acetic acid is suitable for submerging the medicinal materials by 10cm during soaking.

In the step C, the addition amount of the resin is 2-8 times of the quality of the decoction pieces.

In the step C, the stirring rotating speed is 300-450 r/min, and the stirring time is 30-90 min.

In step C, the resins include, but are not limited to, resins WH825, WH912, or LSC-As.

In the step C, cu is less than or equal to 0.7ppm, as is less than or equal to 1.6ppm, cd is less than or equal to 0.1ppm, hg is less than or equal to 0ppm and Pb is less than or equal to 0.2ppm in the seaweed extract.

The invention also provides the seaweed extract prepared by the method and the seaweed preparation prepared by the seaweed extract.

Compared with the prior art, the invention has the following advantages:

(1) The method provided by the invention has the advantages that the seaweed extract is soaked by acetic acid in the medicinal material treatment stage in the preparation process, the extracting solution is adsorbed by resin in the extraction stage, and the heavy metals in the seaweed extract and the seaweed extract preparation can be removed efficiently, simply, conveniently and quickly under the condition of combining the two modes, so that the safety of the seaweed extract and the seaweed extract preparation is ensured, the content of the active ingredients of the seaweed extract is also ensured, and the quality standard requirement of the seaweed extract is met.

(2) In the existing process for preparing the seaweed extract by extracting seaweed medicinal materials, the high-efficiency removal of heavy metals in the seaweed extract and the preparation thereof can be effectively realized by reasonably controlling the consumption of acetic acid and resin and the technological condition parameters thereof, the technical indexes of Cu less than or equal to 0.7ppm, as less than or equal to 1.6ppm, cd less than or equal to 0.1ppm, hg less than or equal to 0.2ppm and Pb less than or equal to 85 percent in the seaweed extract are ensured, the removal rate is more than 85 percent, and the content is far lower than the requirements of Cu less than or equal to 20ppm, cd less than or equal to 4ppm, hg less than or equal to 0.1ppm and Pb less than or equal to 5ppm of the standard range of the heavy metals specified in the seaweed extract and the preparation thereof in Chinese pharmacopoeia, and meanwhile, the effective control of the content of heavy metal arsenic in the extract is increased.

(3) The method is particularly suitable for varieties with the extract heavy metals and the preparation content exceeding the standard, is simple and easy to operate, adds soaking and resin treatment procedures in the existing extraction process flow, can be recycled after regeneration after resin adsorption, and can effectively control the process cost.

Drawings

FIG. 1 is a graph of a comparative thin layer chromatogram of acetic acid at various concentrations.

FIG. 2 is a graph of acetic acid time of action versus thin layer chromatography.

FIG. 3 is a comparative thin layer chromatogram of resin species and fold investigation.

FIG. 4 is a comparative thin layer chromatogram of the combination.

Detailed Description

The objects, technical solutions and advantageous effects of the present invention will be described in further detail below.

It is noted that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed, and unless otherwise indicated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

The invention relates to a method for efficiently removing heavy metals in a traditional Chinese medicine extract and a preparation thereof, which is particularly suitable for varieties with the content of the heavy metals in the extract and the preparation thereof exceeding the standard. Particularly for seaweed, the seaweed has rich nutrition, higher health care value and unique biological activity, but is easy to enrich a large amount of heavy metals. In the Chinese pharmacopoeia, the standard range of heavy metals is Cu less than or equal to 20ppm, cd less than or equal to 4ppm, hg less than or equal to 0.1ppm and Pb less than or equal to 5ppm, so that in order to ensure the safe use of the seaweed extract and the preparation, a proper method for removing the heavy metal content in the extract and the preparation is needed.

The existing researches and patent documents show that the strong acid ion exchange resin can adsorb heavy metals Pb, cu and Cd in the traditional Chinese medicine extract, but the recovery rate of the active ingredient flavone in the traditional Chinese medicine extract is required to be ensured; the gracilaria seaweed is soaked by adopting an organic acid solution, so that lead and cadmium in the gracilaria seaweed can be removed, but heavy metal copper cannot be removed; the polymer prepared from sulfated polysaccharide and chitosan has high adsorption capacity only for heavy metal arsenic in seaweed extract. Therefore, the comprehensive removal rate of heavy metals in the extract does not reach the standard in the prior art, and the method for efficiently removing various heavy metals in the extract and the preparation thereof is provided for meeting the requirements on heavy metal content in Chinese pharmacopoeia and effectively controlling the quality and safety performance of the traditional Chinese medicine preparation.

The following examples are given to illustrate specific embodiments of the present invention, but the scope of the present invention is not limited to the following examples.

Example 1:

cleaning 500g of seaweed medicinal material with water, adding acetic acid with mass fraction of 2% to submerge the medicinal material for 10cm, soaking for 2h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH825 with the decoction piece amount of 4 times, adding into the extractive solution, stirring at 400r/min for 60min, filtering, collecting the adsorption solution, washing with water, mixing the adsorption solutions, and drying to obtain seaweed extract.

Example 2:

taking 500g of seaweed medicinal material, washing with water, adding acetic acid with the mass fraction of 1%, preferably immersing for 2-6 hours when the medicinal material is submerged for 10cm, washing with water to be neutral, cutting into segments, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH912 with the decoction piece amount of 8 times, adding into the standby seaweed extract, stirring at 450r/min for 90min, filtering, collecting the adsorption liquid, washing with water, mixing the adsorption liquid, and drying to obtain seaweed extract.

Example 3:

washing 500g of seaweed medicinal material with water, adding citric acid with mass fraction of 5% to submerge the medicinal material for 10cm, soaking for 6h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin LSC-As with the decoction piece amount of 6 times, adding the standby seaweed extract, stirring at 300r/min for 60min, filtering, collecting the adsorption liquid, washing the resin with water, mixing the adsorption liquid, and drying to obtain seaweed extract.

Example 4:

cleaning 500g of seaweed medicinal material with water, adding acetic acid with mass fraction of 4% to submerge the medicinal material for 10cm, soaking for 3h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH825 with the decoction piece amount of 5 times, adding into the extractive solution, stirring at 350r/min for 80min, filtering, collecting the adsorption solution, washing with water, mixing the adsorption solutions, and drying to obtain seaweed extract.

Example 5:

cleaning 500g of seaweed medicinal material with water, adding acetic acid with mass fraction of 2% to submerge the medicinal material for 10cm, soaking for 4h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH825 with the decoction piece amount of 4 times, adding into the extractive solution, stirring at 450r/min for 55min, filtering, collecting the adsorption solution, washing with water, mixing the adsorption solutions, and drying to obtain seaweed extract.

Example 6:

washing 500g of seaweed medicinal material with water, adding hydrochloric acid with the mass fraction of 3.5%, preferably 10cm, soaking for 6h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH912 with 3 times of decoction pieces, adding into the extractive solution, stirring at 400r/min for 70min, filtering, collecting the adsorption solution, washing with water, mixing the adsorption solutions, and drying to obtain seaweed extract.

Example 7:

cleaning 500g of seaweed medicinal material with water, adding acetic acid with mass fraction of 3%, preferably 10cm, soaking for 5 hr, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH825 with the decoction piece amount of 6 times, adding into the extractive solution, stirring at 380r/min for 45min, filtering, collecting the adsorption solution, washing with water, mixing the adsorption solutions, and drying to obtain seaweed extract.

Example 8:

cleaning 500g of seaweed medicinal material with water, adding acetic acid with mass fraction of 2% to submerge the medicinal material for 10cm, soaking for 5h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin LSC-As with the decoction piece amount of 4 times, adding the prepared seaweed extract, stirring at 500r/min for 60min, filtering, collecting the adsorption liquid, washing with water, mixing the adsorption liquid, and drying to obtain seaweed extract.

The seaweed extracts obtained in examples 1 to 8 were examined, and the decoction pieces after washing were used as a blank group. The heavy metal content is detected according to the second method of the fourth general rule 2321 of China pharmacopoeia 2015, and the detection result is shown in the following table 1.

TABLE 1 seaweed extract heavy metal content detection Table

As shown in Table 1, the seaweed extracts obtained in examples 1 to 8 had a heavy metal Cu content of 0.8ppm or less and a removal rate of 91.0%; the As content is less than or equal to 1.6ppm, and the removal rate is 99.6 percent; the Cd content is less than or equal to 0.1ppm, and the removal rate is 85.7 percent; hg reaches the undetected limit, and the removal rate is 100.0 percent; the Pb content is less than or equal to 0.2ppm, and the removal rate is 88.2%, and the result proves that the method can efficiently, simply and quickly remove the heavy metal content in the seaweed extract.

Example 9:

cleaning 20kg of seaweed medicinal material with water, adding acetic acid with mass fraction of 2% to submerge the medicinal material for 10cm, soaking for 6h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH825 with the decoction piece amount of 4 times, adding into the extractive solution, stirring at 400r/min for 90min, filtering, collecting the adsorption solution, washing with water, mixing the adsorption solutions, concentrating to a certain density, and drying to obtain seaweed extract. Directly granulating the seaweed extract by dry method to obtain seaweed formula granules. The resin containing heavy metals is reused after regeneration.

Example 10:

cleaning 20kg of seaweed medicinal material with water, adding hydrochloric acid with mass fraction of 5% to submerge the medicinal material for 10cm, soaking for 2h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH825 with the decoction piece amount of 6 times, adding into the extractive solution, stirring at 450r/min for 60min, filtering, collecting the adsorption solution, washing with water, mixing the adsorption solutions, concentrating to a certain density, and drying to obtain seaweed extract. Directly granulating the seaweed extract by dry method to obtain seaweed formula granules. The resin containing heavy metals is reused after regeneration.

Example 11:

cleaning 20kg of seaweed medicinal material with water, adding acetic acid with mass fraction of 4% to submerge the medicinal material for 10cm, soaking for 5h, washing with water to neutrality, cutting, drying to obtain seaweed decoction pieces, and weighing. Adding water with 20 times of decoction pieces, decocting for 2 times, 40min each time, filtering with 200 mesh sieve, mixing filtrates to obtain seaweed extract, and standing at room temperature. Taking activated resin WH912 with the decoction piece amount of 8 times, adding into the standby seaweed extract, stirring at 420r/min for 90min, filtering, collecting the adsorption liquid, washing with water, mixing the adsorption liquid, concentrating to a certain density, and drying to obtain seaweed extract. Directly granulating the seaweed extract by dry method to obtain seaweed formula granules. The resin containing heavy metals is reused after regeneration.

The seaweed formulation granules obtained in examples 9 to 11 were examined, and the decoction pieces after washing were used as a blank group. The heavy metal content is detected according to the second method of the fourth general rule 2321 of China pharmacopoeia 2015, and the detection result is shown in the following table 2.

Table 2 table for detecting heavy metal content of seaweed formula particles

As shown in the above Table 2, the seaweed formulation particles obtained in examples 9 to 11 had a heavy metal Cu removal rate of 91.0%; the As removal rate is 99.5%; the Cd removal rate is 85.7%; hg reaches the undetected limit, and Pb removal rate is 88.2%, and the result proves that the combined method can efficiently, simply and quickly remove heavy metal content in the seaweed extract preparation, and ensures and improves the safety of the preparation.

Example 12: acetic acid investigation

1. Acetic acid concentration

Weighing a proper amount of medicinal materials, washing with water, respectively adding acetic acid with mass fractions of 0.5%, 1%, 2%, 5% and 10% to soak the medicinal materials for 6 hours, washing with water to neutrality, cutting into segments, drying to obtain decoction pieces, preparing water extract, and drying to obtain the extract. Setting a blank group: weighing appropriate amount of medicinal materials, washing with water, cutting, drying, preparing water extract, concentrating, and drying to obtain blank extract. The heavy metal detection results are shown in the following table 3, and the thin layer identification is shown in fig. 1.

TABLE 3 examination of acetic acid concentration

From the data in the table 3, acetic acid with different concentrations is used for treating medicinal materials, and the acetic acid with the mass fraction of 1-5% can play a role in removing heavy metals in the extract, but the removal rate is not more than 71%; when the acetic acid consumption is increased to more than 5%, the heavy metal removal effect is not obviously increased, which indicates that a higher removal effect cannot be achieved by using acetic acid alone.

The results shown in fig. 1 indicate that after the medicinal materials are treated by acetic acid with different concentrations, fluorescent spots with the same color appear on the positions of the chromatogram of the test sample corresponding to the control medicinal materials and the blank group. That is, the acetic acid treatment of the medicinal materials with different concentrations does not cause the increase or decrease of chemical components. In fig. 1, 1: seaweed control; 2: blank; 3:0.5% acetic acid; 4:1% acetic acid; 5:2% acetic acid; 6:5% acetic acid; 7:10% acetic acid.

2. Acetic acid action time

Weighing a proper amount of medicinal materials, washing with water, adding acetic acid with mass fraction of 2% to soak for 0.5h, 1h, 2h, 6h and 10h respectively, washing with water to neutrality, cutting into segments, and drying to obtain decoction pieces. In addition, the decoction pieces are prepared into water extract, and the water extract is dried to obtain the extract. The heavy metal detection results are shown in the following table 4, and the thin layer identification is shown in fig. 2.

TABLE 4 examination of acetic acid action time

As shown in the data of the table 4, the extract has a certain effect of removing heavy metals after the medicinal materials are treated by 2% acetic acid for different time, and the removal rate is only 59.9% at most within 1-6 hours; after 6 hours, the soaking time is prolonged, and the heavy metal removal effect is not obviously improved, which indicates that the effect of obviously removing the heavy metal in the extract can not be achieved by the mode of prolonging the soaking time.

The results shown in fig. 2 show that the acetic acid soaks the medicinal materials for different times, and fluorescent spots with the same color appear on the positions of the chromatogram of the test sample corresponding to the control medicinal materials and the blank group. In fig. 2, 1: seaweed control; 2: blank; 3:30min;4:1h;5:2h;6:6h;7: and 10h.

Example 13: investigation of resin types and multiples

Removing heavy metals from the seaweed extract which is not subjected to any treatment by a resin adsorption principle, respectively adding activated resin LSC-As 1 times, 2 times, 4 times and 8 times of decoction pieces, activated resin WH825 2 times, 4 times and 10 times of decoction pieces, stirring and adsorbing the extract by the activated resin WH912 2 times, 4 times and 10 times of decoction pieces, respectively collecting the adsorption liquid, and drying to obtain the extract. The resin containing heavy metals can be regenerated and reused. The heavy metal detection results are shown in the following table 5, and the thin-layer chromatogram is shown in fig. 3.

TABLE 5 investigation of resin types and multiples

As shown in the data of Table 5, the effect of the resin on the various decoction pieces was varied to a certain extent, the removal rate was only 59.2% at maximum, although the effect of the resin LSC-As was 2 to 8 times the decoction pieces, the effect of the resin WH825 was 4 to 10 times the decoction pieces, and the effect of the resin WH912 was 4 to 10 times the decoction pieces.

The results shown in figure 3 show that the three resin treatment liquid medicines show fluorescent spots with the same color on the positions of the chromatogram of the test sample corresponding to the control medicinal materials and the blank group; under different usage times, each resin shows fluorescent spots with the same color on the positions of the chromatogram of the test sample corresponding to the control medicinal material and the blank group. Namely, the operation of resin treatment of the liquid medicine has no influence on the chemical components of the medicinal materials. In fig. 3, 1: seaweed control; 2: blank; 3: LSC-As 1-fold; 4: LSC-As 2 times; 5: LSC-As 4 times; 6: LSC-As 8-fold; 7: WH825 times; 8: WH825 4 times; 9: WH825 10 times; 10: WH912 times; 11: WH912 times; 12: WH912 times.

In summary, the above experiments show that the removal of heavy metals is not achieved by the acetic acid treatment or the resin treatment alone, so that a combined method is proposed to treat the medicinal materials in the first stage by acetic acid and to treat the extracts in the second stage by resin treatment, and the investigation of the removal of heavy metals in the seaweed extract and the preparation thereof is carried out.

Example 14: combined method for removing heavy metals from extract

Combination method 1: washing the medicinal materials with water, adding acetic acid with mass fraction of 1% to soak the medicinal materials for 6 hours, washing with water to neutrality, cutting into segments, drying to obtain decoction pieces, preparing an extracting solution, adding activated resin LSC-As with the decoction pieces of 8 times, stirring to adsorb the extracting solution for 60 minutes, collecting the adsorbing solution, and drying to obtain extract 1;

combination method 2: washing the medicinal materials with water, adding acetic acid with mass fraction of 2% to soak the medicinal materials for 3 hours, washing with water to neutrality, cutting into segments, drying to obtain decoction pieces, preparing an extracting solution, adding activated resin LSC-As with the decoction piece amount of 4 times, stirring to adsorb the extracting solution for 60 minutes, collecting the adsorbing solution, and drying to obtain extract 2;

combination method 3: washing the medicinal materials with water, adding acetic acid with mass fraction of 2% to soak the medicinal materials for 6h, washing with water to neutrality, cutting, drying to obtain decoction pieces, preparing an extract, adding activated resin LSC-As with 2 times of the decoction pieces, stirring to adsorb the extract for 60min, collecting the adsorption liquid, and drying to obtain extract 3;

combination method 4: washing the medicinal materials with water, adding acetic acid with mass fraction of 2% to soak the medicinal materials for 6h, washing with water to neutrality, cutting, drying to obtain decoction pieces, preparing an extract, adding activated resin WH825 with the decoction pieces amount of 4 times, stirring to adsorb the extract for 60min, collecting the adsorption liquid, and drying to obtain extract 4;

the combination method 5: washing the medicinal materials with water, adding acetic acid with mass fraction of 5% to soak the medicinal materials for 6h, washing with water to neutrality, cutting, drying to obtain decoction pieces, preparing an extract, adding activated resin WH912 with the decoction pieces 10 times of the amount of the decoction pieces, stirring to adsorb the extract for 60min, collecting the adsorbed solution, and drying to obtain extract 5;

the results of the detection of heavy metals, binding and treatment with acid alone or resin alone are shown in Table 6 below and the thin layer chromatogram is shown in FIG. 4.

TABLE 6 results of removal of heavy metals from extracts in combination

From the data in the table 6, the heavy metals in the extract can be efficiently removed by different combination modes, and the Cu removal rate reaches 89.7%; the As removal rate reaches 99.6%; the removal rate of Cd reaches 85.7%, hg reaches undetected limit, pb removal rate reaches 94.1%, and heavy metal removal rate reaches 86% or more.

The results shown in fig. 4 show that under the five combination methods in the experiment, fluorescent spots with the same color appear on the positions of the chromatogram of the test sample corresponding to the control medicinal material and the blank group. In fig. 4, 1: seaweed control; 2: blank; 3: combining method 1;4: combining method 2;5: combining method 3;6: combining method 4;7: combining method 5.

Based on the examination of the above examples 12 and 13, the results show that the heavy metal content of the prepared extract is obviously reduced to a safe level by adding 1-5% of acetic acid to soak the medicinal materials and using 2-10 times of resin to stir and adsorb the extract.

The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present invention fall within the scope of the present invention.

Claims

1. A preparation method of seaweed extract capable of efficiently removing heavy metals is characterized by comprising the following steps: the method comprises the following steps:

A. soaking seaweed medicinal materials in acetic acid with the mass concentration of 1-5%, washing with water to be neutral, and drying to obtain seaweed decoction pieces;

B. preparing seaweed decoction pieces into seaweed extract;

C. adding resin 2-8 times of decoction piece mass into seaweed extract, stirring and adsorbing, collecting adsorption liquid, drying to obtain seaweed extract,

the resin is resin WH825, resin WH912 or resin LSC-As.

2. The method for preparing seaweed extract capable of efficiently removing heavy metals according to claim 1, which is characterized in that: in the step A, the soaking time is 2-6 hours.

3. The method for preparing seaweed extract capable of efficiently removing heavy metals according to claim 1, which is characterized in that: in the step C, the stirring rotating speed is 300-450 r/min, and the stirring time is 30-90 min.

4. The method for preparing seaweed extract capable of efficiently removing heavy metals according to claim 1, which is characterized in that: in the step C, cu is less than or equal to 0.7ppm, as is less than or equal to 1.6ppm, cd is less than or equal to 0.1ppm, hg is less than or equal to 0ppm and Pb is less than or equal to 0.2ppm in the seaweed extract.

5. A seaweed extract obtained by the method of claim 1.

6. A seaweed preparation prepared by using the seaweed extract of claim 5.