Method for extracting doubt source class based on ultrasonic-filtering

Abstract

The invention provides a method for extracting suspicious sources based on ultrasound-filtration, and relates to the technical field of suspicious source extraction.The method comprises the steps that firstly, hydrogen peroxide is used for dissolving a sample, then filtration is conducted under the ultrasonic condition, and finally diluted hydrochloric acid is added, so that efficient extraction of suspicious sources can be achieved; the ultrasonic effect can be utilized to promote a sample to be in full contact with hydrogen peroxide, so that the sample is fully dispersed, and the sample is filtered under the ultrasonic effect, so that the filtering efficiency is effectively improved, ineffective components (clay particles, silt and the like) are ensured to be fully removed, the enrichment of the effective components is realized to a certain extent, and the time required by the extraction process is shortened; the use amount of hydrochloric acid in the subsequent extraction process is greatly reduced, the use of heavy liquid in the traditional extraction mode is avoided, and the cost required by the extraction process is reduced. Through the mode, the suspicious source extraction method which is high in extraction rate, simple to operate, simple in process and green is provided.

Description

Technical Field

[0001] The invention relates to the technical field of suspected source extraction, and in particular to a method for extracting suspected source based on ultrasound-filtration. Background Art

[0002] The apocrysts are a group of organic-walled microfossils of unknown or uncertain biological affinities, including organic-walled cysts of marine variegated algae, green algae and unicellular protozoa, as well as some fungal spores and other non-marine morphological types. The vast majority of apocrysts are marine planktonic protists, generally preserved in marine carbonate rocks and fine clastic rocks, and usually formed in deeper water sedimentary environments. The apocrysts have diverse shapes, including round, oval, disc-shaped, elongated or polygonal hollow shells or centrosomes, and may also have peripheral decorations such as protrusions, ridges, particles, wings, membranes, etc. on the shell surface. The size of the apocrysts varies greatly, with diameters ranging from 10μm to 1mm, but the vast majority of species are between 15-90μm in size.

[0003] The apocrysts are very useful in determining the age of geological strata and comparing biostratigraphy, especially in Proterozoic and Paleozoic strata, where they are sometimes the only fossils that can be found. Therefore, the apocrysts are widely used in the scientific research of biostratigraphy, paleogeography and paleoenvironment.

[0004] Rock or sediment samples (carbonate rocks, clastic rocks, coarse sand, fine sand, silt, mud, soil, etc.) containing apocrysts obtained in the field must first be subjected to laboratory extraction to remove impurities such as organic matter, clay, and quartz sand in order to obtain apocrysts with high purity and few impurities. Therefore, obtaining a large number of laboratory treatment methods for intact and pure apocryst fossils is an important step in scientific research. Existing apocryst sample pretreatment methods include processes such as removing organic matter, removing carbonates, removing calcium, heavy liquid flotation, and centrifugal purification. However, the above-mentioned treatment methods mainly use hydrochloric acid, hydrofluoric acid, and heavy liquid as the main reagents. For marine sediments with high carbonate and silica content, this method still contains a certain amount of silica and quartz sand in the treated samples, and the treatment effect is not good.

[0005] In view of this, it is necessary to design an improved method for extracting suspected source classes based on ultrasound-filtration to solve the above problems. Summary of the invention

[0006] The object of the present invention is to provide a method for extracting suspected source classes based on ultrasound-filtration.

[0007] To achieve the above-mentioned object of the invention, the present invention provides a method for extracting suspected source classes based on ultrasound-filtration, comprising the following steps:

[0008] Drying and grinding the sample containing the quercetin to obtain a quercetin sample of silt particle size;

[0009] The sample is added into hydrogen peroxide to dissolve and fully disperse the particles; under ultrasonic conditions, the sample solution is filtered using mesh sieves with a pore size of 100 μm and a pore size of 10 μm in turn to retain effective samples within the particle size range of 10-100 μm;

[0010] The solid material remaining on the 10 μm sieve after filtration was added to dilute hydrochloric acid, and fully reacted for 24 hours under stirring conditions, and then centrifuged, washed, and dried to obtain a solid source of the substance.

[0011] Preferably, the mass percentage of hydrogen peroxide is 12%.

[0012] Preferably, the amount of hydrogen peroxide added is 50 mL.

[0013] Preferably, the mass percentage of dilute hydrochloric acid is 20%.

[0014] Preferably, the ratio of the mass of the solid matter to the volume of the dilute hydrochloric acid is 1:3.

[0015] Preferably, the centrifugal conditions are: rotation speed 4000 rpm, time 3 min.

[0016] Preferably, the samples containing apophysis are produced from Proterozoic, Paleozoic, or Mesozoic strata.

[0017] Preferably, the power of ultrasound is 300 W, the frequency is 60 kHz, and the time is 3 min.

[0018] Preferably, the drying temperature is 25° C. and the drying time is 1 h.

[0019] The beneficial effects of the present invention are:

[0020] The method for extracting quercetin based on ultrasound-filtration provided by the present invention can achieve efficient extraction of quercetin by first dissolving the sample with hydrogen peroxide, then filtering under ultrasonic conditions, and finally adding dilute hydrochloric acid. In this process, ultrasound can be used to promote full contact between the sample and hydrogen peroxide, so that the sample is fully dispersed, and filtering under ultrasound effectively improves the filtration efficiency, ensuring that the ineffective components with a particle size greater than 100 μm and less than 10 μm are removed, achieving enrichment of effective components to a certain extent, reducing the time required for the extraction process, greatly reducing the amount of hydrochloric acid used in the subsequent extraction process, and avoiding the use of heavy liquid in the traditional extraction method, reducing the cost required for the extraction process. Through the above method, a quercetin extraction method with high extraction rate, simple operation, simple process and green is provided. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 A flow chart of the method for extracting suspected source classes based on ultrasound-filtration provided by the present invention;

[0022] Figure 2 A flow chart of a method for extracting suspected sources based on ultrasound-filtration provided in Comparative Example 1 of the present invention;

[0023] Figure 3 The microscope analysis result of Example 1 of the present invention;

[0024] Figure 4 This is the microscope analysis result of Comparative Example 1 of the present invention. DETAILED DESCRIPTION

[0025] In order to make the purpose, technical solutions and advantages of the present invention more clear, the present invention is described in detail below with reference to the accompanying drawings and specific embodiments.

[0026] It should also be noted that, in order to avoid obscuring the present invention due to unnecessary details, only structures and / or processing steps closely related to the scheme of the present invention are shown in the drawings, while other details that are not closely related to the present invention are omitted.

[0027] In addition, it should be noted that the terms "comprises", "includes" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or apparatus that includes a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or apparatus.

[0028] See also Figure 1 As shown, the method for extracting suspected source classes based on ultrasound-filtration provided by the present invention comprises the following steps:

[0029] The samples containing the queasigens were dried and ground to obtain the queasigens samples with silt particle size (particle size range greater than 0.0039 mm);

[0030] The sample is added into hydrogen peroxide to dissolve and fully disperse the particles; under ultrasonic conditions, the sample solution is filtered using mesh sieves with a pore size of 100 μm and a pore size of 10 μm in turn to retain effective samples within the particle size range of 10-100 μm;

[0031] The solids left on the 10μm sieve after filtration are added to dilute hydrochloric acid and fully reacted for 24 hours under stirring conditions to remove carbonates, organic matter and calcium in the sample, and then centrifuged, washed and dried to obtain solid analytes. During the application process, the solid analytes can be dispersed in a dispersant (such as acetone, etc.) as needed for analysis and identification.

[0032] In the above technical scheme, efficient extraction of the suspected source can be achieved by first dissolving the sample with hydrogen peroxide, then filtering under ultrasonic conditions, and finally adding dilute hydrochloric acid. In this process, ultrasonic action can be used to promote full contact between the sample and hydrogen peroxide, so that the sample is fully dispersed, and filtering under ultrasonic action effectively improves the filtration efficiency, ensuring that the invalid components with a particle size greater than 100μm and less than 10μm are removed, achieving enrichment of effective components to a certain extent, reducing the time required for the extraction process, greatly reducing the amount of hydrochloric acid used in the subsequent extraction process, and avoiding the use of heavy liquid in the traditional extraction method, reducing the cost required for the extraction process, and simplifying the extraction process.

[0033] Secondly, by filtering with meshes of 100 μm and 10 μm in aperture, physical screening can be used to effectively remove invalid impurities (clay particles, silt, etc.), reduce the amount of chemical reagents (hydrochloric acid), and improve the acquisition rate and extraction efficiency of the extracts; at the same time, the reduction in the amount of hydrochloric acid used can reduce its corrosion loss to the active ingredients of the source, and the results obtained are more ideal. In particular, adding hydrochloric acid in the later stage of extraction can shorten the contact time between hydrochloric acid and the active ingredients during the extraction process, and delay the corrosion loss of the acidic reagent (hydrochloric acid) to the active ingredients of the source.

[0034] As an embodiment of the present invention, the samples containing apocrysts are derived from apocryst sediment samples produced in Proterozoic, Paleozoic, Mesozoic strata and the like.

[0035] As an embodiment of the present invention, the power of ultrasound is 300W, the frequency is 60kH, and the time is 3min.

[0036] As an embodiment of the present invention, the mass percentage of hydrogen peroxide is 12%, and the added amount is 50 mL, wherein g / L represents the mass of solid added to 1 L of hydrogen peroxide solution.

[0037] As an embodiment of the present invention, the centrifugal conditions are: rotation speed 4000 rpm, time 3 min.

[0038] As an embodiment of the present invention, the mass percentage of dilute hydrochloric acid is 20%, and the ratio of the mass of the solid matter to the volume of the dilute hydrochloric acid is 1:3. In other embodiments, if there is still a small amount of silicate precipitate after the reaction of the sample with the dilute hydrochloric acid, a small amount of hydrofluoric acid with a mass percentage of 30% (such as 10-20mL) can be added according to the actual situation. It should be noted that the stirring in the above technical solution is mechanical stirring, and its purpose is to make each reactant fully contact.

[0039] As an embodiment of the present invention, the drying temperature is 25° C. and the drying time is 1 hour.

[0040] The method for extracting suspicious source classes based on ultrasound-filtration proposed by the present invention is further described below in conjunction with specific embodiments:

[0041] Example 1

[0042] This embodiment provides a method for extracting suspected source classes based on ultrasound-filtration, comprising the following steps:

[0043] 20 g of the sample containing parasites (from the Huangniuyan Village section of Yiling District, Yichang City, Hubei Province (111°8′25.008″ east longitude, 30°40′12.137″ north latitude)) was dried and ground to obtain a parasite sample of silt-grade;

[0044] The sample was added into 30 mL of 12% hydrogen peroxide to dissolve and fully disperse the particles; under ultrasonic conditions, the sample solution was filtered using mesh sieves with a pore size of 100 μm and a pore size of 10 μm in turn to retain effective samples within the particle size range of 10-100 μm; wherein the ultrasonic power was 300 W, the frequency was 60 kHz, and the time was 3 min;

[0045] The solid matter remaining on the 10 μm sieve after filtration was added to 20 mL of 20% by mass dilute hydrochloric acid and fully reacted for 24 hours under stirring conditions to remove carbonates, organic matter and calcium in the sample; the solid matter after the reaction was washed with deionized water several times until the supernatant was neutral (pH = 7), and the solution was centrifuged at 4000 rpm for 3 minutes, the solid part was collected, and dried in an oven at 80°C for 60 minutes to obtain a solid source of the compound.

[0046] The above solid analytes are added to acetone and analyzed and identified using a microscope. The results are as follows: Figure 3 As shown in the figure, it can be seen that the field of view is mainly suspicious source, with less impurities, and the suspicious source is easier to distinguish. Figure 4 The comparison results show that the extraction method of this embodiment can achieve high-purity extraction of chelonoids.

[0047] Comparative Example 1

[0048] This comparative example provides a method for extracting quercetin based on ultrasound-filtration. The extraction process is as follows: Figure 2 As shown, the following steps are included:

[0049] 20 g of the sample containing the parasites was dried and ground to obtain the parasite sample of silt-grade (derived from the Huangniuyan Village section of Yiling District, Yichang City, Hubei Province (111°8′25.008″E, 30°40′12.137″N));

[0050] The sample was added to 50 mL of 20% by mass dilute hydrochloric acid, stirred with a manual glass rod, and allowed to react for 24 h. The solid matter after the reaction was washed several times with deionized water until the supernatant was neutral (pH = 7), and the solution containing the solid at the bottom was collected;

[0051] Add 100 mL of 30% hydrofluoric acid by mass to the above solution containing solids, stir thoroughly with a polyethylene plastic stirring rod and react for 24 hours. After the reaction is completed, wash the solid matter after the reaction with deionized water several times until the supernatant is neutral (pH=7), and dry the sample;

[0052] The dried sample was floated with a heavy liquid with a specific gravity of 2.2, and the solution after flotation was poured into a 20% by mass acetic acid solution to separate the quercetin from the heavy liquid; the separated solution was centrifuged at 3000 rpm for 3 minutes, the upper clear liquid was removed, and the solution containing solids at the bottom was retained, and washed with deionized water for multiple times until the supernatant was neutral (pH = 7), and dried in an oven at 80°C for 120 minutes to obtain solid quercetin. The heavy liquid was specifically a zinc iodide solution (a mixed solution after the reaction of KI + Zn + HI), and the flotation time was 4 hours;

[0053] The above solid analytes are added to acetone and analyzed and identified using a microscope. The results are as follows: Figure 4 As shown in the figure, it can be seen that the suspected source class is covered by impurities, which seriously interfere with the effective target objects, and the suspected source class cannot be directly distinguished from the field of view, indicating that this method cannot achieve effective extraction of the suspected source class.

[0054] During the experiment, in order to improve the accuracy of the experiment, 10 samples were selected for comparison experiments. All 10 samples were from the Huangniuyan Village section of Yiling District, Yichang City, Hubei Province (111°8′25.008″ east longitude, 30°40′12.137″ north latitude). The analysis and identification results of Example 1 and Comparative Example 1 are shown in Table 1. From the data in the table, it can be seen that the extraction method proposed in the present invention can effectively extract the quercetin in the sample. This is because: the extraction method proposed in the present invention can effectively remove clay impurities in the sample by filtering under ultrasonic conditions first. In addition, hydrochloric acid is added after most of the impurities are removed. Compared with the traditional extraction method (Comparative Example 1), the amount of hydrochloric acid reagent used is greatly reduced, the addition time of hydrochloric acid is delayed, and the contact time between hydrochloric acid and the quercetin in the sample during the extraction process is shortened. The corrosion loss of the effective ingredient quercetin by the acidic reagent (hydrochloric acid) is delayed, and the result obtained is more ideal.

[0055] Table 1 Analysis and identification results of Example 1 and Comparative Example 1

[0056]

[0057] The above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solution of the present invention.

Claims

1. A method for extracting suspicious source classes based on ultrasound-filtration, characterized in that: The steps include: Drying and grinding the sample containing the quercetin to obtain a quercetin sample of silt particle size; The sample is added into hydrogen peroxide to dissolve and fully disperse the particles; under ultrasonic conditions, the sample solution is filtered using mesh sieves with a pore size of 100 μm and a pore size of 10 μm in turn to retain effective samples within the particle size range of 10-100 μm; The solid material remaining on the 10 μm sieve after filtration was added to dilute hydrochloric acid, and fully reacted for 24 hours under stirring conditions, and then centrifuged, washed, and dried to obtain a solid source of the substance.

2. The method according to claim 1, characterized in that The mass percentage of hydrogen peroxide is 12%.

3. The method according to claim 1 or 2, characterized in that: The amount of hydrogen peroxide added was 50 mL.

4. The method according to claim 1, characterized in that: The mass percentage of dilute hydrochloric acid is 20%.

5. The method according to claim 1 or 4, characterized in that: The ratio of the mass of solid matter to the volume of dilute hydrochloric acid is 1:

3.

6. The method according to claim 1, characterized in that The centrifugal conditions were: speed 4000 rpm, time 3 min.

7. The method according to claim 1, characterized in that The samples containing ambiguity species were produced in Proterozoic, Paleozoic and Mesozoic strata.

8. The method according to claim 1, characterized in that The power of ultrasound was 300W, the frequency was 60 kHz, and the time was 3 min.

9. The method according to claim 1, characterized in that: The drying temperature was 25°C and the drying time was 1 h.

Images