CN111721600A - Method for extracting and separating dissolved organic matters in soil and dissolved organic matters extracted and separated by method - Google Patents

Method for extracting and separating dissolved organic matters in soil and dissolved organic matters extracted and separated by method Download PDF

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CN111721600A
CN111721600A CN202010594955.XA CN202010594955A CN111721600A CN 111721600 A CN111721600 A CN 111721600A CN 202010594955 A CN202010594955 A CN 202010594955A CN 111721600 A CN111721600 A CN 111721600A
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张银萍
李晓宁
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Abstract

The invention discloses a method for extracting and separating dissolved organic matters in soil and the dissolved organic matters extracted and separated by the method; the method comprises (1) dissolving and separating: sequentially carrying out inorganic acid dissolution, oscillation, centrifugation and filtration on the collected soil, and then collecting filtrate; (2) adsorption desalting: adsorbing the filtrate obtained in the step (1) by adopting a solid phase extraction method, eluting dissolved organic matters in the filtrate, and collecting the eluent; (3) concentration and enrichment: and (3) concentrating and enriching the eluent obtained in the step (2), and dissolving the concentrated sample by using a methanol water solution to obtain an extracted sample, namely the high-purity salinity-free DOM sample. According to the invention, inorganic acid is used as a solvent, and the three steps of dissolving separation, adsorption desalting and concentration enrichment are respectively carried out, so that the soluble organic matters in the soil can be efficiently extracted, the extraction method is simple, the extraction efficiency is high, and the alicyclic aromatic hydrocarbon with low solubility and various different DOM molecules can be obtained.

Description

Method for extracting and separating dissolved organic matters in soil and dissolved organic matters extracted and separated by method
Technical Field
The invention belongs to soil environment analytical chemistry, and particularly relates to a method for extracting and separating dissolved organic matters in soil.
Background
Dissolved Organic Matter (DOM) is a continuum of organic matter (e.g., low molecular weight organic acids, carbohydrates, free amino acids, etc., high molecular weight phenols, enzymes, polysaccharides, humus, etc.) of varying molecular weights and molecular structures that can pass through a 0.45 μm filter membrane, and is one of the largest pools of activated organic carbon on earth. It is widely present in soil, sediment and natural water, and its concentration content is usually expressed by soluble organic carbon. DOM is a complex mixture of ingredients, different sources of DOM, and its composition and nature are very different, usually contains many functional groups such as phenolic hydroxyl, carboxyl, alcoholic hydroxyl, carbonyl. It is a natural complexing agent and an adsorption carrier, and has great influence on the activation, migration, transformation and final homing of inorganic pollutants such as heavy metals and organic pollutants in soil, the biogeochemical cycle of nutrients and the like, so people carry out a great deal of research on DOM in soil.
However, the soil components are complex, a unified method for DOM extraction is not available at present, and treatment methods such as headspace, air stripping and trapping, liquid-liquid extraction, resin adsorption and separation, ultrafiltration and reverse osmosis are mainly available at present, but the methods have the defects of low extraction rate, organic matter loss in the extraction process and the like
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides the method for extracting and separating the soluble organic matter (DOM) in the soil, which can effectively overcome the defects that the extraction rate of the DOM in the soil is low, the organic matter is lost in the extraction process and the like, can obtain a high-concentration DOM sample, is convenient to implement, and can obtain different types of soluble organic matters.
The invention also provides the dissolved organic matters extracted and separated by the extraction and separation method.
The technical scheme is as follows: the invention relates to a method for extracting and separating soluble organic matters in soil, which comprises the following steps:
(1) dissolving and separating: dissolving organic matters in soil by using an inorganic acid solution, specifically, sequentially performing inorganic acid dissolution, oscillation, centrifugation and filtration on the collected soil, and then collecting filtrate;
(2) adsorption desalting: adsorbing the filtrate obtained in the step (1) by adopting a solid phase extraction method, eluting dissolved organic matters in the filtrate, and collecting the eluent;
(3) concentration and enrichment: and (3) concentrating and enriching the eluent obtained in the step (2), and dissolving the concentrated sample by using a methanol water solution to obtain an extracted sample, namely the dissolved organic matter in the soil, which can be used as a high-resolution mass spectrum computer sample.
Wherein, the inorganic acid solution in the step (1) has the concentration of 0.01-0.2 mol.L-1The dissolving ratio of the soil and the inorganic acid is 1:5-20 g/mL.
Wherein the oscillation condition in the step (1) is as follows: 100 to 300rpm, 10 to 50 ℃, 10 to 100 hours; the centrifugation conditions were: 3000-10000 rpm for 3-60 min; the filtration conditions were: GF/F glass fiber filter membrane with pore size of 0.45 μm or nylon filter membrane with pore size of 0.45 μm.
Further, the dissolving and separating in the step (1) can be repeated for 1-10 times.
Wherein, the solid phase extraction column of the solid phase extraction in the step (2) is a C18, XAD-8 or PPL polymer-based extraction column.
And (3) activating the solid-phase extraction column before solid-phase extraction in the step (2), wherein the activation process comprises soaking and activating for 2-4 hours by using methanol or acetonitrile (both mass spectrum levels), and washing for 2-4 times by using pure water with the pH value of 2-4.
Wherein the column passing speed of the adsorption in the step (2) is 2-5 mL/min-1The eluent in the elution process is methanol or acetonitrile (both in mass spectrum level).
Wherein, the concentration and enrichment in the step (3) adopt a nitrogen blowing instrument for concentration or evaporation concentration.
Preferably, the methanol in step (3) is a 50% volume fraction methanol aqueous solution.
The method for extracting and separating the soluble organic matters in the soil extracts and separates the soluble organic matters in the soil.
Wherein the soluble organic matters in the soil comprise alicyclic aromatic hydrocarbons with low solubility, wherein O/C is more than 0 and less than 0.25, H/C is more than 0.5 and less than 1.25, and the extraction efficiency of the soluble organic matters in the soil is improved by more than 50%.
According to the invention, inorganic acid is used as a solvent, soluble organic matters which can be dissolved in water but adsorbed on the surfaces of mineral components are obtained, and the solid phase extraction technology is adopted to completely enrich the soluble organic matters in the water phase and remove salt, so that the subsequent mass spectrometry is facilitated. The invention breaks through the traditional extraction and enrichment mode, finds the enrichment separation method which can better reflect DOM components, and is beneficial to the deep research of the soil organic chemistry subject.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) compared with the conventional extraction and separation method taking water as a solvent, the method disclosed by the invention adopts an inorganic acid solution as the solvent, so that the extraction rate of soluble organic matters in soil is improved, and the extraction of DOM with relatively high content is facilitated.
(2) The TOC content measured by the method provided by the invention is about four times of that measured by the traditional water-soluble method, the sample injection volume can be reduced during on-machine detection, and the extraction efficiency is improved.
(3) The extraction and separation of more soluble organic matters in the soil are realized, more soluble organic matters with different molecular weights, different molecular weight ranges and different types are obtained in mass spectrometry, and the time and the cost are saved. In conclusion, the method for extracting and separating the soluble organic matters in the soil is established by adopting the inorganic acid as the solvent and combining the solid phase extraction technology, so that the extraction rate is greatly improved, more soluble organic matters with different molecular weight ranges are obtained, and the method is an efficient extraction and separation method.
Drawings
FIG. 1 is a high resolution mass spectrum and relative abundance distribution diagram of DOM with pure water as solvent and 5 times of dissolution, separation and extraction;
figure 2 is a high resolution mass spectrum and relative abundance distribution graph of DOM with dilute hydrochloric acid solution as solvent and 5 times of dissolution separation extraction.
FIG. 3 is a high resolution mass spectrum and relative abundance distribution diagram of DOM with pure water as solvent and 10 times of dissolution, separation and extraction;
figure 4 is a high resolution mass spectrum and relative abundance distribution plot of DOM with dilute nitric acid solution as solvent and 10 times of dissolution separation extraction.
Detailed Description
The present invention will be described in further detail with reference to examples.
Soil sample sources and treatment methods in the examples:
soil sample sources in the examples: and (3) removing fine roots and stones from the rice soil in the soil station in Jiangxi, and screening the soil by using a 2mm sieve to obtain a pretreatment sample. The operating conditions for mass spectrometric detection in the examples were: samples were measured at 120mL h by Bruker SolariX mass spectrometry using a 9.4T superconducting magnet and electrospray ion source configuration-1The flow rate of the solution is continuously injected into the electrospray device, the voltage of an electrospray needle is set to be 3.8kV, and all samples adopt a negative ion mode. Ions are accumulated for 0.1s in the hexapole ion trap and then are introduced into the cyclotron ion chamber. The lower and upper limits of the mass are set to m/z 200Da and 1000Da, respectively.
The calculation formula used in the examples:
Figure BDA0002554700570000031
example 1
Dissolving a pretreated soil sample and a solvent according to a mass-volume ratio of 1:10g/mL, sequentially dissolving (1:10g/mL), shaking (100rpm, 10 ℃ and 10 hours), centrifuging (3000rpm and 3 minutes) and filtering (a GF/F glass fiber filter membrane with the aperture of 0.45 mu m) by adopting a pure water solution, and repeatedly dissolving, shaking, centrifuging and filtering for 10 times to collect filtrate; 10mL of the obtained filtrate was taken to measure the TOC concentration, which was 5.343mg/L, and the required injection volume at the TOC concentration was calculated to be 375mL based on the mass spectrometric injection concentration of 100 ppm. Adsorbing and eluting dissolved organic matter in the filtrate by solid phase extraction, activating PPL polymer-based solid phase extraction column (soaking in methanol for 2 hr, washing with pure water with pH of 2 for 2 times), and washing 375mL filtrate with 2mL min-1Eluting with 10mL of methanol after adsorbing and passing through the column, and collecting the eluent; and concentrating and enriching the obtained eluent by using a nitrogen blowing instrument, and dissolving the concentrated sample by using 10mL of methanol aqueous solution with the volume ratio of 50:50 to obtain an extracted sample. The mass spectrometry of the extracted sample is shown in figure 3.
CollectingThe filtrate is detected by high resolution mass spectrum to obtain alicyclic aromatic hydrocarbon with low solubility (O/C is more than 0 and less than 0.25, H/C is more than 0.5 and less than 1.25), and C detected in soilcHhOoNnThe molecular formula number (S/N is more than or equal to 6) is 344.
Example 2
Dissolving the pretreated soil sample and a solvent according to the mass-to-volume ratio of 1:10g/mL, sequentially dissolving (1:10g/mL), shaking (200rpm, 30 ℃, 25h), centrifuging (5000rpm, 10min) and filtering (a nylon filter membrane with the aperture of 0.45 mu m) by adopting a pure water solution, and repeatedly dissolving, shaking, centrifuging and filtering for 5 times to collect filtrate; 10mL of the obtained filtrate was taken to determine the TOC concentration, which was 5.13mg/L, and the sample volume required for the TOC concentration was calculated to be 390mL based on the mass spectrometry sample concentration of 100 ppm. Adsorbing and eluting dissolved organic matters in the filtrate by solid phase extraction, activating PPL polymer-based solid phase extraction column (soaking in methanol for 4 hr, washing with pure water with pH of 2 for 2 times), and washing 390mL filtrate with 2mL min-1Eluting with 10mL of methanol after adsorbing and passing through the column, and collecting the eluent; and concentrating and enriching the obtained eluent by using a nitrogen blowing instrument, and dissolving the concentrated sample by using 10mL of methanol aqueous solution with the volume ratio of 50:50 to obtain an extracted sample.
The collected filtrate is detected by high resolution mass spectrometry to obtain alicyclic aromatic hydrocarbon with low solubility (O/C is more than 0 and less than 0.25, H/C is more than 0.5 and less than 1.25), and C detected in soilcHhOoNnThe molecular formula number (S/N is more than or equal to 6) is 320. The mass spectrometry of the extracted sample is shown in figure 1.
Example 3
Dissolving a pretreated soil sample and a solvent according to a mass-volume ratio of 1:10g/mL, sequentially dissolving (1:10g/mL), shaking (300rpm, 30 ℃, 25h), centrifuging (10000rpm, 10min) and filtering (a GF/F glass fiber filter membrane with the aperture of 0.45 mu m) by adopting a pure water solution, and repeatedly dissolving, shaking, centrifuging and filtering for 5 times to collect filtrate; adsorbing and eluting soluble organic substances in the filtrate by solid phase extraction, activating C18 solid phase extraction column (soaking in acetonitrile for 4 hr, washing with pure water of pH 4 for 2 times), and filtering with 5 mL/min-1Eluting with 10mL of acetonitrile after adsorbing and passing through the column, and collecting eluent; and concentrating and enriching the obtained eluent by using a nitrogen blowing instrument, and dissolving the concentrated sample by using 10mL of methanol aqueous solution with the volume ratio of 50:50 to obtain an extracted sample.
Example 4
Dissolving the pretreated soil sample and a solvent according to the mass-volume ratio of 1:10g/mL, and adopting 0.01 mol.L-1Dissolving hydrochloric acid solution (1:10g/mL), shaking (200rpm, 30 deg.C, 25h), centrifuging (5000rpm, 30min), filtering (GF/F glass fiber filter membrane with pore size of 0.45 μm), repeating dissolving, shaking, centrifuging, and filtering for 5 times, and collecting filtrate; 10mL of the obtained filtrate was taken to measure the TOC concentration, which was 19.63mg/L, and the sample volume required for the TOC concentration was calculated to be 100mL based on the mass spectrometric sample concentration of 100 ppm. Adsorbing and eluting soluble organic matter in the filtrate by solid phase extraction, activating PPL polymer-based solid phase extraction column (soaking in methanol for 4 hr, washing with pure water with pH of 2 for 2 times), and washing 100mL filtrate with 2mL min-1Eluting with 10mL of methanol after adsorbing and passing through the column, and collecting the eluent; and concentrating and enriching the obtained eluent by using a nitrogen blowing instrument, and dissolving the concentrated sample by using 10mL of methanol aqueous solution with the volume ratio of 50:50 to obtain an extracted sample. The mass spectrometry of the extracted sample is shown in figure 2.
The collected filtrate is detected by high resolution mass spectrometry to obtain alicyclic aromatic hydrocarbon with low solubility (O/C is more than 0 and less than 0.25, H/C is more than 0.5 and less than 1.25), and C detected in soilcHhOoNnThe molecular formula number (S/N is more than or equal to 6) is 344.
The extraction solvent of example 4 was hydrochloric acid in mineral acid to give 344 molecular formulas; while the same volume of water was used as solvent in example 2, a molecular formula number of 320 was obtained and it is evident from figure 2 that acid dissolution gave more molecular types than the aqueous solution method.
Example 5
Dissolving the pretreated soil sample and a solvent according to the mass-volume ratio of 1:10g/mL, and adopting 0.01 mol.L-1The sulfuric acid solution was sequentially dissolved (1:10g/mL), shaken (200rpm, 50 ℃ C., 10 hours), centrifuged (3000rpm, 3min), filtered (well)Nylon filter membrane with diameter of 0.45 μm), repeating dissolving, shaking, centrifuging, and filtering for 10 times to collect filtrate; adsorbing and eluting soluble organic substances in the filtrate by solid phase extraction, activating PPL polymer-based solid phase extraction column (soaking in acetonitrile for 4 hr, washing with pure water with pH of 4 for 2 times), and washing the filtrate with 5 mL/min-1Eluting with 10mL of acetonitrile after adsorbing and passing through the column, and collecting eluent; and concentrating and enriching the obtained eluent by using a nitrogen blowing instrument, and dissolving the concentrated sample by using 10mL of methanol aqueous solution with the volume ratio of 50:50 to obtain an extracted sample.
Example 6
Dissolving the pretreated soil sample and a solvent according to the mass-volume ratio of 1:10g/mL, and adopting 0.2 mol.L-1Dissolving (1:10g/mL), shaking (300rpm, 30 ℃, 10h), centrifuging (3000rpm, 30min), filtering (GF/F glass fiber filter membrane with the aperture of 0.45 mu m), repeating the dissolving, shaking, centrifuging and filtering processes for 10 times, and collecting the filtrate; 10mL of the obtained filtrate was taken to measure the TOC concentration, which was 20.54mg/L, and the sample volume required for the TOC concentration was calculated to be 97mL based on the mass spectrometric sample concentration of 100 ppm. Adsorbing and eluting dissolved organic matters in the filtrate by solid phase extraction, activating PPL polymer-based solid phase extraction column (soaking in methanol for 2 hr, washing with pure water with pH of 2 for 4 times), and washing 97mL filtrate with 2mL min-1Eluting with 10mL of methanol after adsorbing and passing through the column, and collecting the eluent; and concentrating and enriching the obtained eluent by using a nitrogen blowing instrument, and dissolving the concentrated sample by using 10mL of methanol aqueous solution with the volume ratio of 50:50 to obtain an extracted sample. The mass spectrum analysis chart of the extracted sample is shown in the attached 4.
The collected filtrate is detected to obtain alicyclic aromatic hydrocarbon with low solubility (O/C is more than 0 and less than 0.25, H/C is more than 0.5 and less than 1.25), and C detected in soilcHhOoNnThe molecular formula number (S/N is more than or equal to 6) is 356.
Example 6 extraction solvent was nitric acid in mineral acid to give a molecular formula number of 356, while the same volume of water as in example 1 gave a molecular formula number of 344 and clearly from figure 4 it can be seen that acid dissolution gave a higher molecular type than water solubility.
Example 7
Dissolving the pretreated soil sample and a solvent according to the mass-volume ratio of 1:5g/mL, and adopting 0.2 mol.L-1Sequentially dissolving, shaking (100rpm, 10 deg.C, 100h), centrifuging (10000rpm, 3min), filtering (nylon filter membrane with pore diameter of 0.45 μm), repeating dissolving, shaking, centrifuging, and filtering for 5 times, and collecting filtrate; adsorbing and eluting soluble organic substances in the filtrate by solid phase extraction, activating C18 solid phase extraction column with methanol (MS grade) for 2 hr, washing with pure water of pH 2 for 2 times, and filtering with 2 mL/min-1Eluting with 10mL of methanol (MS grade) after adsorbing and passing through the column, and collecting the eluent; and (3) evaporating and concentrating the obtained eluent, and dissolving the concentrated sample by using 10mL of methanol aqueous solution with the volume ratio of 50:50 to obtain an extracted sample.
Example 8
Dissolving the pretreated soil sample and a solvent according to the mass-volume ratio of 1:20(g/mL) and adopting 0.1 mol.L-1Sequentially dissolving hydrochloric acid solution, shaking (300rpm, 50 deg.C, 10 hr), centrifuging (3000rpm, 60min), filtering (nylon filter membrane with pore diameter of 0.45 μm), repeating dissolving, shaking, centrifuging, and filtering for 8 times, and collecting filtrate; adsorbing and eluting soluble organic substances in the filtrate by solid phase extraction, activating XAD-8 solid phase extraction column with methanol (MS grade) for 4 hr, washing with pure water of pH 4 for 4 times, and filtering with 5 mL/min-1Eluting with 10mL of methanol after adsorbing and passing through the column, and collecting the eluent; and concentrating and enriching the obtained eluent by using a nitrogen blowing instrument, and dissolving the concentrated sample by using 10mL of methanol aqueous solution with the volume ratio of 50:50 to obtain an extracted sample.
In inventive examples 1, 2, 4, 6, the TOC content of DOM was measured by extracting water and acid 5 and 10 times, respectively, using a PPL solid phase extraction column, as shown in table 1.
TABLE 1
Figure BDA0002554700570000061
As can be seen from Table 1, when DOM in the soil solution with the same concentration is extracted, the TOC content measured by the method provided by the invention is about four times that measured by the traditional water-soluble method, and the sample injection volume can be reduced and the extraction efficiency can be improved during machine detection.

Claims (10)

1. The method for extracting and separating the soluble organic matters in the soil is characterized by comprising the following steps of:
(1) dissolving and separating: sequentially carrying out inorganic acid dissolution, oscillation, centrifugation and filtration on the collected soil, and then collecting filtrate;
(2) adsorption desalting: adsorbing the filtrate obtained in the step (1) by adopting a solid phase extraction method, eluting dissolved organic matters in the filtrate, and collecting the eluent;
(3) concentration and enrichment: and (3) concentrating and enriching the eluent obtained in the step (2), and dissolving the concentrated sample by using a methanol water solution to obtain an extracted sample, namely the high-purity salinity-free DOM sample.
2. The method for extracting and separating soluble organic matter from soil according to claim 1, wherein the concentration of the inorganic acid solution in the step (1) is 0.01 to 0.2 mol-L-1The dissolving ratio of the soil and the inorganic acid is 1:5-20 g/mL.
3. The method for extracting and separating dissolved organic matters from soil according to claim 1, wherein the shaking conditions in step (1) are preferably: 100 to 300rpm, 10 to 50 ℃, 10 to 100 hours; the centrifugation conditions were: 3000-10000 rpm for 3-60 min; the filtration conditions were: GF/F glass fiber filter membrane with pore size of 0.45 μm or nylon filter membrane with pore size of 0.45 μm.
4. The method for extracting and separating soluble organic matters from soil according to claim 1, wherein the dissolving and separating in the step (1) can be repeated for 1 to 10 times.
5. The method for extracting and separating dissolved organic matters from soil according to claim 1, wherein the solid phase extraction column for solid phase extraction in the step (2) is a C18, XAD-8 or PPL polymer-based extraction column.
6. The method for extracting and separating soluble organic matters from soil according to claim 1, wherein the solid phase extraction column is activated before the solid phase extraction in the step (2), the activation process comprises soaking in methanol or acetonitrile for 2-4 h, and washing with pure water at a pH of 2-4 for 2-4 times.
7. The method for extracting and separating soluble organic matters from soil according to claim 1, wherein the column passing speed of the adsorption in the step (2) is 2 to 5 mL-min-1And the eluent in the elution process is methanol or acetonitrile.
8. The method for extracting and separating dissolved organic matters from soil according to claim 1, wherein the concentration and enrichment in the step (3) are performed by nitrogen blowing or evaporation concentration.
9. A method for extracting and separating dissolved organic matter from soil according to any one of claims 1 to 8.
10. Dissolved organic matter in soil according to claim 9, wherein said dissolved organic matter in soil comprises less soluble alicyclic aromatic hydrocarbons, wherein 0 < O/C < 0.25, 0.5 < H/C < 1.25.
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CN113155558A (en) * 2021-02-05 2021-07-23 北京市理化分析测试中心 Method for extracting, separating and purifying micro-plastic in soil
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CN113405877A (en) * 2021-07-30 2021-09-17 苏州含光微纳科技有限公司 Biomolecule extraction method
CN113405877B (en) * 2021-07-30 2024-04-02 苏州含光微纳科技有限公司 Biological molecule extraction method
CN113624831A (en) * 2021-08-05 2021-11-09 广东农工商职业技术学院 Method for separating enriched sediment organic nitrogen and determining isotope and content
CN113624831B (en) * 2021-08-05 2024-05-10 广东农工商职业技术学院 Method for separating and enriching organic nitrogen in sediment and measuring isotope and content
CN114216951A (en) * 2021-12-08 2022-03-22 中国石油大学(北京) Separation method of sulfonate compounds in sewage and analysis method of soluble organic matter molecule composition

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