CN111208228A - Method for enriching and purifying MC-RR in water by using solid phase extraction column - Google Patents
Method for enriching and purifying MC-RR in water by using solid phase extraction column Download PDFInfo
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- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 62
- JIGDOBKZMULDHS-UHFFFAOYSA-N cyanogenosin-RR Natural products N1C(=O)C(CCCN=C(N)N)NC(=O)C(C)C(C(O)=O)NC(=O)C(CCCN=C(N)N)NC(=O)C(C)NC(=O)C(=C)N(C)C(=O)CCC(C(O)=O)NC(=O)C(C)C1C=CC(C)=CC(C)C(OC)CC1=CC=CC=C1 JIGDOBKZMULDHS-UHFFFAOYSA-N 0.000 title claims abstract description 44
- JIGDOBKZMULDHS-UUHBQKJESA-N microcystin RR Chemical compound C([C@H](OC)[C@@H](C)\C=C(/C)\C=C\[C@H]1[C@@H](C(=O)N[C@H](CCC(=O)N(C)C(=C)C(=O)N[C@H](C)C(=O)N[C@@H](CCCN=C(N)N)C(=O)N[C@H]([C@H](C)C(=O)N[C@@H](CCCN=C(N)N)C(=O)N1)C(O)=O)C(O)=O)C)C1=CC=CC=C1 JIGDOBKZMULDHS-UUHBQKJESA-N 0.000 title claims abstract description 44
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- 238000000034 method Methods 0.000 title claims abstract description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 54
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 5
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- 241000234671 Ananas Species 0.000 claims description 37
- 235000007119 Ananas comosus Nutrition 0.000 claims description 37
- 239000000945 filler Substances 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 235000013372 meat Nutrition 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
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- 238000011049 filling Methods 0.000 claims description 2
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- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- 108010004476 microcystin RR Proteins 0.000 description 7
- JIGDOBKZMULDHS-HZJVMCKBSA-N microcystin RR Natural products CO[C@@H](Cc1ccccc1)[C@@H](C)C=C(C)C=C[C@@H]2NC(=O)[C@H](CCCNC(=N)N)NC(=O)[C@@H](C)[C@@H](NC(=O)[C@H](CCCNC(=N)N)NC(=O)[C@@H](C)NC(=O)C(=C)N(C)C(=O)CC[C@@H](NC(=O)[C@H]2C)C(=O)O)C(=O)O JIGDOBKZMULDHS-HZJVMCKBSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000000746 purification Methods 0.000 description 4
- DIDLWIPCWUSYPF-UHFFFAOYSA-N microcystin-LR Natural products COC(Cc1ccccc1)C(C)C=C(/C)C=CC2NC(=O)C(NC(CCCNC(=N)N)C(=O)O)NC(=O)C(C)C(NC(=O)C(NC(CC(C)C)C(=O)O)NC(=O)C(C)NC(=O)C(=C)N(C)C(=O)CCC(NC(=O)C2C)C(=O)O)C(=O)O DIDLWIPCWUSYPF-UHFFFAOYSA-N 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- SRUWWOSWHXIIIA-UKPGNTDSSA-N Cyanoginosin Chemical compound N1C(=O)[C@H](CCCN=C(N)N)NC(=O)[C@@H](C)[C@H](C(O)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](C)NC(=O)C(=C)N(C)C(=O)CC[C@H](C(O)=O)N(C)C(=O)[C@@H](C)[C@@H]1\C=C\C(\C)=C\[C@H](C)[C@@H](O)CC1=CC=CC=C1 SRUWWOSWHXIIIA-UKPGNTDSSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
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- 108010067094 microcystin Proteins 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 206010019851 Hepatotoxicity Diseases 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
- 230000007686 hepatotoxicity Effects 0.000 description 1
- 231100000304 hepatotoxicity Toxicity 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- General Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
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Abstract
The invention relates to a method for enriching and purifying MC-RR in water by using a solid phase extraction column, which comprises the following steps: step one, purifying the solid phase extraction column by using 5ml of pure water, 5ml of methanol and 5ml of acetic acid aqueous solution with pH value of 4; step two, taking 20ml of water sample containing MC-RR, adjusting the pH value to 1-12 with acetic acid, and enriching the water sample through a purified solid phase extraction column at a rate of 1 ml/min; and step three, eluting by using 5ml of a mixed solution of 95% methanol and 5% ammonia water with pH value of 10, drying the eluent by using nitrogen, and dissolving by using 0.5ml of methanol for LC-MS/MS detection. The solid phase extraction column used in the method for enriching and purifying the MC-RR in water has larger capacity, stronger anti-interference capability and reusability, effectively ensures the final enriching and purifying effect and reduces the cost.
Description
Technical Field
The invention relates to a method for enriching and purifying MC-RR in water by using a solid phase extraction column, which can be used for enriching microcystin-RR in water and belongs to the technical field of pretreatment of chemical detection.
Background
The biochar is a carbon-rich product generated by thermal cracking of biomass under an anoxic condition, and has strong adsorption capacity due to the rich microporous structure, oxygen-containing functional groups and large specific surface area. In recent years, the biochar has wide application prospects in soil remediation and treatment of organic matter pollution in water environments. The pineapple pulp has an acidic characteristic and a unique pore size structure, and can be used for preparing biochar to better exert the advantages of the biochar.
Microcystin (MC) has hepatotoxicity and is one of three major liver cancer factors. The microcystins are cyclic heptapeptides, and 70 structural variants are reported, wherein the variants with higher toxicity and relatively higher content are as follows: MC-LR, MC-RR and MC-YR. MC-LR was the most toxic and most of the concern. However, the content of MC-RR in the blue algae bloom in Taihu lake is the largest, and the produced harm is probably larger than that of MC-LR. However, MC-RR has not been used as a monitoring index in China, and has not been limited in magnitude. At present, the detection of MC-RR is mainly performed by HPLC-MS and HPLC methods. However, because the MC-RR content in the water environment is low, purification and enrichment are required. Compared with the traditional C18 and other fillers, the biochar has higher adsorption capacity and acid and alkali resistance due to the special physical and chemical structure, and can be reused after special treatment. At present, no research report on the application of biochar in preparing a solid phase extraction column exists. Therefore, the pineapple pulp biochar is used for preparing the solid phase extraction column for enriching the microcystin-RR in water, and compared with the traditional solid phase extraction column, the solid phase extraction column has larger capacity, stronger anti-interference capability and reusability, and has positive significance for monitoring MC-RR pollution in lake Tai water and repairing water.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for enriching and purifying MC-RR in water by using a solid phase extraction column in the prior art, wherein the used solid phase extraction column has larger capacity and stronger anti-interference capability, can be repeatedly used, effectively ensures the final enriching and purifying effect and reduces the cost.
The technical scheme adopted by the invention for solving the problems is as follows: a solid phase extraction column is used for enriching and purifying MC-RR in water, and the method comprises the following steps:
step one, purifying the solid phase extraction column by using 5ml of pure water, 5ml of methanol and 5ml of acetic acid aqueous solution with pH value of 4;
step two, taking 20ml of water sample containing MC-RR, adjusting the pH value to 1-12 with acetic acid, and enriching the water sample through a purified solid phase extraction column at a rate of 1 ml/min;
and step three, eluting by using 5ml of a mixed solution of 95% methanol and 5% ammonia water with pH value of 10, drying the eluent by using nitrogen, and dissolving by using 0.5ml of methanol for LC-MS/MS detection.
Preferably, the solid-phase extraction column comprises a column body, an upper sieve plate and a lower sieve plate are arranged in the column body, and a pineapple pulp matrix biochar filler is arranged between the upper sieve plate and the lower sieve plate.
Preferably, the preparation method of the pineapple pulp matrix biochar filler comprises the following steps:
cleaning pineapple, peeling, cutting, placing 500g of broken pineapple flesh in a corundum crucible, placing in a muffle furnace under the protection of argon, baking at 95 ℃ for 3h, and removing water; and then, continuously heating the muffle furnace to 650 ℃ at a speed of 55 ℃/min under the protection of argon, keeping for 4h, cooling, soaking the modified pineapple meat biochar for 24h in 5% acetic acid, washing to be neutral, drying, and screening with a 100-mesh screen to be dried to obtain the pineapple meat biochar filler.
Preferably, the lower sieve plate is arranged at the bottom of the column tube, 5g of the pineapple pulp biochar filler is filled in the solid-phase extraction column tube, the solid-phase extraction column tube is oscillated to uniformly disperse the pineapple pulp biochar and then compact the pineapple pulp biochar, and then the upper sieve plate is fixed above the solid-phase extraction column filler, so that the pineapple pulp matrix biochar filler solid-phase extraction column is prepared.
Preferably, the water sample of MC-RR in step two is adjusted to pH 4 with acetic acid.
Preferably, the column capacity is 4000. mu.g by measuring the MC-RR content in the column liquid by passing the excess micro MC-RR solution through a solid phase extraction column.
Preferably, the MC-RR solution with known low, medium and high concentrations is added to pass through a solid phase extraction column, the content of the enriched and purified MC-RR is measured, and the standard addition recovery rate is calculated to be between 82.7 and 93.8 percent.
Preferably, after the third step, the solid phase extraction column is washed with 10ml of a mixture of 95% methanol + 5% aqueous ammonia solution with pH of 10, 10ml of methanol, and 10ml of pure water at a rate of 1ml/min, and then dried with nitrogen gas, and the column is left for the next time to be used repeatedly.
Compared with the prior art, the invention has the advantages that:
1. the solid phase extraction column used in the invention has low cost, simple manufacture and convenient industrialization;
2. the biochar filler solid-phase extraction column used in the invention has large capacity which can reach 4000 mu g, strong anti-interference capability and standard recovery rate of 82.7-93.8%;
3. the biochar filler solid-phase extraction column used in the invention is acid and alkali resistant, can be reused after treatment, and has low cost.
Drawings
FIG. 1 is a scanning electron microscope image of pineapple flesh biochar filler.
FIG. 2 is a schematic structural diagram of a pineapple flesh biochar solid-phase extraction column.
FIG. 3 is a schematic diagram of the recovery rate of MC-RR in water by using a solid-phase extraction column of pineapple meat biochar for enrichment and purification.
Wherein:
Filler 4
A liquid outlet connecting pipe 7.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
The invention relates to a preparation method of a pineapple pulp matrix biochar filler solid-phase extraction column, which comprises the following steps:
step one, preparing the pineapple meat biochar filler
Cleaning pineapple, peeling, cutting, placing 500g of broken pineapple flesh in a corundum crucible, placing in a muffle furnace under the protection of argon, baking at 95 ℃ for 3h, and removing water; then, continuously heating the muffle furnace to 650 ℃ at a speed of 55 ℃/min under the protection of argon, keeping for 4h, cooling, soaking the modified pineapple meat biochar for 24h in 5% acetic acid, washing to be neutral, drying, and airing through a 100-mesh net to obtain the pineapple meat biochar filler; scanning electron microscope images of the prepared pineapple meat biochar filler are taken, and are shown in figure 1;
secondly, arranging a lower sieve plate at the bottom of a solid-phase extraction column tube, filling 5g of pineapple pulp biochar filler into the solid-phase extraction column tube, oscillating the solid-phase extraction column tube to uniformly disperse the pineapple pulp biochar and then compacting the pineapple pulp biochar, and fixing an upper sieve plate above the solid-phase extraction column filler to obtain the pineapple pulp matrix biochar filler solid-phase extraction column as shown in figure 2;
the column tube 1 is a polypropylene shell, the inner diameter of the column tube is 13mm, the outer diameter of the column tube is 16mm, the length of the column tube is 7cm, the diameters of the upper sieve plate 2 and the lower sieve plate 3 are 13mm, the thickness of the sieve plate is 1.6mm, and the aperture of the sieve plate is 50 micrometers.
The method for enriching and purifying the MC-RR in water by using the pineapple meat matrix biochar filler solid-phase extraction column comprises the following steps:
step one, purifying a pineapple pulp matrix biochar filler solid-phase extraction column by using 5ml of pure water, 5ml of methanol and 5ml of acetic acid aqueous solution with pH value of 4;
step two, taking 20ml of water sample containing MC-RR, adjusting the pH value to 4 by using acetic acid, and enriching by passing through a purified solid phase extraction column at a rate of 1 ml/min;
the enrichment and purification of microcystin-RR in water by 5ml of acetic acid aqueous solution with pH value of 1-12 at 1ml/min are investigated, and the experimental result shows that the adsorption effect is best when the pH value is 4, so that the pH value of 4 is selected as the optimal pH value of the liquid to be detected passing through a solid phase extraction column;
eluting with 5ml of a mixed solution of 95% methanol and 5% ammonia water with the pH value of 10, drying the eluent by nitrogen, dissolving the eluent with 0.5ml of methanol, and detecting by using an LC-MS/MS (liquid chromatography-mass spectrometer);
passing the excessive microcystin-RR solution through a solid phase extraction column, and measuring the content of microcystin-RR in the column solution to obtain the column capacity of 4000 mug;
adding known solutions of microcystin-RR with low, medium and high concentrations, passing through solid phase extraction column, measuring the content of microcystin-RR after enrichment and purification, and calculating the standard recovery rate to be 82.7-93.8%, as shown in FIG. 3;
and step four, sequentially washing the solid-phase extraction column with 10ml of mixed solution of 95% methanol and 5% ammonia water solution with pH value of 10, 10ml of methanol and 10ml of pure water at a rate of 1ml/min, drying the column with nitrogen, and keeping the column for next reuse, so that the regeneration of the solid-phase extraction column is realized, the utilization rate of the solid-phase extraction column is improved, and the use cost is reduced.
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (8)
1. A method for enriching and purifying MC-RR in water by using a solid phase extraction column is characterized by comprising the following steps:
step one, purifying the solid phase extraction column by using 5ml of pure water, 5ml of methanol and 5ml of acetic acid aqueous solution with pH value of 4;
step two, taking 20ml of water sample containing MC-RR, adjusting the pH value to 1-12 with acetic acid, and enriching the water sample through a purified solid phase extraction column at a rate of 1 ml/min;
and step three, eluting by using 5ml of a mixed solution of 95% methanol and 5% ammonia water with pH value of 10, drying the eluent by using nitrogen, and dissolving by using 0.5ml of methanol for LC-MS/MS detection.
2. The method for enriching and purifying MC-RR in water by using the solid phase extraction column as claimed in claim 1, wherein: the solid phase extraction column comprises a column body, an upper sieve plate and a lower sieve plate are arranged in the column body, and a pineapple pulp matrix biochar filler is arranged between the upper sieve plate and the lower sieve plate.
3. The method for enriching and purifying MC-RR in water by using the solid phase extraction column as claimed in claim 2, wherein: the preparation method of the pineapple meat matrix biochar filler comprises the following steps:
cleaning pineapple, peeling, cutting, placing 500g of broken pineapple flesh in a corundum crucible, placing in a muffle furnace under the protection of argon, baking at 95 ℃ for 3h, and removing water; and then, continuously heating the muffle furnace to 650 ℃ at a speed of 55 ℃/min under the protection of argon, keeping for 4h, cooling, soaking the modified pineapple meat biochar for 24h in 5% acetic acid, washing to be neutral, drying, and screening with a 100-mesh screen to be dried to obtain the pineapple meat biochar filler.
4. The method for enriching and purifying MC-RR in water by using the solid phase extraction column as claimed in claim 3, wherein: arranging a lower sieve plate at the bottom of the column tube, filling 5g of the pineapple pulp biochar filler in the solid-phase extraction column tube, oscillating the solid-phase extraction column tube to uniformly disperse the pineapple pulp biochar and then compacting, and fixing an upper sieve plate above the solid-phase extraction column filler to obtain the pineapple pulp matrix biochar filler solid-phase extraction column.
5. The method for enriching and purifying MC-RR in water by using the solid phase extraction column as claimed in claim 1, wherein: the water sample of MC-RR in step two was adjusted to pH 4 with acetic acid.
6. The method for enriching and purifying MC-RR in water by using the solid phase extraction column as claimed in claim 1, wherein: the excessive micro MC-RR solution passes through a solid phase extraction column, and the content of MC-RR in the column solution is measured to obtain the column capacity of 4000 mu g.
7. The method for enriching and purifying MC-RR in water by using the solid phase extraction column as claimed in claim 1, wherein: adding known MC-RR solutions with three concentrations of low concentration, medium concentration and high concentration, passing through a solid phase extraction column, measuring the content of the enriched and purified MC-RR, and calculating the standard addition recovery rate to be between 82.7 and 93.8 percent.
8. The method for enriching and purifying MC-RR in water by using the solid phase extraction column as claimed in claim 1, wherein: and after the third step, washing the solid-phase extraction column by using 10ml of a mixed solution of 95% methanol and a solution of 5% pH (pH) 10 ammonia, 10ml of methanol and 10ml of pure water at a rate of 1ml/min, drying the column by using nitrogen, and keeping the column for next repeated use.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114280197A (en) * | 2021-12-29 | 2022-04-05 | 安徽环球药业股份有限公司 | Washing method of morphine solid-phase extraction column |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974080A (en) * | 2010-11-22 | 2011-02-16 | 中国科学院水生生物研究所 | Method for separating and purifying microcystin by utilizing series-connected solid phase extraction columns |
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