CN211863943U - Solid-phase extraction column for pineapple pulp matrix biochar filler - Google Patents
Solid-phase extraction column for pineapple pulp matrix biochar filler Download PDFInfo
- Publication number
- CN211863943U CN211863943U CN202020069753.9U CN202020069753U CN211863943U CN 211863943 U CN211863943 U CN 211863943U CN 202020069753 U CN202020069753 U CN 202020069753U CN 211863943 U CN211863943 U CN 211863943U
- Authority
- CN
- China
- Prior art keywords
- biochar
- filler
- phase extraction
- pineapple
- solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 235000007119 Ananas comosus Nutrition 0.000 title claims abstract description 40
- 239000000945 filler Substances 0.000 title claims abstract description 39
- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 36
- 239000011159 matrix material Substances 0.000 title claims abstract description 16
- 244000099147 Ananas comosus Species 0.000 title 1
- 241000234671 Ananas Species 0.000 claims abstract description 39
- 235000013372 meat Nutrition 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000011148 porous material Substances 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 3
- -1 polypropylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 2
- 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 description 16
- 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 description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 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
- 239000000243 solution Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 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
- 238000011084 recovery Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 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
- 239000003513 alkali Substances 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 108010067094 microcystin Proteins 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 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
- 108010049746 Microcystins Proteins 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 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
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 description 1
- 231100000171 higher toxicity Toxicity 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 201000007270 liver cancer Diseases 0.000 description 1
- 208000014018 liver neoplasm Diseases 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Abstract
The utility model relates to a pineapple day meat matrix biochar filler solid-phase extraction post, it includes cylinder (1), be provided with sieve (2) and lower sieve (3) in cylinder (1), it is provided with filler (4) to go up between sieve (2) and lower sieve (3), filler (4) are pineapple meat biochar filler, cylinder (1) top is provided with inlet (5), cylinder (1) bottom is provided with liquid outlet (6), liquid outlet (6) position department is provided with out liquid takeover (7). The utility model relates to a pineapple meat matrix biochar filler solid phase extraction post, it uses pineapple meat biochar as the filler, and extraction post is capacious, interference killing feature is strong and repeatedly usable.
Description
Technical Field
The utility model relates to a pineapple pulp matrix biochar filler solid phase extraction column, which can be used for enriching microcystin-RR in water and belongs to the technical field of chemical detection pretreatment.
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.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that a pineapple meat matrix biochar filler solid phase extraction post is provided to above-mentioned prior art, it uses pineapple meat biochar as the filler, and extraction post is capacious, the interference killing feature is strong and repeatedly usable.
The utility model provides a technical scheme that above-mentioned problem adopted does: the solid-phase extraction column comprises a column body, wherein an upper sieve plate and a lower sieve plate are arranged in the column body, a filler is arranged between the upper sieve plate and the lower sieve plate, and the filler is a pineapple pulp biochar filler.
Preferably, a liquid inlet is formed in the top of the column body, a liquid outlet is formed in the bottom of the column body, and a liquid outlet connecting pipe is arranged at the position of the liquid outlet.
Preferably, the cylinder material is polypropylene.
Preferably, the inner diameter of the column body is 13mm, the outer diameter of the column body is 16mm, and the length of the column body is 7-10 cm.
Preferably, the diameter of the upper sieve plate and the lower sieve plate is 13mm, and the thickness of the upper sieve plate and the lower sieve plate is 1.6 mm.
Preferably, the upper sieve plate and the lower sieve plate are uniformly provided with sieve pores, and the diameter of each sieve pore is 50 μm.
Preferably, the preparation method of the pineapple meat biochar filler comprises the following steps:
preferably, the pineapple is cleaned, peeled and cut, 500g of the broken pineapple flesh is put into a corundum crucible and placed into a muffle furnace under the protection of argon, and the corundum crucible is baked for 3 hours at 95 ℃ to remove 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.
Compared with the prior art, the utility model has the advantages of:
1. the utility model has low production cost, simple manufacture and convenient industrialization;
2. the capacity of the biochar filler solid phase extraction column prepared by the utility model is as large as 4000 mug, and the standard recovery rate is between 82.7 and 93.8 percent;
3. the biochar filler solid-phase extraction column of the utility model is acid and alkali resistant, can be repeatedly used after being processed, 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 present invention will be described in further detail with reference to the following embodiments.
The utility model relates to a preparation method of a solid-phase extraction column of pineapple pulp matrix biochar filler, 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 all technical solutions formed by equivalent transformation or equivalent replacement should fall within the protection scope of the claims of the present invention.
Claims (6)
1. A solid phase extraction column of pineapple pulp matrix biochar filler is characterized in that: it includes cylinder (1), be provided with upper screen plate (2) and lower sieve plate (3) in cylinder (1), be provided with filler (4) between upper screen plate (2) and lower sieve plate (3), filler (4) are pineapple flesh biochar filler.
2. The pineapple meat matrix biochar filler solid-phase extraction column as claimed in claim 1, is characterized in that: the liquid inlet (5) is arranged at the top of the column body (1), the liquid outlet (6) is arranged at the bottom of the column body (1), and the liquid outlet connecting pipe (7) is arranged at the position of the liquid outlet (6).
3. The pineapple meat matrix biochar filler solid-phase extraction column as claimed in claim 1, is characterized in that: the cylinder (1) is made of polypropylene.
4. The pineapple meat matrix biochar filler solid-phase extraction column as claimed in claim 1, is characterized in that: the inner diameter of the column body (1) is 13mm, the outer diameter of the column body is 16mm, and the length of the column body is 7-10 cm.
5. The pineapple meat matrix biochar filler solid-phase extraction column as claimed in claim 1, is characterized in that: the diameter of the upper sieve plate (2) and the lower sieve plate (3) is 13mm, and the thickness of the upper sieve plate and the lower sieve plate is 1.6 mm.
6. The pineapple meat matrix biochar filler solid-phase extraction column as claimed in claim 1, is characterized in that: the upper sieve plate (2) and the lower sieve plate are uniformly provided with sieve pores, and the diameter of each sieve pore is 50 mu m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020069753.9U CN211863943U (en) | 2020-01-14 | 2020-01-14 | Solid-phase extraction column for pineapple pulp matrix biochar filler |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020069753.9U CN211863943U (en) | 2020-01-14 | 2020-01-14 | Solid-phase extraction column for pineapple pulp matrix biochar filler |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211863943U true CN211863943U (en) | 2020-11-06 |
Family
ID=73260102
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202020069753.9U Expired - Fee Related CN211863943U (en) | 2020-01-14 | 2020-01-14 | Solid-phase extraction column for pineapple pulp matrix biochar filler |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211863943U (en) |
-
2020
- 2020-01-14 CN CN202020069753.9U patent/CN211863943U/en not_active Expired - Fee Related
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107096500B (en) | Method for preparing magnetic biochar from traditional Chinese medicine residues, magnetic biochar and application | |
| CN107403698B (en) | A kind of application preparing the method for activated carbon and its active carbon of preparation using biomass | |
| CN111318272B (en) | Biochar capable of adsorbing heavy metals and preparation method and application thereof | |
| CN109482152B (en) | Metal oxide composite nano material based on eggshell membrane template, and preparation method and application thereof | |
| CN109621929B (en) | Regeneration method and application of waste activated carbon | |
| CN112263989A (en) | Method for preparing magnetic biochar by one-step method | |
| CN111111739B (en) | Preparation of nitrogen-doped biochar material and method for improving dark fermentation hydrogen production performance | |
| CN110559991A (en) | Modified biochar and preparation method and application thereof | |
| CN111533201B (en) | Biomass water treatment agent based on porous coffee grounds and preparation method thereof | |
| CN211863943U (en) | Solid-phase extraction column for pineapple pulp matrix biochar filler | |
| CN111208228A (en) | Method for enriching and purifying MC-RR in water by using solid phase extraction column | |
| CN111266084A (en) | Porous aquatic plant-based biomass charcoal material and application thereof | |
| CN112958033B (en) | Gaseous iodine adsorption material with foamed nickel as framework and preparation method and application thereof | |
| CN110252247A (en) | A kind of spherical shape microballon shape walnut shell Quito hole carbon adsorbing material and its preparation method and application | |
| KR20120132175A (en) | Method for Preparing Anthracite-based High Surface Powder Activated Carbon | |
| CN111228855A (en) | Preparation method of pineapple pulp matrix biochar filler solid-phase extraction column | |
| CN113828277A (en) | Modified biochar and preparation method and application thereof | |
| CN111790352B (en) | Adsorbent capable of removing heavy metals in industrial wastewater and preparation method thereof | |
| CN110980654B (en) | Method for cleaning active alumina balls in hydrogen peroxide production | |
| CN110846043A (en) | Biomass charcoal heavy metal composite passivator and preparation method thereof | |
| CN113479876A (en) | Belladonna herb residue porous carbon and preparation method and application thereof | |
| CN109319777A (en) | A kind of pinecone base prepares the method and its application of biological activated carbon | |
| CN113578265A (en) | Preparation and application method of modified corncob biochar adsorbent | |
| CN210186877U (en) | Anhydrous ethanol preparation device utilizing molecular sieve membrane | |
| CN109046271B (en) | Preparation method of water treatment adsorbent based on composite biomass-based material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20201106 |