CN111228855A - Preparation method of pineapple pulp matrix biochar filler solid-phase extraction column - Google Patents
Preparation method of pineapple pulp matrix biochar filler solid-phase extraction column Download PDFInfo
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- CN111228855A CN111228855A CN202010050475.7A CN202010050475A CN111228855A CN 111228855 A CN111228855 A CN 111228855A CN 202010050475 A CN202010050475 A CN 202010050475A CN 111228855 A CN111228855 A CN 111228855A
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- biochar
- extraction column
- phase extraction
- solid
- pineapple
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- 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
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
-
- 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
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/206—Packing or coating
-
- 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
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention relates to a preparation method of a pineapple pulp matrix biochar filler solid-phase extraction column, which comprises the following steps: firstly, cleaning pineapples, peeling and chopping, putting 500g of chopped pineapple pulp into a corundum crucible, placing the corundum crucible into a muffle furnace under the protection of argon, and baking at 95 ℃ for 3 hours to remove 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; and secondly, arranging a lower sieve plate at the bottom of the solid-phase extraction column tube, filling 5g of the 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. According to the invention, the pineapple pulp biochar is used as a filler, and the prepared extraction column has large capacity and strong anti-interference capability and can be repeatedly used.
Description
Technical Field
The invention relates to a preparation method of a pineapple meat 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.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a pineapple pulp matrix biochar filler solid-phase extraction column in the prior art, which takes pineapple pulp biochar as a filler, and the prepared extraction column has large capacity, strong anti-interference capability and can be repeatedly used.
The technical scheme adopted by the invention for solving the problems is as follows: a preparation method of a pineapple pulp matrix biochar filler solid-phase extraction column 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;
and secondly, arranging a lower sieve plate at the bottom of the solid-phase extraction column tube, filling 5g of the 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.
Compared with the prior art, the invention has the advantages that:
1. the invention has low production cost, simple manufacture and convenient industrialization;
2. the capacity of the biochar filler solid-phase extraction column prepared by the invention is as large as 4000 mu g, and the standard recovery rate is between 82.7 and 93.8 percent;
3. the biochar filler solid-phase extraction column prepared by the invention is acid and alkali resistant, can be repeatedly used after being treated, and is low in 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 (1)
1. A preparation method of a pineapple pulp matrix biochar filler solid-phase extraction column is characterized by comprising 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;
and secondly, arranging a lower sieve plate at the bottom of the solid-phase extraction column tube, filling 5g of the 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.
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Application publication date: 20200605 |