CN107445242A - A kind of adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions - Google Patents

A kind of adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions Download PDF

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Publication number
CN107445242A
CN107445242A CN201710822086.XA CN201710822086A CN107445242A CN 107445242 A CN107445242 A CN 107445242A CN 201710822086 A CN201710822086 A CN 201710822086A CN 107445242 A CN107445242 A CN 107445242A
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China
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adsorbed film
antibiotics
sea conditions
multiple classes
under sea
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CN201710822086.XA
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CN107445242B (en
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陈景文
解怀君
李雪花
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Dalian University of Technology
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Dalian University of Technology
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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
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • 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
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • 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
    • C02F2101/34—Organic compounds containing oxygen
    • 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
    • C02F2101/36—Organic compounds containing halogen
    • 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
    • C02F2101/38—Organic compounds containing nitrogen
    • 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
    • C02F2101/40—Organic compounds containing sulfur

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Medicinal Preparation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention belongs to diffusion thin film technique field, there is provided a kind of adsorbed film that Multiple Classes of Antibiotics is fixed under sea conditions.A kind of adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions, it includes the toners of XDA 1, agarose powder and ultra-pure water, and its mass ratio is 10：1.5：100；Adsorbed film diameter 25mm, thickness 0.5mm；The described adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions is in Chinese red.The specific surface area of the described resins of XDA 1 is 1279m2g‑1, aperture 30nm.The present invention it is a kind of under sea conditions synchronously fix Multiple Classes of Antibiotics adsorbed film adsorption capacity it is big.Adsorbed film specific surface area prepared by the present invention is big, strong to weak hydrophobicity antibiotic adsorption capacity, and compared with other types resin material, it is bigger to the adsorbance of antibiotic in the seawater, adsorption capacity is stronger.

Description

A kind of adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions
Technical field
The invention belongs to diffusion thin film technique field, is related to a kind of suction that Multiple Classes of Antibiotics is fixed under sea conditions Membrane.
Background technology
Micropollutants in seawater are ecology and the important risk source of health, have that ambient concentration is low, pollution situation The characteristics of multiple elements design, big health risk.The pollution of antibiotic and ecological risk especially merit attention in seawater, and it can induce carefully The bacterium resistance to the action of a drug, cause the appearance of resistant gene, so can not only influence the ecological balance, can also give human body health care belt to carry out very big prestige The side of body.Therefore, the level of pollution for determining antibiotic in seawater is significant to evaluating its ecological risk.
Common antibiotic sample mode moves to laboratory and carries out pre-treatment, test sample actively to sample after sampling.Actively adopt Sample manpower, resource consumption are big, and sample transport is not convenient, and pre-treatment flow is cumbersome.Corresponding passive sampling is in recent years The focus of research.Passive sampling is time saving, laborsaving, and the pre-treatment steps such as filtering, enrichment, and energy are completed simultaneously in sampling process The time weighted average concentration of pollutant is provided.Diffusion thin film technique (Diffusive gradients in thin- Films, DGT) one kind as passive sampling, the characteristics of its dynamics samples is more smart compared with for other passive sampling technologies It is accurate, convenient.
At present DGT be applied to trace metal in fresh water, in the measure of organic matter and seawater trace metal measure, its The application for organic matter especially antibiotic has no report in the seawater.Document " Journal of Environmental Monitoring.2012,14(6):It is assembled in 1523 " using XAD-18 adsorbed films in DGT and determines antibiotic in fresh water, but Adsorbed film performance under high ionic strength reduces, it is impossible to applied to sea conditions.Seawater matrix condition shows as alkaline pH (7.9-8.2), high ionic strength (about 0.7M), most of antibiotic dissociate under the conditions of the pH, show as molecular state, from Sub- state coexists, due under the conditions of Competition, Coulomb repulsion and high ionic strength sorbing material internal void change etc. factor, often DGT adsorption layers can not show antibiotic good absorption property on this condition.
XDA-1 macroporous absorbent resins are the non-polar polymer adsorbents of a kind of high-crosslinking-degree, high-specific surface area.Its high ratio Surface area and continuous pore structure assign its excellent absorption property to antibiotic.It is widely used in antibiotic in pharmaceutical field Separation ＆ Purification.
The content of the invention
It is adapted to detect for it is an object of the invention to provide one kind using XDA-1 macroporous absorbent resins as made of adsorbent in seawater The DGT combination phases of the weak hydrophobic organic pollutant such as antibiotic, it can overcome seawater alkaline pH and high ionic strength to absorption Adverse effect.Simple operation, it is easily assembled in DGT, is suitable for the application of the measure of the antibiotic in seawater.
Technical scheme：
A kind of adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions, it includes XDA-1 toners and agar Icing Sugar end, its mass ratio are 10：1.5；Adsorbed film diameter 25mm, thickness 0.5mm；Described is synchronously fixed more under sea conditions The adsorbed film of kind antibiotic is in Chinese red.
The specific surface area of described XDA-1 resins is 1279m2g-1, aperture 30nm.
Beneficial effects of the present invention：
A kind of adsorbed film for synchronously fixing Multiple Classes of Antibiotics under sea conditions of the present invention has high-specific surface area, to weak Hydrophobicity antibiotic adsorption capacity is strong.Compared with other types resin material, its, absorption bigger to the adsorbance of antibiotic in the seawater Ability is stronger.
A kind of adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions of the present invention can overcome pH and ionic strength Influence to adsorbed film absorption antibiotic, is properly applied to DGT, is polluted to determine antibiotic in seawater.
The present invention it is a kind of under sea conditions synchronously fix Multiple Classes of Antibiotics adsorbed film preparation method and prepared Journey is easily controllable, and adsorbed film stable performance made from different batches simultaneously has higher-strength.
Brief description of the drawings
Fig. 1 is that antibiotic absorption of the adsorbed film and other types resin adsorption film of the invention prepared in simulated seawater is total Measure contrast situation；
Fig. 2 is the DGT devices for being assembled with the adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions prepared by the present invention Structural representation；
Fig. 3 (1) be assembled with the DGT devices of adsorbed film prepared by the present invention to the adsorbance of sulfamethoxazole with placing when Between variation diagram.
Fig. 3 (2) is to be assembled with the DGT devices of adsorbed film prepared by the present invention to the adsorbance of Enrofloxacin with standing time Variation diagram.
Fig. 3 (3) is to be assembled with the DGT devices of adsorbed film prepared by the present invention to the adsorbance of chloramphenicol with standing time Variation diagram.
In figure：1 plastic casing；2 adsorbed films；3 diffusion barriers；4 filter membranes.
Embodiment
To be best understood from present disclosure, below by embodiment, the invention will be further described, but the cited case It is not intended to limit protection scope of the present invention.
Embodiment 1
Preparation flow is as follows：
Step 1, prepare XDA-1 functional resin powder
(1) XDA-1 macroreticular resins are dried, ground with pulverizer；
(2) toner after grinding is sieved twice, continues to employ center section；
Step 2, the XDA-1 toners that step 1 is screened out, is activated with methanol, afterwards with ultrapure water wash；
Step 3, the resin after step 2 activation elution and agarose powder, ultra-pure water are pressed into 10 (quality)：1.5 (matter Amount)：100 (volumes) are uniformly mixed so as to obtain glue solution；
Step 4, the mixed solution that step 3 is obtained are placed on magnetic stirring apparatus heating stirring to clear, while hot Irrigate to the inner space thickness for preheating (50 DEG C) in advance to be kept flat in 0.5mm glass mold, be cooled to after about 30-40min Room temperature.
Step 5, the gel mould after the cooling that step 4 is obtained cut into a diameter of 25mm disk, produce required suction Membrane.
Preferably, the sieve size of crossing twice described in step 1 is 200 mesh and 400 mesh, and Sieving and casing is 38 and 75 microns.
Preferably, the activation described in step 2, washing is carry out using methanol, ultra-pure water successively, resin used, first Alcohol, ultrapure water volume ratio are about 1：8：8.
Embodiment 2
Adsorbed film prepared by the present invention is placed in the 10mL antibiotic simulated seawater solution of various concentrations, the concentration of setting Gradient is 10,20,50,100,150,200 μ g/L, and shaking table concussion is adsorbed 24 hours.Use ultra performance liquid chromatography tandem mass spectrum Antibiotic concentration in solution before and after measure absorption, to calculate ratio of adsorption (%) of the adsorbed film to antibiotic.It can be seen by table 1 Go out, for most of antibiotic, the ratio of adsorption of the adsorbed film prepared by the present invention is above 90%, and adsorption effect is excellent It is different, show that it is applied to the feasibility of antibiotic in DGT measure seawater.
Adsorbed film prepared by the present invention of table 1 is in various concentrations solution to the ratio of adsorption (%) of antibiotic
Embodiment 3
DGT containing adsorbed film prepared by the present invention is applied to the measure of antibiotic in actual seawater.DGT is immersed in 8 hours in seawater, adsorbed film is taken out, adsorbed film is eluted twice using methanol of the 5mL containing 0.1% formic acid, liquid nitrogen will be eluted afterwards It is blown to and closely does, reuses liquid phase redissolution, finally carry out quantitative analysis using ultra performance liquid chromatography tandem mass spectrum.Passively In sampling process, while actively sampling is carried out as control.As a result show, passive sampling and traditional active sample mode, survey The antibiotic levels obtained have preferable uniformity.
The antibiotic measurement result of sampling in actual seawater containing the DGT of adsorbed film prepared by the present invention and actively of table 2

Claims (2)

1. a kind of adsorbed film that Multiple Classes of Antibiotics is synchronously fixed under sea conditions, it is characterised in that described adsorbed film includes XDA-1 toners and agarose powder, its mass ratio are 10：1.5；The diameter 25mm of adsorbed film, thickness 0.5mm；Adsorbed film In Chinese red.
2. the adsorbed film according to claim 1 that Multiple Classes of Antibiotics is synchronously fixed under sea conditions, it is characterised in that institute The specific surface area for the XDA-1 resins stated is 1279m2g-1, aperture 30nm.
CN201710822086.XA 2017-09-13 2017-09-13 Adsorption film for synchronously fixing multiple antibiotics under seawater condition Active CN107445242B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110108809A (en) * 2019-04-29 2019-08-09 南京大学 A kind of measuring method of essence crudefiber crop drug
CN110327903A (en) * 2019-07-19 2019-10-15 大连理工大学 A kind of preparation method and application of antibiotics molecular engram adsorbed film
CN110702802A (en) * 2019-10-24 2020-01-17 上海海洋大学 Method for passively monitoring antibiotic content in aquaculture water in situ

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS598176B2 (en) * 1977-12-02 1984-02-23 ベイラ−・カレツジ・オブ・メデイシン Resin for selectively removing antibiotics from bacterially infected body fluid samples and method of using the same
CN101058068A (en) * 2007-05-31 2007-10-24 浙江工商大学 Macroporous adsorption resin special used for separating antibiotic and its preparation method
CN104492376A (en) * 2014-12-19 2015-04-08 南京大学 Preparation method of activated carbon adsorption film and method for measuring bisphenol substances in wetland soil or sediment based on thin-film diffusion gradient technique
CN107037193A (en) * 2017-06-22 2017-08-11 泉州师范学院 A kind of water body free state pollutant passive sampling apparatus and the method for sampling

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS598176B2 (en) * 1977-12-02 1984-02-23 ベイラ−・カレツジ・オブ・メデイシン Resin for selectively removing antibiotics from bacterially infected body fluid samples and method of using the same
CN101058068A (en) * 2007-05-31 2007-10-24 浙江工商大学 Macroporous adsorption resin special used for separating antibiotic and its preparation method
CN104492376A (en) * 2014-12-19 2015-04-08 南京大学 Preparation method of activated carbon adsorption film and method for measuring bisphenol substances in wetland soil or sediment based on thin-film diffusion gradient technique
CN107037193A (en) * 2017-06-22 2017-08-11 泉州师范学院 A kind of water body free state pollutant passive sampling apparatus and the method for sampling

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHANG-ER CHEN等: ""A novel passive water sampler for in situ sampling of antibiotics"", 《J. ENVIRON. MONIT.》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110108809A (en) * 2019-04-29 2019-08-09 南京大学 A kind of measuring method of essence crudefiber crop drug
CN110108809B (en) * 2019-04-29 2021-09-28 南京大学 Method for measuring fine sesame drugs
CN110327903A (en) * 2019-07-19 2019-10-15 大连理工大学 A kind of preparation method and application of antibiotics molecular engram adsorbed film
CN110702802A (en) * 2019-10-24 2020-01-17 上海海洋大学 Method for passively monitoring antibiotic content in aquaculture water in situ

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