CN115254063B - Gel adsorption film, gradient diffusion device and application thereof in artificial sweetener sampling - Google Patents
Gel adsorption film, gradient diffusion device and application thereof in artificial sweetener sampling Download PDFInfo
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Abstract
The application discloses a gel adsorption film, a gradient diffusion device and application thereof in artificial sweetener sampling. The gel adsorption film is prepared according to the following method: adding an adsorption resin filler into a polymerization reaction system of polyacrylamide gel to obtain a mixture system; the polymerization reaction system of the polyacrylamide gel comprises an acrylamide monomer, an initiator and a catalyst; after the mixed system is subjected to polymerization reaction, cooling and forming the system after the polymerization reaction to form a gel adsorption film; the adsorption resin filler is at least one of HLB filler, PWAX filler and WAX filler. The gel adsorption film is filled in the gradient diffusion device, so that the artificial sweetener in the environment to be detected can be quantitatively enriched in situ, the time weighted average concentration of the artificial sweetener in the sampling time period is provided, and the sampling result is more representative; and the measurement result of the artificial sweetener concentration in the environment to be measured is not required to be calibrated, so that the artificial sweetener concentration in the environment to be measured is estimated more accurately.
Description
Technical Field
The application belongs to the technical field of environmental science, and particularly relates to a gel adsorption film, a gradient diffusion device and application of the gel adsorption film and the gradient diffusion device in artificial sweetener sampling.
Background
Artificial sweeteners (ases) are synthetic or semi-synthetic organic compounds that replace sucrose and are widely used in food, beverage, pharmaceutical, personal care products because of their generally much higher sweetness than sucrose. The earliest of the synthetic ases was Saccharin (SAC), after which the sweeteners synthesized were cyclamate (CYC) and Aspartame (ASP) in sequence, which were combined with saccharin and referred to as first generation sweeteners; acesulfame k (ACE) and Sucralose (SUC) were synthesized artificially in 1967 and 1976, respectively, and are called new generation sweeteners because of their difficult biodegradability. As a non-nutritive food additive, as a substitute for sucrose, as fashionable as a product of sucrose, its kind and application have been rapidly developed, in which asia, particularly china, is the largest production and consumer market of asa, because of the fact that as a result of the increasing importance of obesity, diabetes and the like, as the fact that as a result of the fact that as little heat is generated in the human body, the asa is being produced in the human body. Because of the wide application of ASs and their characteristic of not participating in human metabolic reactions, reports of detecting ASs in living sewage treatment systems and natural water bodies are frequent, which also causes a certain concern. In one aspect, some studies indicate that ingestion of ASs may be harmful to humans, as one study in France indicates that obesity and cancer among experimental populations may be associated with long-term consumption of foods containing ASs. On the other hand, the ASs may affect the growth activities of small animals, plants and microorganisms in natural water, thereby affecting the regional ecosystem. Therefore, the concentration and pollution level of the ASs in the domestic sewage system and the natural water body are monitored and researched, and data support can be provided for better understanding of sources, distribution, migration, transformation and ecological toxicity effects of the ASs in the water body.
Currently, sampling methods for ASs in a water body mainly comprise active grabbing and sampling and passive sampling by using a polar organic compound integrated sampling technology (POCIS). Active grab sampling can only provide the instantaneous concentration of the target substance at a specific sampling time, cannot reflect the fluctuation of the concentration of pollutants along with time, and is not representative. The POCIS sampler, however, must perform field calibration on the sampling rate due to different field conditions than laboratory calibration, and hydrodynamic conditions such as flow rate, temperature and turbulence may affect the sampling rate, resulting in uncertainty in estimating the concentration of the target in the water. The gradient diffusion film (diffusive gradients in thin-film, DGT) technology is a high-efficiency passive sampling technology based on Fick's first diffusion law, the DGT technology can quantitatively enrich pollutants to be detected in situ, and the Time Weighted Average (TWA) concentration of the pollutants to be detected passing through diffusion gel with a certain thickness in a sampling time period is measured, so that the defect of active sampling is overcome. In addition, the DGT technology quantifies the diffusion process of the target object in the diffusion glue, so that the target object is insensitive to the change of hydrologic conditions, and measurement errors caused by the change of the hydrologic conditions on site are avoided.
At present, the DGT sampling technology applied to the detection technology of polar organic compounds in natural water bodies is relatively lacking, and particularly the DGT sampling technology aiming at artificial sweeteners is still blank.
Disclosure of Invention
The application aims to overcome the defects of at least one aspect of the prior art, and provides a gel adsorption film, a gradient diffusion device and application thereof in artificial sweetener sampling, so as to solve the technical problems that the sampling concentration of the existing ASs is not representative and the estimation of the concentration of the ASs in a water body is inaccurate.
In order to achieve the object of the above application, in a first aspect of the present application, there is provided a gel adsorption film prepared by:
adding an adsorption resin filler into a polymerization reaction system of polyacrylamide gel to obtain a mixture system; the polymerization reaction system of the polyacrylamide gel comprises an acrylamide monomer, an initiator and a catalyst;
after the mixture system is subjected to polymerization reaction, cooling and forming the system after the polymerization reaction to form the gel adsorption film;
the adsorption resin filler is at least one of HLB (hydrophilic lipophilic balance resin) filler, PWAX (weak anion reverse phase resin) filler and WAX (mixed weak anion resin) filler.
Further, the adsorption resin filler is subjected to methanol and ultrapure water washing and activation treatment.
Further, the initiator is ammonium persulfate; and/or the catalyst is tetramethyl ethylenediamine.
Further, the temperature of the polymerization reaction is 45-47 ℃, and the time of the polymerization reaction is 40-45 min.
In a second aspect of the present application, there is provided a gradient diffusion device, including any one of the above gel adsorption film, diffusion film, protection film and package casing, the protection film the diffusion film with the gel adsorption film is laminated in proper order and is set up in the package casing, the protection film sets up open end one side of package casing.
Further, the diffusion membrane is an agar gel membrane.
Further, the protective film is a PTFE hydrophilic filter film.
In a third aspect of the present application, there is provided an application of a gel adsorption film in artificial sweetener sampling, where the gel adsorption film is placed in an environment to be tested containing artificial sweetener, so that the gel adsorption film adsorbs the artificial sweetener in the environment to be tested.
In a fourth aspect of the present application, there is provided an application of a gradient diffusion device in artificial sweetener sampling, where the gradient diffusion device is placed in an environment to be tested containing artificial sweetener, so that the gradient diffusion device adsorbs the artificial sweetener in the environment to be tested.
Compared with the prior art, the application has the following technical effects:
the gel adsorption film has excellent adsorptivity to the artificial sweetener in the environment to be detected, and can efficiently adsorb the artificial sweetener in the environment to be detected.
The gel adsorption film capable of efficiently adsorbing the artificial sweetener in the environment to be tested is filled in the gradient diffusion device, the artificial sweetener in the environment to be tested can be quantitatively enriched in situ, the time weighted average concentration of the artificial sweetener in the sampling time period is provided, and the sampling result is more representative; and the measurement result of the artificial sweetener concentration in the environment to be measured is not required to be calibrated, so that the artificial sweetener concentration in the environment to be measured is estimated more accurately.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a gradient diffusion apparatus according to an embodiment of the present application;
FIG. 2 is a graph showing the relationship between adsorption quality and adsorption time of ASs by the WAX-DGT apparatus according to example 2 of the present application;
FIG. 3 is a graph showing the relationship between adsorption quality and adsorption time of ASs in a natural water body quantitatively measured by the WAX-DGT apparatus according to example 3 of the present application.
In the figure, 1, a gel adsorption film, 2, a diffusion film, 3, a protection film, 4 and a packaging shell.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved by the present application more clear, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the present application.
In this application, the term "and/or" describes an association relationship of an association object, which means that there may be three relationships, for example, a and/or B may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. The character "/" generally indicates that the context-dependent object is an "or" relationship.
In the present application, "at least one" means one or more, and "a plurality" means two or more. "at least one of" or the like means any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
It should be understood that, in various embodiments of the present application, the sequence number of each process does not mean that the sequence of execution is sequential, and some or all of the steps may be executed in parallel or sequentially, where the execution sequence of each process should be determined by its functions and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weights of the relevant components mentioned in the embodiments of the present application may refer not only to specific contents of the components, but also to the proportional relationship between the weights of the components, and thus, any ratio of the contents of the relevant components according to the embodiments of the present application may be enlarged or reduced within the scope disclosed in the embodiments of the present application. Specifically, the mass described in the specification of the examples of the present application may be a mass unit known in the chemical industry such as μ g, mg, g, kg.
The terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated for distinguishing between objects such as substances from each other. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the present application. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature.
Compared with the active technology, the gradient diffusion film (DGT) technology can quantitatively enrich the pollutants to be detected in situ, determine the Time Weighted Average (TWA) concentration of the pollutants to be detected passing through the diffusion film with a certain thickness in the sampling time period, and make up for the defect of active sampling. And DGT technology is insensitive to hydrodynamic conditions because the thickness of the diffusion membrane is typically thicker than the Diffusion Boundary Layer (DBL), eliminating the need for in situ calibration in a matrix-like solution. Concentration value of analyte in water (C DGT ) The calculation formula (1) of (2) is as follows:
(1)
in the formula (1), M is the amount (ng) of the object to be detected accumulated in the gel adsorption film;t is exposure time(s); d is the diffusion coefficient (cm) of the object to be measured in the diffusion film layer 2 S); a represents the sampling area (cm) of DGT 2 ) The method comprises the steps of carrying out a first treatment on the surface of the Δg is the thickness (cm) of the diffusion film passing before the analyte is absorbed by the binding phase; delta is the thickness (cm) of DBL, when the flow velocity of water is fast enough>0.2 cm/s), delta is negligible.
In a first aspect, embodiments of the present application provide a gel adsorption film prepared according to the following method:
(1) Adding an adsorption resin filler into a polymerization reaction system of polyacrylamide gel to obtain a mixture system; the polymerization reaction system of the polyacrylamide gel comprises an acrylamide monomer, an initiator and a catalyst;
(2) And after the mixture system is subjected to polymerization reaction, cooling and forming the system after the polymerization reaction to form the gel adsorption film.
In the step (1), the adsorbent resin filler is at least one of HLB filler, PWAX filler and WAX filler. In the examples of the present application, experimental tests were performed: the adsorption rate of the WAX filler to the ASs is 75.2% -89.7%, the adsorption rate of the HLB filler to the ASs is 69.8% -82.4%, and the adsorption rate of the PWAX filler to the ASs is 40.2% -86.5%, compared with the HLB filler and the PWAX filler, the WAX filler has better adsorption to the Artificial Sweetener (ASs) in the environment to be tested, and the specific embodiment of the application is exemplified by the preparation of the gel adsorption film by the WAX filler. In order to improve the adsorption performance of the adsorption resin filler to the acs, the adsorption resin filler in the embodiment of the application can be washed and activated by methanol and ultrapure water which are three times the volume of the adsorption resin filler before being used.
In the step (1), ammonium persulfate may be used as an initiator and tetramethyl ethylenediamine may be used as a catalyst in the polymerization reaction system of the polyacrylamide gel. The types of the initiator and the catalyst are not limited to this, and any initiator and catalyst that can promote the polymerization of the acrylamide monomer to form the polyacrylamide gel may be used in the polymerization system. In the specific embodiment of the application, a polymerization reaction system of the polyacrylamide gel comprises an acrylamide solution with the volume fraction of 14-16%, an ammonium persulfate solution with the mass fraction of 9-11% and tetramethyl ethylenediamine, wherein the three solutions are mixed according to the volume ratio of 1000 (5.5-6.5) to 1.4-1.6). The polymerization reaction system can initiate polymerization reaction at 45-47 ℃ for 40-45 min.
The gel adsorption film has excellent adsorptivity to the artificial sweetener in the environment to be detected, and can efficiently adsorb the artificial sweetener in the environment to be detected. The environment to be measured can be water environment, sediment, sludge or soil and other environments.
In a second aspect of the embodiment of the present application, a gradient diffusion device is provided, and the gradient diffusion device is shown in fig. 1, and includes the gel adsorption film 1, the diffusion film 2, the protection film 3 and the package casing 4, where the protection film 3, the diffusion film 2 and the gel adsorption film 1 are sequentially stacked in the package casing 4, and the protection film 3 is disposed on one side of an open end of the package casing 4, that is, on one side that contacts with an environment to be tested and can allow water samples in the environment to be tested to permeate.
The diffusion membrane 2 in the embodiment of the application can be selected from an agar gel membrane or a polyacrylamide gel membrane, and the adsorption rates of the agar gel membrane and the polyacrylamide gel membrane to the ASs in the environment to be detected are low and are below 10%, so that the agar gel membrane and the polyacrylamide gel membrane can be used as the diffusion membranes of the gradient diffusion device. Because the preparation of the agar gel film is more convenient, the specific embodiment of the application uses the agar gel film as a diffusion film. The agar gel film can be prepared by the following method:
adding agar with the mass ratio of 1.4% -1.6% into ultrapure water, heating the solution at 83-87 ℃ and continuously stirring, and simultaneously placing the glass mould into a baking oven and heating to 73-75 ℃. And (3) pouring the solution into a glass mould when the agar is completely dissolved and no suspended particles are visible in the solution. Naturally standing the mold vertically, and cooling the solution to room temperature and condensing to obtain the agar gel film.
The protective membrane 3 of the present embodiment may be selected to be a PTFE hydrophilic filter membrane, i.e., a hydrophilic polytetrafluoroethylene filter membrane. The PTFE hydrophilic filter membrane has extremely low adsorption rate to ASs in the environment to be detected, the adsorption rate is 1.10% -7.49%, and the PTFE hydrophilic filter membrane is used as a protective membrane, so that the influence of the gradient diffusion device on ASs concentration measurement and calculation in the environment to be detected can be reduced.
The packaging shell 4 of the embodiment of the application is made of polytetrafluoroethylene materials, and the adsorption rate of ASs in the environment to be tested of the packaging shell 4 is less than 5%.
According to the gradient diffusion device, the gel adsorption film 1 capable of efficiently adsorbing the artificial sweetener in the environment to be detected is filled in the gradient diffusion device, the diffusion film 2 and the protection film 3 with low adsorption rate of ASs in the environment to be detected are matched, ASs in the environment to be detected can be quantitatively enriched in situ, the time weighted average concentration of the ASs in the sampling time period is provided, and the sampling result is more representative; and the measurement result of the concentration of the ASs in the environment to be measured is not required to be calibrated, so that the concentration estimation of the ASs in the environment to be measured is more accurate.
In a third aspect of the embodiments of the present application, an application of a gel adsorption film in artificial sweetener sampling is provided, where the gel adsorption film is placed in an environment to be tested containing artificial sweetener, so that the gel adsorption film adsorbs the artificial sweetener in the environment to be tested.
In a fourth aspect of the embodiments of the present application, an application of a gradient diffusion device in artificial sweetener sampling is provided, where the gradient diffusion device is placed in an environment to be tested containing artificial sweetener, so that the gradient diffusion device adsorbs the artificial sweetener in the environment to be tested.
The gel adsorption membranes, gradient diffusion devices, and their use in artificial sweetener sampling of embodiments of the present application are illustrated below by a number of specific examples.
Example 1
(1) Preparation of agar gel film (diffusion film): agar of 1.5% by mass was added to ultrapure water, and the solution was heated at 90℃with continuous stirring, while the glass mold was put into an oven and heated to 75 ℃. After the agar was completely dissolved, the solution was poured into a glass mold with a 0.8mm thick spacer sandwiched between the mold and the solution without visible suspended particles. The mold was left to stand naturally, after the solution had cooled to room temperature and coagulated, the glass mold was opened and the gel was cut into discs of 2.5cm diameter to give an agar gel film which was stored in 0.01M NaCl solution at 4 ℃.
(2) Preparing a gel adsorption film: selecting Oasis-WAX solid phase extraction small column with particle size of 30-40 μm, taking out WAX filler, loading into empty column with lower layer of spacer, and cleaning and activating with methanol and ultrapure water with volume of three times of that of the column at flow rate of 1 mL/min. Taking the wet WAX filler, adding an acrylamide solution with the volume fraction of 15%, and uniformly mixing. And adding the ammonium persulfate solution with the mass fraction of 10% and the tetramethyl ethylenediamine into the mixed solution. The volume ratio of the three solutions was 1000:6:1.5, with 2.6mL of acrylamide solution per 1g of filler. After the solutions were mixed uniformly, the solutions were poured into a glass mold having a 0.25mm thick PTFE gasket sandwiched therebetween. The mold is horizontally placed in an oven and heated for 45 minutes at 45-47 ℃, the mold is taken out after the solution in the mold is solidified into a film, and the gel adsorption film is taken out and soaked in sodium chloride solution with the concentration of 0.01M. The solution soaked with the gel adsorption film is replaced every 2 hours, and the solution is taken out after the pH value of the detection solution is lower than 7.0 after 24 hours, so as to obtain the WAX-polyacrylamide gel adsorption film.
(3) Assembly of gradient diffusion device (WAX-DGT device): the DGT housing base was placed horizontally on a tabletop and the WAX-gel adsorption membrane, the agar gel membrane and the PTFE hydrophilic filter membrane were tiled thereon using clean tweezers, respectively. And the DGT cover is buckled, no bubble exists between the films, and the assembly of the WAX-DGT device is completed.
Example 2
Experimental tests were performed on the deployment time of the gradient diffusion device WAX-DGT prepared in example 1 of the present application, and the specific procedure is as follows:
the WAX-DGT apparatus was exposed to a solution with an ASs concentration of 200. Mu.g/L (IS (ionic strength) =0.01M, pH=6.+ -. 0.2, T=22.+ -. 1 ℃,350 rpm), the vessel was covered with aluminum foil, and the WAX-DGT apparatus was removed at 10, 20, 30, 40 and 50 hours. After the WAX-DGT device was taken out, the WAX-DGT housing was rinsed with ultrapure water, the WAX-DGT was removed, the diffusion layer, i.e., the agar gel film layer, was peeled off, the gel adsorption film was placed in a brown bottle, the gel adsorption film was extracted with 5mL of methanol and sonicated twice for 30 minutes each time, the concentration of ASs in the eluent was measured, and the amount of ASs adsorbed by the gel adsorption film was calculated, and was substituted into formula (1) to calculate the WAX-DGT measurement concentration, and the measurement result was shown in FIG. 2.
As seen in FIG. 2, at C DGT Namely, under the condition that the concentration of the target ASs in the solution is basically stable, the adsorption mass M of the target ASs on the gel adsorption film is in direct proportion to the adsorption time t. In the experiment, the adsorption quality and adsorption time of the gel adsorption film to ASs are linearly increased, and the theoretical calculation requirement is met.
Example 3
The gradient diffusion device WAX-DGT prepared in the embodiment 1 of the application is applied to sampling of a field water sample environment, and the specific process is as follows:
selecting two natural water body sampling points, placing three groups of WAX-DGT devices at each sampling point, keeping the WAX-DGT devices at about 15cm below the water surface during placement, and placing the WAX-DGT devices with windows upwards. Three sets of WAX-DGT apparatus were recovered 7 days, 14 days, and 21 days after the standing, and eluted within 24 hours after each recovery and the ASs concentration was measured, and the measurement results are shown in FIG. 3.
As can be seen from FIG. 3, the absorption of ASs in natural bodies of water by the WAX-DGT apparatus increases over a period of three weeks (correlation coefficient R 2 Greater than 0.82), but the adsorption rate of most of the acs in the third week sample was reduced. The results show that the WAX-DGT device can quantitatively measure ASs in natural water, but the placement time is not suitable to exceed two weeks.
The foregoing examples represent only a few embodiments of the present application, which are described in more detail and are not thereby to be construed as limiting the scope of the present application. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.
Claims (5)
1. The application of the gradient diffusion device in artificial sweetener sampling is characterized in that the gradient diffusion device is placed in an environment to be tested containing artificial sweetener, so that the gradient diffusion device adsorbs the artificial sweetener in the environment to be tested;
the gradient diffusion device comprises a gel adsorption film, a diffusion film, a protection film and a packaging shell, wherein the protection film, the diffusion film and the gel adsorption film are sequentially stacked in the packaging shell, and the protection film is arranged on one side of an open end of the packaging shell; the protective film is a PTFE hydrophilic filter film;
the gel adsorption film is prepared according to the following method:
adding an adsorption resin filler into a polymerization reaction system of polyacrylamide gel to obtain a mixture system; the polymerization reaction system of the polyacrylamide gel comprises an acrylamide monomer, an initiator and a catalyst;
after the mixture system is subjected to polymerization reaction, cooling and forming the system after the polymerization reaction to form the gel adsorption film;
the adsorption resin filler is at least one of PWAX filler and WAX filler.
2. The use of a gradient diffusion device according to claim 1, wherein the adsorbent resin filler is cleaned and activated with methanol and ultra-pure water.
3. The use of a gradient diffusion device according to claim 1 for artificial sweetener sampling, wherein the initiator is ammonium persulfate; and/or the catalyst is tetramethyl ethylenediamine.
4. The use of a gradient diffusion device according to any one of claims 1-3 for artificial sweetener sampling, wherein the polymerization reaction is carried out at a temperature of 45-47 ℃ for 40-45 min.
5. Use of a gradient diffusion device according to claim 1, wherein the diffusion membrane is an agar gel membrane.
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