CN116251571A - Method and device for measuring antiviral drugs - Google Patents
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Abstract
The invention discloses a method and a device for measuring antiviral drugs, wherein the device is a DGT device, and the DGT device comprises an adsorption film, a diffusion film and a filter film which are sequentially overlapped; the adsorption film takes an agarose film as a matrix, adsorption materials are distributed in the agarose film, and the particle size of the adsorption materials is not more than 60 mu m; the adsorption material comprises any one or two of graphitized carbon black particles, MCX resin particles and HLB resin particles.
Description
Technical Field
The invention relates to a detection method and a detection device, in particular to a detection method and a detection device for antiviral drugs.
Background
Antiviral drugs (Antiviral drugs) are prescription drugs for preventing and treating diseases caused by various virus infections, and the mechanism of action is to prevent virus replication and shorten disease time by inhibiting synthesis of enzymes required by viruses in different life stages. With the social development and the increase of the demands for medication and the advancement of medical science, the production and use of antiviral drugs are increasing year by year, and more antiviral drugs are used in clinical treatment research, which shows that antiviral drugs are widely existing in sewage, surface water, groundwater and even drinking water. Although the concentration of antiviral drugs in the environment is low, the antiviral drugs entering the water body still have toxic effects on aquatic organisms, and can cause biological drug resistance. For human body, long-term small-scale exposure to antiviral drugs may reduce the immunity of the human body, producing "three-cause" effects of carcinogenesis, teratogenesis and mutagenesis. With the increasing demand of human beings for disease treatment, the variety and quantity of antiviral drugs must continue to increase. Because the anti-virus agent is easy to remain in the environment for a long time and can generate bad environmental influence under the condition of low concentration, accurate and precise monitoring technology and method are important for analysis, research and early warning of the anti-virus agent in water environment and soil. While reliable, stable sampling and assay techniques not only help assess the environmental risk of antiviral drugs, but are also critical to understanding their environmental behavior.
The existing detection method for antiviral drugs in the environment mainly comprises the steps of collecting and transporting environmental samples back to a laboratory through an active sampling method (a water grabbing sampling method), and then preparing the environmental samples into a state which can be measured by an upper machine through pretreatment technologies such as filtering, extraction, concentration, constant volume and the like. However, due to the low concentration of antiviral drugs in the environment, a large amount of water samples must be taken and all samples must be refrigerated for stable quantitative limits. The water sample is subjected to the treatment processes of filtration, SPE small column enrichment, elution, concentration, constant volume and the like. These processes are not only very cumbersome but also prone to errors. Moreover, the active sampling technology can only acquire the instantaneous concentration of the target drug in the water body at a certain time point, and the instantaneous concentration can not reflect the real pollution condition of the target pollutant because the pollutant concentration in the water body can fluctuate at different times. If the actual level of contaminants is to be reflected by active sampling techniques, multiple samplings are required, which can double the effort.
Compared with the active sampling technology, the passive sampling technology has the greatest advantages that the active sampling technology can measure the time average concentration of pollutants in water, better capture the concentration fluctuation of the pollutants in water, is simple to operate, saves time and labor, does not need complicated pretreatment sample steps before measurement, and has small introduction error. Gradient diffusion film technology (Diffusive gradients in thin films, DGT) is a passive sampling technology based on the first law of diffusion of fick, invented by David Williams and Zhang, university of lankast, uk, over the 90 th century. Since the invention, it has been widely used in the determination of metal ions in an effective state in water, soil and sediment. The time-averaged concentration of the contaminant in the body of water and the bioavailable concentration of the contaminant in the soil can be determined. There are some reports about the measurement of various medical compounds in the environment by using the DGT technology, but there are no reports about the development of the DGT method for antiviral drugs.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems that the prior sampling technology has long time consumption, complex operation and can only obtain instantaneous concentration when the antiviral drugs are sampled and detected, the invention provides a method and a device for measuring the antiviral drugs, which aim to measure the antiviral drugs in water by using a DGT device based on a gradient diffusion film technology, and an adsorption film with high adsorption capacity and stable elution efficiency for the antiviral drugs is prepared by selecting a proper adsorption material, and the diffusion coefficient of the antiviral drugs in a diffusion film is obtained. The method is used for measuring the antiviral drugs in the water body. .
2. Technical proposal
Based on the above, the present invention provides the following technical solutions:
[1] in a first aspect of the present invention, there is provided an adsorption film for antiviral drugs, wherein the adsorption film uses an agarose film as a matrix, and adsorption materials are distributed in the agarose film, and the particle size of the adsorption materials is not more than 60 μm;
wherein,,
the adsorption material includes any one or two of graphitized carbon black particles (hereinafter abbreviated as ENVI-CARB), MCX resin particles (hereinafter abbreviated as MCX) and HLB resin particles (hereinafter abbreviated as HLB);
the adsorption film has a bending angle of not less than 60 °, preferably, a bending angle of approximately 90 °, when bent at least in one direction.
[1.1] an adsorption film for an antiviral drug according to any one of the embodiments of the first aspect of the present invention, the adsorption film having an agarose film as a matrix, graphitized carbon black particles distributed in the agarose film, the particles having a particle diameter of not more than 60 [ mu ] m; or alternatively
The adsorption film takes an agarose film as a matrix, MCX resin particles and HLB resin particles are distributed in the agarose film, and the particle size of the particles is not more than 60 mu m; wherein the MCX resin particles and the HLB resin particles are used in an amount (mass) ratio of (2 to 4): (0.5-1.5), preferably the mass ratio is 3:1.
[1.2] an adsorption film for an antiviral drug according to any one of the embodiments of the first aspect of the present invention, the adsorption film being formed by solidification of an agar solution;
the agar solution is prepared by mixing agar powder, an adsorbing material and pure water according to a mass ratio of 1 (7-13): 50, and heating to boil.
[1.3] an adsorption film for antiviral drugs according to any one of the embodiments of the first aspect of the present invention, the adsorption material is subjected to the following treatment before use:
methanol cleaning, namely soaking and cleaning the adsorption material by using methanol; wherein the volume mass ratio of the methanol to the adsorption material is (8-10) 5mL/g;
cleaning with ultrapure water: and cleaning the adsorption material by using ultrapure water.
[1.4]An adsorption film for antiviral drugs according to any one of the embodiments of the first aspect of the present invention, the adsorption film having not less than 73.41. Mu.g/cm 2 Is used as a catalyst.
[2] In a second aspect of the present invention, there is provided an antiviral drug testing device,
the device is a DGT device;
the DGT device comprises an adsorption film, a diffusion film and a filter film which are sequentially overlapped;
the adsorption film according to any one of claims 1 to 3 is selected.
[2.1] an assay device for antiviral drugs according to any one of the embodiments of the second aspect of the present invention, the diffusion membrane is an agarose membrane;
the filter membrane is a track etched membrane.
[3] In a third aspect of the present invention, there is provided a method for assaying antiviral drugs,
(1) The DGT device is placed in a water body to be detected to adsorb antiviral drugs;
(2) Taking out the DGT device from the water body to be detected, taking out the adsorption film, and eluting by using an eluent to obtain an eluent;
(3) And determining the concentration of the antiviral drugs in the eluent by adopting a high performance liquid chromatography-secondary mass spectrometry method.
[3.1] the method for measuring an antiviral drug according to any one of the embodiments of the third aspect of the present invention, wherein the eluent is a mixed solution containing formic acid and acetonitrile; or,
the eluent is a mixed solution containing ammonia water and acetonitrile.
[3.2] according to the method for measuring an antiviral drug according to any one of the embodiments of the third aspect of the present invention, the mixed solution containing formic acid and acetonitrile, specifically, the mixed solution of an aqueous formic acid solution and chromatographically pure acetonitrile, has a ratio of 4:6, wherein the concentration of the aqueous formic acid solution is 0.2% (V/V).
[3.3] the method for measuring an antiviral drug according to any one of the embodiments of the third aspect of the present invention, wherein the aqueous ammonia and acetonitrile-containing mixed solution, specifically, aqueous ammonia and chromatographic pure acetonitrile mixed solution, has a concentration of 20% (V/V).
[3.2] an assay method for an antiviral drug according to any embodiment of the third aspect of the present invention,
the concentration of the antiviral drugs in the water body to be measured is 0.01-500 mg/L.
Advantageous effects
(1) The device based on the gradient diffusion film (DGT) technology provided by the invention uses ENVI-CARB particles, MCX resin particles and HLB resin particles as the adsorption films prepared by the adsorption materials, so that various antiviral drugs in a water body can be effectively measured;
(2) The invention provides a method for measuring antiviral drugs in water, which adopts a DGT device for sampling, and compared with the existing active sampling method, the method can greatly reduce the labor intensity of sampling work and can provide more environmentally-meaningful time average concentration.
(3) According to the method for measuring the antiviral drugs in the water body, the ENVI-CARB and the MCX+HLB adsorption films can respectively correspond to different antiviral drugs, have strong adsorption capacity and larger adsorption capacity, and the adsorption capacities of the two adsorption films are 232.9 mug/tablet and 230.5 mug/tablet respectively through the inventor test.
Drawings
FIG. 1 is a schematic diagram of a DGT apparatus according to an embodiment of the present invention;
FIG. 2 shows the relationship between the mass of antiviral drug adsorbed by MCX+HLB-DGT and the time of placement (solid line is theoretical line) and the relationship between the mass of antiviral drug adsorbed by ENVI-CARB-DGT and the time of placement (solid line is theoretical line) by using a DGT device according to the embodiment of the present invention;
FIG. 3 is a graph showing the adsorption effect of antiviral drugs at different pH using the DGT apparatus according to the embodiment of the present invention;
FIG. 4 is a graph showing the adsorption effect of antiviral drugs at different pH using the DGT apparatus according to the embodiment of the present invention;
FIG. 5 is a graph showing the effect of adsorption of antiviral drugs at different ion concentrations using the DGT apparatus according to the embodiment of the present invention;
FIG. 6 adsorption ratio of MCX, MCX+HLB, ENVI-CARB, HLB and WCX adsorption films against viral drugs in comparative example 1;
FIG. 7 is a graph showing the adsorption ratio of antiviral drugs on a DGT apparatus, two different diffusion gums, and three different filters in comparative example 2;
FIG. 8 shows the bending angle of the MCX+HLB adsorption film
In the figure: 1. a base; 2. an adsorption film; 3. a diffusion film; 4. a filter membrane; 5. a cover with a sampling window; alpha, bending angle.
Detailed Description
The present disclosure may be understood more readily by reference to the following description taken in conjunction with the accompanying drawings and examples, all of which form a part of this disclosure. It is to be understood that this disclosure is not limited to the particular products, methods, conditions, or parameters described and/or shown herein. Further, the terminology used herein is for the purpose of describing particular embodiments by way of example only and is not intended to be limiting unless otherwise indicated.
It is also to be appreciated that certain features of the disclosure may, for clarity, be described herein in the context of separate embodiments, but may also be provided in combination with each other in a single embodiment. That is, each separate embodiment is contemplated to be combinable with any other embodiment, and to be considered as representing a different embodiment, unless expressly incompatible or specifically excluded. Conversely, various features of the disclosure that are, for brevity, described in the context of a single embodiment, may also be provided separately or in any subcombination. Finally, although a particular embodiment may be described as part of a series of steps or as part of a more general structure, each step or sub-structure itself may also be considered a separate embodiment.
Unless otherwise indicated, it should be understood that each individual element in the list and each combination of individual elements in the list are to be construed as different embodiments. For example, a list of embodiments denoted as "A, B or C" should be construed to include embodiments "a", "B", "C", "a or B", "a or C", "B or C" or "A, B or C".
In this disclosure, the singular forms "a," "an," and "the" also include the corresponding plural referents, and reference to a particular value includes at least the particular value unless the context clearly dictates otherwise. Thus, for example, reference to "a substance" is a reference to at least one of such a substance and equivalents thereof.
Terms including ordinal numbers such as "first" and "second" may be used to explain various components or fluids, but the components, fluids are not limited by these terms. Accordingly, these terms are merely used to distinguish one component/fluid from another component/fluid without departing from the teachings of the present disclosure.
When items are described using the conjunctive terms "… … and/or … …" and the like, the description should be understood to include any one of the associated listed items, and all combinations of one or more of the same.
In general, the use of the term "about" refers to an approximation that may vary depending on the desired properties obtained by the disclosed subject matter, and will be interpreted in a context-dependent manner based on the function. Thus, one of ordinary skill in the art will be able to interpret a degree of variability on an individual case basis. In some cases, the number of significant digits used in expressing a particular value can be a representative technique for determining the variance allowed by the term "about. In other cases, a gradient in a series of values may be used to determine the range of differences permitted by the term "about". Further, all ranges in this disclosure are inclusive and combinable, and reference to a value recited in a range includes each value within the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the term and/or any and all combinations including one or more of the associated listed items.
As described herein:
MCX: refers to a mixed cation exchange resin;
mcx+hlb; refers to a mixed cation exchange-hydrophilic lipophilic balance mixed resin;
ENVI-CARB; refers to graphitized carbon black;
HLB; refers to a hydrophilic lipophilic balance resin;
WCX: refers to weak cation exchange resins.
The present invention is further illustrated below with reference to specific examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art. The essential features and significant effects of the invention can be seen from the following examples, which are described as some, but not all, of which, therefore, are not limiting of the invention, and some of the insubstantial modifications and adaptations of the invention by those skilled in the art are within the scope of the invention.
The DGT device used in the following embodiments is specifically as follows:
as shown in fig. 1, the DGT device is assembled from a base 1, an adsorption membrane 2, a diffusion membrane 3, a filter membrane 4, and a cover 5 with a sampling window in this order. Wherein the base and the cover of the DGT apparatus are made of acrylonitrile-butadiene-styrene copolymer.
As the adsorption film 2, an agarose film is used as a matrix, adsorption materials are distributed in the agarose film, and the particle size of the adsorption materials is not more than 60 mu m; wherein the adsorption material comprises any one or two of graphitized carbon black particles, MCX resin particles and HLB resin particles.
For example, one specific form of the adsorption film has an agarose film as a matrix, in which graphitized carbon black particles having a particle diameter of not more than 60 μm are distributed;
the adsorption film in another specific form takes an agarose film as a matrix, MCX resin particles and HLB resin particles are distributed in the agarose film, and the mass ratio of the MCX to the HLB is 3:1; the particle size of the particles is not more than 60 μm. In particular, the adsorption film of this type has a bending angle of not less than 60 ° when bent at least in one direction, preferably, a bending angle of approximately 90 °.
The adsorption film 2 can be prepared by the following method:
(1) Soaking ENVI-CARB, MCX and HLB in methanol, and cleaning with ultrapure water for later use, wherein the preparation method comprises the following steps:
methanol cleaning: respectively adding ENVI-CARB, MCX, HLB into methanol solvent, shaking and ultrasonic treating to completely soak, soaking, centrifuging, and removing supernatant to obtain sediment solid; the volume-mass ratio of the methanol solvent to ENVI-CARB, MCX or HLB is 8:5mL/g;
cleaning with ultrapure water: adding pure water into the deposited solid, oscillating, centrifuging, removing supernatant, and repeating for three times;
(2) Mixing agar powder, prepared ENVI-CARB, MCX+HLB and pure water according to a certain mass ratio, shaking uniformly, and heating to boil to form a uniform suspension;
(3) Injecting the prepared agar suspension into a gap between two glass plates with a U-shaped Teflon sheet, extruding bubbles between the glass plates, horizontally placing the glass plates, cooling at room temperature for 50-80 min, and solidifying the solution in the glass plates to form an adsorption film.
As the diffusion membrane 3, an agarose membrane is selected;
as the filter membrane 4, a track etching membrane is selected;
the antiviral drugs are measured by using the DGT device, and the steps can be referred to as follows:
(1) Assembly of the DGT device: sequentially superposing an adsorption film, a diffusion film and a filter film between a base of the DGT device and a cover with a window to assemble the DGT device;
(2) Placement of the DGT device: placing the DGT device in the step (1) into a water body to be detected to adsorb antiviral drugs;
(3) Recovery and elution of the adsorption membranes: taking out the DGT device from the water body to be detected, washing the device by pure water, taking out the adsorption film, placing the adsorption film in a glass bottle, and adding an eluent to obtain an eluent;
(4) Determination of antiviral drug: measuring the concentration of the antiviral drug in the eluent obtained in the step (3) by adopting a high performance liquid chromatography-secondary mass spectrometry method;
(5) Calculation of antiviral drug adsorption: the adsorption amount of the antiviral drug on the adsorption film was calculated according to the following formula (I)
M＝C e (V g +V e )/f e (I)
Wherein M is the adsorption quantity of the antiviral drug on the adsorption film, and the unit is ng; c (C) e The unit is ng/mL for the mass concentration of the antiviral drug in the eluent; v (V) g Is the volume of the adsorption film, and the unit is mL; v (V) e Is the volume of the eluent, and the unit is mL; f (f) e Is the elution efficiency of the antiviral drug, obtained by eluting an adsorption film of known adsorption amount of the antiviral drug;
according to the Fick's first diffusion law, the DGT concentration is converted by the following formula (II) to calculate the concentration of antiviral drugs in water,
C DGT ＝M*Δ g /(D*A*t)(II)
wherein C is DGT Is the concentration of antiviral drugs in water body, the unit is ng/mL; delta g Is the sum of the thicknesses of the diffusion film and the filter film, and the unit is cm; d is the diffusion coefficient of the antiviral drug in the impurity filtering membrane and the diffusion membrane, and the unit is cm 2 S; a is the window area of the DGT apparatus in cm 2 The method comprises the steps of carrying out a first treatment on the surface of the t is the placement time of the DGT apparatus in s.
As the "desorbing agent", a specific form of the mixed solution of 0.2% (volume ratio) of formic acid aqueous solution and chromatographic pure acetonitrile is that the ratio of the formic acid aqueous solution to the chromatographic pure acetonitrile is 4:6, preparing a base material; if the adsorption membrane is an ENVI-CARB adsorption membrane, the desorbent is recommended to be selected;
as the desorption agent, another specific form is 20 percent (volume ratio) of ammonia acetonitrile solution; if the adsorbent membrane is an MCX-HLB adsorbent membrane, then it is recommended to select this desorbent.
The invention is further described below in connection with specific embodiments.
Example 1
In the DGT device of the embodiment, the selected diffusion membrane 3 is an agarose membrane;
the filter membrane 4 is a track etched membrane (hydrophilic, diameter 25mm, pore size 0.45 μm, whatman);
there are two types of adsorption membranes 2:
the first kind adopts ENVI-CARB adsorption film; wherein the grain size of ENVI-CARB is 60 μm, agar powder, adsorbing material (wet weight) and pure water are prepared to form agar solution in the ratio of 1:8:50, the prepared agar solution is injected into the gap between two glass plates with U-shaped Teflon material sheets sandwiched therebetween, air bubbles are extruded between the glass plates, the glass plates are horizontally placed and cooled for 80min at room temperature, and the solution in the glass plates is solidified to form an adsorbing film.
With such an adsorption membrane, the subsequent eluent composition was as follows, 0.2% aqueous formic acid-acetonitrile solution 4:6.
the second one adopts MCX+HLB adsorption film; wherein the mass ratio of MCX to HLB is 4:6, preparing a base material; the MCX+HLB particle size is 60 mu m, agar powder, an adsorption material (wet weight) and pure water are prepared to form an agar solution in the ratio of 1:7:50, the prepared agar solution is injected into a gap between two glass plates with a U-shaped Teflon sheet sandwiched therebetween, bubbles are extruded between the glass plates, the glass plates are horizontally placed and cooled at room temperature for 60min, and the solution in the glass plates is solidified to form an adsorption film.
With such an adsorption membrane, the subsequent eluent composition is as follows, 20% aqueous ammonia acetonitrile solution.
The specific procedure for activation of ENVI-CARB or MCX+HLB resins using methanol is as follows:
1) Activation of methanol: adding 50g of ENVI-CARB, MCX or HLB resin into 70mL of methanol solvent, soaking for 30min, centrifuging at 7200r/min for 5min, and removing supernatant to obtain sediment solid;
2) Cleaning with ultrapure water: adding pure water into the deposited solid, carrying out oscillation treatment, centrifuging at a rotating speed of 7200r/min for 5min, removing supernatant, and washing with ultrapure water for three times to obtain activated ENVI-CARB, MCX or HLB resin;
3) And (3) preserving: adding ultrapure water again into the activated resin, wherein the adding amount is that the liquid level exceeds the resin, storing, pouring the supernatant when taking, and directly weighing the rest sediment (namely the activated resin), wherein the state is wet weight.
The specific detection steps are as follows:
(1) Placement of the DGT device: the DGT device is placed into fully stirred water containing the antiviral drug to be tested for 3-168 hours, wherein the concentration of the antiviral drug clamped in the water to be tested is 20 mug/L.
(2) Recovery and elution of resin adsorption membranes: and taking out the DGT device from the water body to be detected, flushing dirt on the surface of the device by using pure water, taking out the ENVI-CARB or MCX+HLB resin adsorption film, placing the film in a glass bottle, adding an eluent (the eluent of the ENVI-CARB adsorption film is 0.2% formic acid-acetonitrile solution 4:6, and the eluent of the MCX-HLB adsorption film is 20% ammonia water acetonitrile solution), and performing ultrasonic treatment for 30min to obtain the eluent.
(3) Determination of antiviral drug: and (3) measuring the concentration of the antiviral drug in the eluent obtained in the step (3) by adopting a high performance liquid chromatography-secondary mass spectrometry method.
(4) Calculation of antiviral drug adsorption: the adsorption amount of the antiviral drug on the resin adsorption film was calculated according to the following formula (I)
M＝C e (V g +V e )/f e (I)
Wherein M is the adsorption quantity of the antiviral drug on the resin adsorption film, and the unit is ng; c (C) e The unit is ng/mL for the mass concentration of the antiviral drug in the eluent; v (V) g Is the volume of the resin adsorption film, and the unit is mL; v (V) e Is the volume of the eluent, and the unit is mL; f (f) e Is the elution efficiency of the antiviral drug, and the adsorption amount of the antiviral drug is known by eluting the resin adsorption filmTo obtain;
according to the Fick's first diffusion law, the DGT concentration is converted by the following formula (II) to calculate the concentration of antiviral substances in water,
C DGT ＝M*Δ g /(D*A*t)(II)
wherein C is DGT Is the concentration of antiviral drugs in water body, the unit is ng/mL; delta g Is the sum of the thicknesses of the diffusion film and the filter film, and the unit is cm; d is the diffusion coefficient of the antiviral drug in the diffusion membrane in cm 2 S; a is the window area of the DGT apparatus in cm 2 The method comprises the steps of carrying out a first treatment on the surface of the t is the placement time of the DGT apparatus in s.
In this example, the diffusion coefficients of the above-mentioned various antiviral substances measured at a measurement temperature of 25℃are shown in Table 1.
TABLE 1 diffusion coefficient of various antiviral drugs
Window area a:3.14cm 2 ；
The antiviral drug is measured within a measurement time t of 3 to 168 hours.
Calculating the measured concentration (C) of each antiviral drug measured according to the above formula DGT ) The ratio of the total concentration to the actual concentration (20 mug/L) is in the range of 0.9-1.1, thereby meeting the DGT measurement requirement. As shown in FIG. 2, the mass of the antiviral drugs enriched on the DGT adsorption membrane can be well matched with the mass calculated by the DGT theoretical formula. It is shown that DGT can well determine the concentration of antiviral drugs in water when left for a long period of time.
Example 2
In the embodiment, under the condition of detecting different pH values, the influence of the antiviral drugs in the water body is measured by using a DGT technology, wherein the concentration of the antiviral drugs in the water body to be detected is 20 mug/L, and the pH values of the water solution to be detected are respectively: 3.16, 5.57, 7.23, 8.41 and 9.74.
As shown in FIGS. 3 and 4, for the DGT of ENVI-CARB as the adsorption film, the DGT is calculated according to the formulaConcentration of most antiviral drug C DGT And actually measuring antiviral drug C in solution solu The ratio of (2) is between 0.9 and 1.1, which shows that the pH of the water body has no obvious influence on the measurement of most DGT. While such an adsorption membrane is not suitable as an adsorption membrane for SOF, SOP, 3TC and OTV. And DGT using MCX+HLB as the adsorption film, measurement value C for SOF, SOP, 3TC and OTV DGT C with the concentration in the actual measurement solution solu The ratio of (2) is between 0.9 and 1.1, which indicates that the MCX+HLB adsorption film can fill the deficiency of the ENVI-CARB adsorption film.
Example 3
In this embodiment, under the condition of detecting different ion concentrations, the influence of antiviral drugs in water is determined by using a DGT technology, in this embodiment, the antiviral drugs in water are determined by using a DGT device, the DGT device is placed in fully stirred water containing the antiviral drugs to be detected, the placement time is 24 hours, the antiviral concentration in the water to be detected is 20 mug/L, and the ion concentration (calculated by NaCl) of the aqueous solution to be detected is respectively: 0.1, 1, 10, 100, 500mmol/L.
As shown in FIG. 5, for DGT with ENVI-CARB as the adsorption film, the antiviral drug concentration C is calculated according to the formula DGT And actually measuring the concentration C of the antiviral drug in the solution solu Most of the ratios between 0.9 and 1.1, which shows that the ionic strength of the water bodies of the substances has no obvious influence on the measurement of DGT. But for RBV, FTC and 3TC are not applicable in water with ionic strength exceeding 100mmol/L, and for SOP, ENVI-CARB is not applicable. The deficiency of ENVI-CARB in SOP measurement can be overcome by using MCX+HLB as the DGT of the adsorption film. However, for FTC and 3TC, the ionic strength still cannot exceed 100mmol/L.
Comparative example 1
The purpose of this comparative example was to compare the adsorption capacity of several adsorption membranes against viral drugs. The adsorption films are respectively as follows:
MCX adsorption membrane, mcx+hlb adsorption membrane, ENVI-CARB adsorption membrane, HLB adsorption membrane, WCX adsorption membrane.
And (3) putting the adsorption membranes into an antiviral drug solution containing 20ng/mL, vibrating for 24 hours, taking out, and eluting to obtain the antiviral drug in the eluent.
As can be seen from fig. 6, the MCX adsorption membrane, mcx+hlb adsorption membrane, and ENVI-CARB adsorption membrane have strong adsorption capacity for most antiviral drugs. However, the MCX adsorption film has higher brittleness, is easy to break when being arranged in a water body for a long time, and the adsorption effect of the mcx+hlb adsorption film is identical with that of the MCX adsorption film, but the flexibility of the MCX adsorption film is far higher than that of the MCX adsorption film, so that the MCX adsorption film is more suitable for field arrangement. First kind: an agarose film is used as a matrix, and activated XAD18 resin is distributed in the agarose film.
Further tests show that the bending angle of the MCX adsorption film can reach 60 degrees at most, and if the bending angle is continuously increased, the MCX adsorption film is broken; whereas the bending angle of the mcx+hlb adsorption film can reach 80 ° without breaking, the description of the bending angle is shown in fig. 8.
Comparative example 2
Firstly, it should be pointed out that the filter membrane and the diffusion membrane are also important components in the DGT device, when the DGT technology is used for measuring the antiviral drugs in the water body, not only an appropriate adsorption membrane is needed, but also an appropriate filter membrane is needed, the adsorption quantity of the filter membrane to the target object is required to be as small as possible, so that the diffusion of the target object to the resin adsorption membrane is not affected, the adsorption capacities of different organic matters on different filter membranes are different, and therefore, the appropriate filter membrane is needed to be selected for the target substance before the method is developed, so that the adsorption or interception of the target object to be detected is reduced, and the measurement error is caused.
The comparative example selects three filter membranes and two diffusion membranes, and the adsorption performance of the antiviral drugs on the filter membranes and the diffusion membranes is detected, and the specific steps are as follows:
(1) Three kinds of filter membranes, as shown in FIG. 7, namely, a Nuclecore track etching membrane (PC), a polyethersulfone membrane (PES) and a polytetrafluoroethylene membrane (PTFE), were selected, and the new membrane was immersed in ultrapure water containing 0.01M NaCl for one day. Two diffusion membranes were selected, agarose diffusion membrane (AGE) and acrylamide diffusion membrane (APA), respectively.
(2) Three filters and two diffusion filters were placed in 10mL triangular flasks containing 20. Mu.g/L of the target antiviral drug, respectively, and shaken at 25℃for 24 hours.
(3) And taking 200 mu/L of water sample from the triangular flask before and after the membrane is put in, and measuring the concentration of a target object in the water sample.
(4) The percentage of adsorption of the target substance by the membrane was calculated using the following formula:
Adsorption％＝(C a -C b )/Ca×100％
wherein C is a Is the original target concentration in the conical flask, C b Is the concentration of the target in the erlenmeyer flask after removal of the membrane.
Meanwhile, as a component of the DGT, the DGT housing is also tested synchronously.
As shown in FIG. 6, the inventor has obtained through professional theoretical analysis and repeated experiments that only PC membrane has minimum adsorption to target, and the filter membrane made of polyethersulfone or polytetrafluoroethylene can adsorb antiviral drugs in large quantity, so that the substances cannot form diffusion gradient in the filter membrane and the diffusion membrane and are further captured by the resin adsorption membrane, and the adsorption of the antiviral drugs by the agarose membrane is less than that of the acrylamide membrane. In addition, DGT shells have very little adsorption of antiviral drugs. Therefore, when the antiviral drugs in the water body are measured, the PC membrane is selected as a filter membrane of the DGT device, and the agarose membrane is selected as a diffusion membrane of the DGT device.
Claims (10)
1. An adsorption film of antiviral drugs, which is characterized in that,
the adsorption film takes an agarose film as a matrix, adsorption materials are distributed in the agarose film, and the particle size of the adsorption materials is not more than 60 mu m;
wherein,,
the adsorption material comprises any one or two of graphitized carbon black particles, MCX resin particles and HLB resin particles;
the adsorption film has a bending angle of not less than 60 °, preferably, a bending angle of approximately 90 °, when bent at least in one direction.
2. The adsorption film of antiviral drug as in claim 1, wherein,
the adsorption film takes an agarose film as a matrix, graphitized carbon black particles are distributed in the agarose film, and the particle size of the particles is not more than 60 mu m;
or,
the adsorption film takes an agarose film as a matrix, MCX resin particles and HLB resin particles are distributed in the agarose film, and the particle size of the particles is not more than 60 mu m.
3. The adsorption film of antiviral drug as in claim 1, wherein,
the adsorption film is formed by solidifying agar solution;
the agar solution is prepared by mixing agar powder, an adsorbing material and pure water according to a mass ratio of 1 (7-13): 50, and heating to boil.
4. An adsorption film for antiviral drugs according to any one of claims 1 to 3, characterized in that,
the following treatments are needed before the adsorption material is used:
methanol cleaning, namely soaking and cleaning the adsorption material by using methanol; wherein the volume mass ratio of the methanol to the adsorption material is (8-10) 5mL/g;
cleaning with ultrapure water: and cleaning the adsorption material by using ultrapure water.
5. An adsorption film for antiviral drugs according to any one of claims 1 to 3, characterized in that,
the adsorption film has a particle size of not less than 73.41. Mu.g/cm 2 Is used as a catalyst.
6. An antiviral drug measuring device is characterized in that,
the device is a DGT device;
the DGT device comprises an adsorption film, a diffusion film and a filter film which are sequentially overlapped;
the adsorption film according to any one of claims 1 to 3 is selected.
7. The antiviral drug testing device of claim 6, wherein,
the diffusion membrane is an agarose membrane;
the filter membrane is a track etched membrane.
8. A method for measuring antiviral drugs is characterized in that,
(1) The DGT device is placed in a water body to be detected to adsorb antiviral drugs;
(2) Taking out the DGT device from the water body to be detected, taking out the adsorption film, and eluting by using an eluent to obtain an eluent;
(3) And determining the concentration of the antiviral drugs in the eluent by adopting a high performance liquid chromatography-secondary mass spectrometry method.
9. The method for measuring an antiviral drug as claimed in claim 8, wherein,
the eluent is a mixed solution containing formic acid and acetonitrile; or,
the eluent is a mixed solution containing ammonia water and acetonitrile.
10. The method for measuring an antiviral drug as claimed in claim 8, wherein,
the concentration of the antiviral drugs in the water body to be measured is 0.01-500 mg/L.
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