CN110501203B - On-site rapid enrichment and purification device and method for mental active substances in water environment - Google Patents
On-site rapid enrichment and purification device and method for mental active substances in water environment Download PDFInfo
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- CN110501203B CN110501203B CN201910716621.2A CN201910716621A CN110501203B CN 110501203 B CN110501203 B CN 110501203B CN 201910716621 A CN201910716621 A CN 201910716621A CN 110501203 B CN110501203 B CN 110501203B
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Classifications
-
- 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
-
- 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
Abstract
The invention provides a device and a method for on-site rapid enrichment and purification of mental active substances in water environment, wherein the device comprises a liquid storage bottle, a leaching solution bottle, a first activation solution bottle, a first liquid injection pump, an enrichment disc, an adsorption trap, a sample bottle, a second liquid injection pump, a waste liquid bottle and an elution device; the outlet of the liquid storage bottle and the outlet of the first liquid injection pump are respectively connected with an inlet pipeline of the enrichment disc; the leaching liquid bottles and the first activating liquid bottles are connected with an inlet pipeline of the first liquid injection pump; the outlet of the enrichment disc and the outlet of the second liquid injection pump are respectively connected with an inlet pipeline of the adsorption trap, and the sample bottle and the waste liquid bottle are respectively connected with an outlet pipeline of the adsorption trap; the elution device is connected to an inlet conduit of a second liquid injection pump. The device has the advantages of simple structure, reasonable design, high speed, low energy consumption and simple operation, and can be used for carrying out pretreatment on samples under field conditions.
Description
Technical Field
The invention relates to a device and a method for on-site rapid enrichment and purification of mental active substances in water environment.
Background
Psychoactive substances refer to substances which can significantly affect human mental activities and can cause addiction after being inhaled from outside the human body, and mainly comprise CNS inhibitors, stimulants, cannabis, hallucinogens, opioids and the like. Most of the psychoactive substances belong to national regulatory drugs, and are illegally abused, namely 'drugs'. Currently, the widespread abuse of psychoactive substances has become an increasing global concern. Meanwhile, due to ingestion abuse, psychoactive substances and metabolites thereof enter the environmental water body, and great ecological environment and crowd health risks are brought.
Due to social problems and environmental problems caused by abuse of psychoactive substances, quantitative analysis and detection are carried out on the psychoactive substances, and the evaluation of the abuse and the corresponding environmental risk evaluation is of great significance. In recent years, a new approach, sewage epidemiology, has been widely used to assess and monitor psychoactive substance abuse. The U.S. environmental protection agency's Daugton doctor in 2001 first Proposed the concept of epidemiology of sewage, namely, the average human consumption of a drug or its metabolite was calculated by measuring the content of the drug in sewage in a certain area (Daugton C G. Illicit drugs in municipal sewage: proposed new non-intrusive tool to heighten public awareness of societal use of illicit/abused drugs and their potential for ecological sequences 2001:348-364.). Professor Zuccano, italy et al, in 2005 detected the psychoactive substance cocaine in surface water for the first time (Zuccano E, chiabrando C, castiglini S, et al Cocaine in surface waters: a new evaluation-based tool to monitor community drug use Environmental Health, 2005, 4 (1): 1-7.). Thereafter, there is an increasing research on assessing abuse of psychoactive substances by detecting them in an aqueous environment, and the method for studying and evaluating abuse of psychoactive substances by environmental detection has the advantages of objectivity, high efficiency, quantification and the like.
At present, the technical methods for detecting the mental active substances in the water environment at home and abroad are field sampling, laboratory processing and instrument analysis. The method has some defects, firstly, the sample collection and transportation process needs to occupy quite large manpower and material resources, and the cost is higher; secondly, when the field sampling points are more and the distance from the laboratory is long, a large amount of samples cannot be immediately transported back to the laboratory, and analysis has hysteresis; thirdly, the field does not have the conditions of sample storage such as freezing, acidification and the like, and the incorrect sample storage can cause great influence on experimental results. Therefore, from methodology, there is an urgent need for a technique that can rapidly pre-process samples in the field, purify and enrich the samples and preserve them.
Disclosure of Invention
The invention aims to provide a device for rapidly enriching and purifying mental active substances in water environment on site, which has the advantages of simple structure, reasonable design, rapid speed, low energy consumption and simple operation, and can be used for carrying out pretreatment on samples under field conditions.
The invention is realized in the following way:
the on-site rapid enrichment and purification device for the mental active substances in the water environment comprises a liquid storage bottle, a leaching solution bottle, a first activation solution bottle, a first liquid injection pump, an enrichment disc, an adsorption trap, a sample bottle, a second liquid injection pump, a waste liquid bottle and an elution device; the outlet of the liquid storage bottle and the outlet of the first liquid injection pump are respectively connected with an inlet pipeline of the enrichment disc; the leaching liquid bottles and the first activating liquid bottles are connected with an inlet pipeline of the first liquid injection pump; the outlet of the enrichment disc and the outlet of the second liquid injection pump are respectively connected with an inlet pipeline of the adsorption trap, and the sample bottle and the waste liquid bottle are respectively connected with an outlet pipeline of the adsorption trap; the elution device is connected to an inlet conduit of a second liquid injection pump.
Specifically, the eluting device comprises two eluting solution bottles which are respectively connected with an inlet pipeline of the second liquid injection pump, wherein one eluting solution bottle is a water/methanol eluting bottle, and the other eluting solution bottle is a normal hexane eluting bottle; the volume ratio of the mixing proportion in the water/methanol elution bottle is that: methanol=2:3.
Specifically, the device also comprises a second activation liquid bottle connected with the inlet pipeline of the second liquid injection pump.
Specifically, a filter head is arranged at the outlet of the liquid storage bottle and is connected with an inlet pipeline of the enrichment disc through the filter head; and a plurality of layers of acetate fibers or glass fiber filter membranes with the aperture of 0.45 mu m and the diameter of 5cm are arranged in the filter head.
More specifically, the liquid storage bottle is provided with an air pump for compressing air into the liquid storage bottle.
Further, the system also comprises a control system, wherein the control system comprises a controller, a first valve arranged at an outlet of the leaching solution bottle, a second valve arranged at an outlet of the first activation solution bottle, a third valve arranged at an inlet of the sample bottle, a fourth valve arranged at an inlet of the waste liquid bottle, a fifth valve arranged at an outlet of the water/methanol eluting bottle, a sixth valve arranged at an outlet of the n-hexane eluting bottle and a seventh valve arranged at an outlet of the second activation solution bottle; the first to seventh valves are connected with the controller.
As a preferable scheme, the liquid storage bottle is a borosilicate glass bottle and is used for storing the stock solution to be treated; the eluting liquid bottle is a borosilicate glass bottle and is used for storing eluting liquid acetone of the enrichment disc; the first activation liquid bottle is a high-density polyethylene bottle and is used for storing activation liquid deionized water of the enrichment disc; the waste liquid bottle is a polyethylene bottle; the sample bottle is a brown glass bottle; the enrichment disc is a polytetrafluoroethylene disc, and a special solid polymer adsorbent corresponding to the mental active substance to be detected is contained in the enrichment disc; the adsorption trap is a polytetrafluoroethylene trap, and a special selective adsorbent is contained in the adsorption trap to adsorb only corresponding target substances.
As another preferable scheme, the first activation liquid bottle is also connected with a second liquid injection pump pipeline through a second valve.
The invention also aims to provide a method for carrying out on-site rapid enrichment and purification on the mental active substances in the water environment by utilizing the device, which is simple to operate, good in pretreatment quality and high in efficiency, and is suitable for rapid enrichment and purification of various mental active substances.
Specifically, the method for rapid enrichment and purification comprises the following steps:
(1) Activation equilibration of enrichment discs: opening a second valve, a first liquid injection pump and a fourth valve, injecting the first activating liquid into the enrichment disc three times, wherein 10ml of the first activating liquid is respectively injected into the enrichment disc every time, the interval is 1-3 s, and closing the second valve and the first liquid injection pump after the completion of the injection;
(2) Activating the adsorption trap: starting a seventh valve and a second liquid injection pump, injecting 5ml of second activating liquid into the adsorption trap for 1 time, then closing the seventh valve, starting the second valve, and injecting the first activating liquid into the adsorption trap for 2 times, wherein 10ml of second activating liquid are respectively injected into the adsorption trap each time; closing the second valve, the fourth valve and the second liquid injection pump after completion;
(3) Sample loading: starting an air pump, starting to operate, loading a water sample after 50 seconds, continuously operating the air pump, and closing the air pump after the water sample is loaded;
(4) Leaching: starting a first valve, a fourth valve and a first liquid injection pump, injecting eluent into the enrichment disc, leaching for 2 times, wherein 10mL of eluent enters an adsorption trap each time;
(5) Purifying by an adsorption trap: the leacheate in the enrichment plate enters an adsorption trap, target substances are reserved on an adsorption material in the adsorption trap, and non-target substances enter a waste liquid bottle;
(6) Eluting: closing the first valve, the fourth valve and the first liquid injection pump, and opening the third valve, the fifth valve and the second liquid injection pump to inject water/methanol eluent into the adsorption trap for 1 time and 5ml; closing a fifth valve, opening a sixth valve, and injecting n-hexane into the adsorption trap for 1 time and 3ml; the eluate was collected in whole into a sample bottle.
In the step (3), the water sample is injected into the enrichment disc at a speed of 20ml/min.
The beneficial effects of the invention are as follows:
(1) The device has the advantages of simple structure, reasonable design, common main parts, direct assembly and low cost. The device can be used for carrying out rapid pretreatment on the sample in the field, and the sample is purified and enriched and then stored.
(2) The device provided by the invention is used for rapidly enriching and purifying the mental active substances in the water sample under the field condition, so that the requirements on the conditions of sample storage and transportation can be reduced, the influence of the links of sample storage and transportation on experimental detection results can be reduced, and the sampling and detection efficiency can be integrally improved.
The device of the invention carries out pretreatment of the sample under the field condition, has high speed, low energy consumption, simple and convenient operation, and the pretreatment has good quality and high efficiency. Can be used for pretreatment of various psychoactive substances such as methamphetamine, amphetamine, ephedrine and the like.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the structure of the enrichment and purification device of the present invention;
FIG. 2 is a measurement of the concentration of methamphetamine in example 1;
FIG. 3 is a measurement of the concentration of methamphetamine at two inlets (1 and 2) of the sewage plant of example 2.
Icon:
1-liquid storage bottle, 2-leacheate bottle, 3-first activating liquid bottle, 4-first liquid injection pump, 5-enriching tray, 6-adsorption trap, 7-sample bottle, 8-second liquid injection pump, 9-waste liquid bottle, 10-water/methanol eluting bottle, 11-normal hexane eluting bottle, 12-second activating liquid bottle, 13-filter head and 14-air pump.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
In the description of the present invention, it should be understood that the terms "orientation" or "positional relationship" are based on the orientation or positional relationship shown in the drawings, and are merely for convenience of description and to simplify the description, rather than to indicate or imply that the apparatus or elements referred to must have a particular orientation, be constructed and operate in a particular orientation, and therefore should not be construed as limiting the invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., are directions or positional relationships based on those shown in the drawings, or are directions or positional relationships conventionally put in use of the inventive product, are merely for convenience of describing the present invention and simplifying the description, and are not indicative or implying that the apparatus or element to be referred to must have a specific direction, be constructed and operated in a specific direction, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal," "vertical," "overhang," and the like do not denote a requirement that the component be absolutely horizontal or overhang, but rather may be slightly inclined. As "horizontal" merely means that its direction is more horizontal than "vertical", and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the present invention, unless expressly stated or limited otherwise, a first feature may include first and second features directly contacting each other, either above or below a second feature, or through additional features contacting each other, rather than directly contacting each other. Moreover, the first feature being above, over, and on the second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is higher in level than the second feature. The first feature being below, beneath, and beneath the second feature includes the first feature being directly below and obliquely below the second feature, or simply indicates that the first feature is less level than the second feature.
Examples:
the on-site rapid enrichment and purification device for the mental active substances in the water environment is simple in structure, convenient to operate, low in energy consumption, good in pretreatment quality and high in efficiency. Referring to fig. 1, the device comprises a liquid storage bottle 1, a leaching liquid bottle 2, a first activating liquid bottle 3, a first liquid injection pump 4, an enrichment disc 5, an adsorption trap 6, a sample bottle 7, a second liquid injection pump 8, a waste liquid bottle 9 and an elution device.
The liquid storage bottle 1 is made of 500mL borosilicate glass and is used for storing a water sample to be treated; the outlet of the liquid storage bottle 1 is provided with a filter head 13, and the liquid storage bottle 1 is connected with an inlet pipeline of the enrichment disc 5 through the filter head 13; the inside of the filter head 13 is provided with a plurality of layers of acetate fibers or glass fiber filter films with the aperture of 0.45 mu m and the diameter of 5cm, which are used for filtering water samples, and because the positions of the collected water samples are different, the impurity content in the water samples is different, and the water samples generally comprise regular impurities such as gravel, branches and leaves, and the like, so as to accelerate the filtration, the liquid storage bottle 1 is also provided with an air pump 14 used for compressing air into the liquid storage bottle 1.
The inlet of the first liquid injection pump 4 is provided with a tee joint, one end of the tee joint is communicated with the inlet of the liquid injection pump, the other two ends of the tee joint are respectively communicated with the leaching liquid bottle 2 and the first activation liquid bottle 3, and the outlet of the first liquid injection pump 4 is communicated with the inlet of the enrichment disc 5. The leaching solution bottle 2 is a 200mL borosilicate glass bottle and is used for storing leaching solution acetone of the enrichment disc 5; the first activation liquid bottle 3 is a 500mL high-density polyethylene bottle and is used for storing activation liquid deionized water of the enrichment disc 5; to prevent misinjection of liquid into the enrichment plate 5, a first valve and a second valve are therefore provided at the outlet of the rinse liquid bottle 2 and the first activation liquid bottle 3, respectively.
The enrichment disc 5 is a polytetrafluoroethylene disc, has the diameter of 10cm and the thickness of 1cm, and is internally provided with 0.8g of special solid polymer adsorbent, so as to enrich target substances.
The outlet of the enrichment disc 5 and the outlet of the second liquid injection pump 8 are respectively connected with the inlet pipeline of the adsorption trap 6, and the sample bottle 7 and the waste liquid bottle 9 are respectively connected with the outlet pipeline of the adsorption trap 6. Wherein, the adsorption trap 6 is made of polytetrafluoroethylene material, has the capacity of 25mL, is internally provided with 0.6g of special selective adsorbent, only adsorbs target substances, and non-target substances are not adsorbed and reserved for purifying the target substances; the waste liquid bottle is a 500mL polyethylene bottle and is used for collecting waste liquid; the sample bottle was a 10mL brown borosilicate glass bottle and the purified sample was collected. It should be noted here that the outlet of the enrichment plate can also be connected to the waste liquid bottle alone, without affecting the operation and the enrichment purification effect of the present application. In addition, the inlets of the waste liquid bottle 9 and the sample bottle 7 are respectively provided with a fourth valve and a third valve, so that errors in sample collection can be avoided.
The eluting device comprises two eluent bottles respectively connected with an inlet pipeline of the second liquid injection pump 8, wherein one eluent bottle is a water/methanol eluting bottle 10, the water/methanol eluting bottle 10 is made of 200mL borosilicate glass material and is used for storing a first-stage eluent water/methanol mixture of an adsorption trap, and the water is mixed in a ratio by volume: methanol=2:3; the other eluent bottle is a normal hexane eluent bottle 11, the normal hexane eluent bottle 11 is made of 200mL borosilicate glass material, and the second-stage eluent n-hexane of the adsorption trap is stored. The inlet of the second liquid injection pump 8 is also connected with a second valve and a second activation liquid bottle 12 on the first activation liquid bottle 3 through pipelines respectively, the second activation liquid bottle 12 is made of 200mL borosilicate glass, and the activation liquid ethyl acetate in the storage adsorption trap is stored. Wherein, the outlet of the second activating liquid bottle 12 is also provided with a seventh valve, the outlet of the water/methanol eluting bottle 10 is provided with a fifth valve, and the outlet of the n-hexane eluting bottle 11 is provided with a sixth valve.
In order to facilitate centralized control, the embodiment is specially provided with a 51 single-chip microcomputer as a controller, and the controller is electrically connected with all valves and connected with a background PC (personal computer) so as to facilitate operation. This technology is relatively mature and therefore will not be described here again, and the drawing of the valve is omitted from fig. 1.
The embodiment also provides a method for carrying out on-site rapid enrichment and purification on the mental active substances in the water environment by utilizing the device, and the method is simple to operate, good in pretreatment quality and high in efficiency, and is suitable for rapid enrichment and purification on the mental active substances such as methamphetamine, amphetamine and ephedrine.
Specifically, the method for rapid enrichment and purification comprises the following steps:
(1) Activation equilibration of enrichment discs: opening a second valve, a first liquid injection pump and a fourth valve, injecting the first activating liquid into the enrichment disc three times, wherein 10ml of the first activating liquid is respectively injected into the enrichment disc every time, the interval is 1-3 s, and closing the second valve and the first liquid injection pump after the completion of the injection;
(2) Activating the adsorption trap: starting a seventh valve and a second liquid injection pump, injecting 5ml of second activating liquid into the adsorption trap for 1 time, then closing the seventh valve, starting the second valve, and injecting the first activating liquid into the adsorption trap for 2 times, wherein 10ml of second activating liquid are respectively injected into the adsorption trap each time; closing the second valve, the fourth valve and the second liquid injection pump after completion;
(3) Sample loading: starting an air pump, starting to operate, loading a water sample after 50 seconds, continuously operating the air pump, and closing the air pump after the water sample is loaded; the air pump is started to ensure that the water sample is injected into the enrichment disc at a speed of 20 ml/min;
(4) Leaching: starting a first valve, a fourth valve and a first liquid injection pump, injecting eluent into the enrichment disc, leaching for 2 times, wherein 10mL of eluent enters an adsorption trap each time;
(5) Purifying by an adsorption trap: the leacheate in the enrichment plate enters an adsorption trap, target substances are reserved on an adsorption material in the adsorption trap, and non-target substances enter a waste liquid bottle;
(6) Eluting: closing the first valve, the fourth valve and the first liquid injection pump, and opening the third valve, the fifth valve and the second liquid injection pump to inject water/methanol eluent into the adsorption trap for 1 time and 5ml; closing a fifth valve, opening a sixth valve, and injecting n-hexane into the adsorption trap for 1 time and 3ml; the eluate was collected in whole into a sample bottle.
Of these, it should be noted that it is best to enrich and elute the water sample under neutral to alkaline conditions. Only because the pH values of surface water and sewage are in the range under most conditions, the water sample can be directly enriched on site without long-distance transportation and acid storage. Moreover, the sample flow rate is an important link to be considered in balance when optimizing pretreatment conditions in the processes of loading, leaching, eluting and the like of a water sample. Generally, recovery is high at lower sample flow rates, but pretreatment time is prolonged; on the other hand, when the sample flow rate is too high, the adsorption of the target substance tends to be insufficient, resulting in a low recovery rate. Therefore, it is necessary to consider the efficiency of solid phase extraction and the treatment time under field conditions in combination. Therefore, the inventor conducts experiments, and the experimental results show that when the flow rate is 20ml/min, the average recovery rate of methamphetamine, amphetamine and ephedrine is 90.0%, 74.1% and 57.2%, so that the requirement of the recovery rate of a target object is met, and the pretreatment time during large-volume loading is reasonably controlled, and therefore 20ml/min is selected as the loading flow rate.
In addition, by using the device of the invention and adopting the optimized method conditions, the processes of nitrogen blowing concentration, re-dissolution filtration and the like are saved, and the portable lithium battery is used for supplying power in the field by using the air pump and the liquid pump with low energy consumption, so that the rapid pretreatment of the water sample can be realized. The process of nitrogen blowing concentration, re-dissolution filtration and the like is saved, the air pump and the liquid pump with low energy consumption are used in the field, the portable lithium battery supplies power, the rapid pretreatment of a water sample can be realized, and the water sample is more energy-saving.
In order to make the device of this example more clear, the experiments of examples 1 and 2 are described below.
Example 1
An automatic sampler is adopted to collect a sewage sample in a river, and the sample is immediately pretreated by the device of the invention on site and then sent back to a laboratory for instrument detection. At the same time, the sample was processed and tested by conventional methods in accordance with the rapid return to the laboratory, and the results were shown in FIG. 2.
In fig. 2, the dark color column is a traditional method, the light color column is a rapid purification and enrichment method of the device, and the accuracy rate is up to 92.5%.
Example 2
An automatic sampler is adopted to collect a sewage sample at the inlet of a sewage treatment plant, the sample collection is immediately pretreated on site by the device of the invention, and then the sample is sent back to a laboratory for instrument detection. At the same time, the sample was processed and tested by conventional methods in accordance with the rapid return to the laboratory, and the results are shown in FIG. 3.
In fig. 3, the dark color column is a traditional method, the light color column is a rapid purification and enrichment method of the device, and the accuracy rate is 92%.
Therefore, the device is used for purifying and enriching the sample and then preserving the sample, has the advantages of high speed, low energy consumption and simple operation, and the accuracy rate of the pretreated sample can still reach 92% -92.5% or even higher, so that the device completely meets the requirements. In addition, the requirements on sample storage and transportation conditions can be reduced, the influence of sample storage and transportation links on experimental detection results is reduced, and the sampling and detection efficiency is improved as a whole.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. The method for carrying out on-site rapid enrichment and purification on mental active substances in water environment by utilizing an enrichment and purification device is characterized in that the enrichment and purification device comprises a liquid storage bottle (1), a leaching solution bottle (2), a first activation solution bottle (3), a first liquid injection pump (4), an enrichment disc (5), an adsorption trap (6), a sample bottle (7), a second liquid injection pump (8), a waste liquid bottle (9) and an elution device; the outlet of the liquid storage bottle (1) and the outlet of the first liquid injection pump (4) are respectively connected with an inlet pipeline of the enrichment disc (5); the leaching solution bottle (2) and the first activation solution bottle (3) are connected with an inlet pipeline of the first liquid injection pump (4); the outlet of the enrichment disc (5) and the outlet of the second liquid injection pump (8) are respectively connected with an inlet pipeline of the adsorption trap (6), and the sample bottle (7) and the waste liquid bottle (9) are respectively connected with an outlet pipeline of the adsorption trap (6); the elution device is connected with an inlet pipeline of a second liquid injection pump (8);
the eluting device comprises two eluting solution bottles which are respectively connected with an inlet pipeline of a second liquid injection pump (8), wherein one eluting solution bottle is a water/methanol eluting bottle (10), and the other eluting solution bottle is a normal hexane eluting bottle (11); the mixing proportion volume ratio in the water/methanol eluting bottle (10) is that: methanol=2:3;
the elution device further comprises a second activation liquid bottle (12) connected with an inlet pipeline of a second liquid injection pump (8);
an air pump (14) for compressing air into the liquid storage bottle (1) is arranged on the liquid storage bottle (1);
the system also comprises a control system, wherein the control system comprises a controller, a first valve arranged at the outlet of the leaching solution bottle (2), a second valve arranged at the outlet of the first activation solution bottle (3), a third valve arranged at the inlet of the sample bottle (7), a fourth valve arranged at the inlet of the waste liquid bottle (9), a fifth valve arranged at the outlet of the water/methanol elution bottle (10), a sixth valve arranged at the outlet of the n-hexane elution bottle (11) and a seventh valve arranged at the outlet of the second activation solution bottle (12); the first valve, the seventh valve and the controller are connected;
the liquid storage bottle (1) is a borosilicate glass bottle and is used for storing raw liquid to be treated; the leaching solution bottle (2) is a borosilicate glass bottle and is used for storing leaching solution acetone of the enrichment disc (5); the first activation liquid bottle (3) is a high-density polyethylene bottle and is used for storing activation liquid deionized water of the enrichment disc (5); the waste liquid bottle (9) is a polyethylene bottle; the sample bottle (7) is a brown glass bottle; the enrichment disc (5) is a polytetrafluoroethylene disc, and a special solid polymer adsorbent corresponding to the mental active substance to be detected is contained in the enrichment disc; the adsorption trap (6) is a polytetrafluoroethylene trap, and a special selective adsorbent is contained in the adsorption trap to adsorb only corresponding target substances;
the first activation liquid bottle (3) is also connected with a second liquid injection pump (8) through a second valve;
the method comprises the following steps:
(1) Activation equilibration of enrichment discs: opening a second valve, a first liquid injection pump and a fourth valve, injecting the first activating liquid into the enrichment disc three times, wherein 10mL of the first activating liquid is respectively filled into the enrichment disc every time, the interval is 1-3 s, and closing the second valve and the first liquid injection pump after the completion of the injection;
(2) Activating the adsorption trap: starting a seventh valve and a second liquid injection pump, injecting 5mL of second activating liquid into the adsorption trap for 1 time, then closing the seventh valve, starting the second valve, and injecting the first activating liquid into the adsorption trap for 2 times, wherein 10mL of second activating liquid are respectively injected into the adsorption trap each time; closing the second valve, the fourth valve and the second liquid injection pump after completion;
(3) Sample loading: starting an air pump, starting to operate, loading a water sample after 50 seconds, continuously operating the air pump, and closing the air pump after the water sample is loaded;
(4) Leaching: starting a first valve, a fourth valve and a first liquid injection pump, injecting eluent into the enrichment disc, leaching for 2 times, wherein 10mL of eluent enters an adsorption trap each time;
(5) Purifying by an adsorption trap: the leacheate in the enrichment plate enters an adsorption trap, target substances are reserved on an adsorption material in the adsorption trap, and non-target substances enter a waste liquid bottle;
(6) Eluting: closing the first valve, the fourth valve and the first liquid injection pump, and opening the third valve, the fifth valve and the second liquid injection pump, and injecting water/methanol eluent into the adsorption trap for 1 time and 5mL; closing a fifth valve, opening a sixth valve, and injecting n-hexane into the adsorption trap for 1 time and 3mL; the eluate was collected in whole into a sample bottle.
2. Method according to claim 1, characterized in that the outlet of the reservoir (1) is provided with a filter head (13) and is connected to the inlet pipe of the enrichment disc (5) by means of the filter head (13); and a plurality of layers of acetate fibers or glass fiber filter membranes with the aperture of 0.45 mu m and the diameter of 5cm are arranged in the filter head (13).
3. The method of claim 1, wherein in step (3), the water sample is injected into the enrichment disc at a rate of 20mL/min.
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| CN112964509B (en) * | 2021-03-17 | 2023-03-03 | 济南市环境研究院 | Natural water sample in-situ suction filtration and solid phase extraction integrated operation system and operation method thereof |
| CN113238065A (en) * | 2021-04-19 | 2021-08-10 | 吴志洪 | Full-automatic detection device and detection method for trace drugs in sewage |
| CN114324804A (en) * | 2021-12-30 | 2022-04-12 | 杭州谱育科技发展有限公司 | Tracing method for contraband in sewage |
| CN114324805A (en) * | 2021-12-30 | 2022-04-12 | 杭州谱育科技发展有限公司 | Online monitoring system and method for contraband in sewage |
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