CN111504741B - Method for detecting micro-plastics in fish body - Google Patents
Method for detecting micro-plastics in fish body Download PDFInfo
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- CN111504741B CN111504741B CN202010323218.6A CN202010323218A CN111504741B CN 111504741 B CN111504741 B CN 111504741B CN 202010323218 A CN202010323218 A CN 202010323218A CN 111504741 B CN111504741 B CN 111504741B
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Abstract
The invention provides a method for detecting micro-plastics in fish bodies, which belongs to the technical field of micro-plastic detection and analysis, wherein hydrogen peroxide and nitric acid are used in a superposition manner, so that the digestion effect on fish samples is good, the influence on the micro-plastics is avoided, and meanwhile, aiming at the phenomenon that part of fish has high fat content and is difficult to remove, a surfactant is combined with an ultrasonic means to degrade grease, so that the influence of the grease on the detection of the micro-plastics in the digestive tracts of the fish bodies is effectively reduced, the filtering speed is effectively increased, the detection environment is improved, and the method has good practical application value.
Description
Technical Field
The invention belongs to the technical field of micro-plastic detection and analysis, and particularly relates to a method for detecting micro-plastic in a fish body.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Plastics are widely used due to high stability, durability and corrosion resistance, and the use of a large amount of plastics causes increasingly serious pollution to the environment, wherein the most prominent is that plastic products can be changed into plastic particles, namely micro plastics, with smaller and smaller particles through certain physical, chemical, biological and other actions after being discarded. However, the plastic particles are not degraded by the natural environment but remain in the environment, and according to the current research, the sea is the sink of micro-plastics, and a large amount of micro-plastics are finally gathered into the sea. The micro-plastic with small size is easily swallowed by marine organisms and is transmitted through a food chain, so that the ecological environment is adversely affected. However, to clarify the environmental problem of the micro-plastics, it is an important step to accurately obtain the content and distribution characteristics of the micro-plastics in the organism. The current research mainly focuses on the detection of micro-plastics in the digestive tract of a fish body, and as the field is still in the research starting stage, a plurality of technical problems still exist and cannot be solved.
The core technical goal of the fish body micro-plastic detection is to remove the interference of contents in the digestive tract of the fish body by a digestion means and obtain the micro-plastic in the digestive tract by filtration and separation. At present, alkaline digestion, acid digestion, enzyme digestion and the like are generally adopted to pretreat the digestive tract of a fish body sample, wherein the acid-alkaline digestion method generally uses acid or alkali with higher concentration for treatment, so that the method has higher danger, and is easy to influence the property of micro-plastic, so that the enzyme is adopted, but the digestion price is higher, and the method is not suitable for the research of large samples; meanwhile, the fat content of part of fingerlings is high, so that the membrane blockage is serious, and the experimental efficiency and the sample separation and detection are influenced.
Disclosure of Invention
Based on the defects of the prior art, the invention provides a method for detecting the micro-plastics in the fish body, the method has good digestion effect on the fish sample by using the hydrogen peroxide and the nitric acid in a superposition manner, the influence on the micro-plastics is avoided, and meanwhile, aiming at the phenomenon that part of fish has high fat content and is difficult to remove, the method adopts a surfactant and ultrasonic combination to degrade the grease, so that the influence of the grease on the detection of the micro-plastics in the digestive tract of the fish body is effectively reduced, the filtering speed is effectively increased, the detection environment is improved, and the method has good practical application value.
In a first aspect of the invention, there is provided a method of detecting micro-plastics in a fish, the method comprising:
digestion: and (3) adding hydrogen peroxide, sodium hydroxide, ferrous sulfate and acid liquor into a fish sample to be detected in sequence for digestion treatment. After the hydrogen peroxide is digested, sodium hydroxide and ferrous sulfate are added, so that the residual hydrogen peroxide is removed, and the effect of subsequently added nitric acid is prevented from being influenced.
The method further comprises the following steps:
degreasing: and (3) treating the digested fish sample by adopting a surfactant and ultrasound, so that the grease is degraded, and the influence of the grease on the detection of the micro-plastic in the digestive tract of the fish is reduced.
The fish body sample to be detected is selected from the digestive tract of the fish body.
In the detection method, other impurities are prevented from entering so as not to influence the accuracy of the detection result.
In a second aspect of the invention, there is provided the use of the above detection method for the qualitative and/or quantitative detection of microplastics in fish.
In particular, qualitative and/or quantitative detection methods include, but are not limited to, detection using electron microscopy, raman spectroscopy, and fourier-infrared spectroscopy.
The micro-plastics include, but are not limited to, micro-plastic samples of polyamide PA, polypropylene PP, polyethylene terephthalate PET, acrylonitrile-butadiene-styrene ABS, polystyrene-based PS, styrene-acrylonitrile copolymer AS, polyethylene PE, high density polyethylene HDPE, low density polyethylene LDPE, high impact polystyrene HIPS.
The beneficial technical effects of one or more technical schemes are as follows:
according to the technical scheme, the digestion process is optimized, the digestion reagent concentration, the combination of different reagents, the adding mode and the like are adjusted, so that the digestion efficiency is effectively improved, the influence on the micro-plastic is reduced, the risk coefficient is reduced, the detection accuracy is improved, the method is simple and easy to implement, the distribution characteristics of the micro-plastic in organisms, particularly in fish bodies can be researched, and the method has good practical application value.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are included to illustrate an exemplary embodiment of the invention and not to limit the invention.
FIG. 1 shows 11.5% HNO in example of the present invention 3 And 30% of H 2 O 2 Directly mixing the pre-digestion test chart; wherein the reagents in a-h are respectively 11.5% HNO 3 ：30％H 2 O 2 1, 2;
FIG. 2 shows 11.5% HNO in example of the present invention 3 With 30% of H 2 O 2 Directly mixing a post-digestion test chart; wherein the reagents in a-h are respectively 11.5% HNO 3 ：30％H 2 O 2 1, 2;
FIG. 3 is 11.5% HNO in example of the present invention 3 With 30% of H 2 O 2 Separately and sequentially adding a test chart before digestion; wherein the reagents in a-h are respectively 11.5% HNO 3 And 30％H 2 O 2 A mixed solution of;
FIG. 4 is 11.5% HNO in example of the present invention 3 With 30% of H 2 O 2 Separately and sequentially adding digested test charts; wherein the reagents in a-h are respectively 11.5% 3 With 30% of H 2 O 2 A mixed solution of;
FIG. 5 is a flow chart of the method for separating micro-plastic in fish according to the embodiment of the present invention;
FIG. 6 is a comparison graph of surface topography before and after ABS digestion in an embodiment of the present invention; the left graph is before digestion, and the right graph is after digestion;
FIG. 7 is a comparison graph of surface topography before and after AS digestion in an embodiment of the present invention; the left image is before digestion, and the right image is after digestion;
FIG. 8 is a comparison of surface topography before and after digestion of HDPE in an embodiment of the present invention; the left graph is before digestion, and the right graph is after digestion;
FIG. 9 is a comparison graph of surface topography before and after digestion of HIPS in an embodiment of the present invention; the left image is before digestion, and the right image is after digestion;
FIG. 10 is a comparison of surface topography before and after digestion of LDPE in an embodiment of the present invention; the left graph is before digestion, and the right graph is after digestion;
FIG. 11 is a comparison of the surface topography before and after digestion of PA in an embodiment of the present invention; the left graph is before digestion, and the right graph is after digestion;
FIG. 12 is a comparison graph of surface topography before and after PE digestion in an embodiment of the present invention; the left graph is before digestion, and the right graph is after digestion;
FIG. 13 is a comparison of surface topography before and after digestion of PET in an embodiment of the present invention; the left graph is before digestion, and the right graph is after digestion;
FIG. 14 is a comparison of surface topography before and after PP digestion in an embodiment of the invention; the left graph is before digestion, and the right graph is after digestion;
FIG. 15 is a comparison graph of surface topography before and after PS digestion in an embodiment of the present invention; the left graph is before digestion, and the right graph is after digestion;
FIG. 16 is a comparison graph of Raman spectra before and after ABS digestion in the example of the present invention;
FIG. 17 is a comparison chart of Raman spectra before and after AS digestion in the embodiment of the present invention;
FIG. 18 is a comparison graph of Raman spectra before and after HDPE digestion in the embodiment of the present invention;
FIG. 19 is a comparison chart of Raman spectrograms before and after HIPS digestion in the embodiment of the invention;
FIG. 20 is a comparison graph of Raman spectra before and after LDPE digestion in the example of the present invention;
FIG. 21 is a comparison chart of Raman spectra before and after PA digestion in the embodiment of the invention;
FIG. 22 is a comparison graph of Raman spectra before and after PE digestion in the embodiment of the present invention;
FIG. 23 is a comparison graph of Raman spectra before and after PET digestion in the example of the present invention;
FIG. 24 is a comparison chart of Raman spectra before and after PP digestion in an embodiment of the invention;
FIG. 25 is a comparison chart of Raman spectra before and after PS digestion in the example of the present invention;
FIG. 26 is a graph showing the recovery of particles in the 60-100 μm diameter interval in the examples of the present invention;
FIG. 27 is a graph showing the recovery rate of particles in the interval of 100 to 200 μm in diameter in the examples of the present invention;
FIG. 28 is a graph showing the recovery rate of particles having a diameter of 200 to 500 μm in the example of the present invention.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. 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.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular forms "a", "an", and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As mentioned above, the core technical goal of fish body micro-plastic detection is to remove the interference of fish body digestive tract contents by digestion means and obtain micro-plastic in the digestive tract by filtration and separation. At present, alkaline digestion, acid digestion, oxidant digestion, enzyme digestion and the like are generally adopted to pretreat the digestive tract of a fish sample, wherein the acid-alkaline digestion method generally uses acid or alkali with higher concentration for treatment, so that the method has higher danger, and is easy to influence the property of micro-plastics, therefore, the enzyme digestion price is higher, and the method is not suitable for the research of large samples; meanwhile, the fat content of part of fingerlings is high, so that the membrane blockage is serious, and the experimental efficiency and the sample separation and detection are influenced.
In view of the above, in one exemplary embodiment of the present invention, there is provided a method for detecting micro-plastics in a fish, the method comprising:
digestion: and (3) adding hydrogen peroxide, sodium hydroxide, ferrous sulfate and acid liquor into the fish body sample to be detected in sequence for digestion treatment.
In still another embodiment of the present invention, the fish sample to be tested is selected from the digestive tract of fish.
Wherein, the concentration of the hydrogen peroxide is controlled to be 24-30 percent, and is preferably 30 percent; the treatment time of the hydrogen peroxide is 1-2h;
the alkali liquor is preferably NaOH, the concentration of the NaOH is 0.1-1M, and the concentration of the NaOH is further preferably 0.5M;
the FeSO 4 The concentration of (A) is 0.001 to 0.01M, more preferably 0.005M;
the treatment time of the alkali liquor containing ferrous sulfate is 3-5h, preferably 4h;
the acid solution is preferably HNO 3 Said HNO 3 The concentration is 10% -12%; more preferably 11.5%, HNO 3 The treatment time is 5-6h, preferably 6h.
In another specific embodiment of the present invention, the digestion process is performed by a standing process.
In another embodiment of the present invention, the method further comprises:
degreasing: and (3) treating the digested fish body sample by adopting a surfactant and/or ultrasound, so that the grease is degraded, and the influence of the grease on the detection of the micro-plastics in the digestive tract of the fish body is reduced.
In yet another embodiment of the present invention, the surfactant includes but is not limited to anionic surfactant, cationic surfactant, zwitterionic surfactant and nonionic surfactant, further, the surfactant is one or more of stearic acid, sodium lauryl sulfate, lecithin, polysorbate (tween); preferably sodium dodecyl sulfate, which has better fat dissolving and degreasing effects under the coordination of ultrasonic treatment.
In another embodiment of the present invention, the degreasing method comprises: after the sodium dodecyl sulfate is added, ultrasonic treatment is carried out after the foam disappears, preferably ultrasonic treatment is carried out for 1-2h at room temperature, and further preferably ultrasonic treatment is carried out for 1h at 30 ℃.
In another embodiment of the present invention, further, the method further comprises washing and filtering the degreased fish body sample to be tested to obtain a micro plastic; wherein the filtration is specifically filtration by adopting a microporous filter membrane; furthermore, the microporous filter membrane is a nitrocellulose membrane, and the pore diameter is 5 μm.
In still another embodiment of the present invention, there is provided the use of the above detection method for qualitatively and/or quantitatively detecting in vivo microplastics in fish.
In particular, qualitative and/or quantitative detection methods include, but are not limited to, detection using electron microscopy, raman spectroscopy, and fourier-infrared spectroscopy.
It should be noted that, in the above detection method, other impurities should be avoided from entering, so as not to affect the accuracy of the detection result.
The micro-plastics include, but are not limited to, micro-plastic samples of polyamide PA, polypropylene PP, polyethylene terephthalate PET, acrylonitrile-butadiene-styrene ABS, polystyrene-based PS, styrene-acrylonitrile copolymer AS, polyethylene PE, high density polyethylene HDPE, low density polyethylene LDPE, high impact polystyrene HIPS.
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Examples
1. Experimental materials and instruments and equipment
1.1 Plastic samples
1) The larger size (4 mm. Times.4 mm. Times.3 mm) 10 types (ABS, AS, HDPE, HIPS, LDPE, PA, PE, PET, PP and PS) were screened from plastics commonly found in life and standard products were purchased.
2) Small size (60-500 μm) in the temperature controlled below 40 deg.C, using a pulverizer to pulverize millimeter plastic particles, and classifying the pulverized sample into different particle size groups through metal mesh gaps with aperture of 500 μm, 200 μm, 100 μm, and 60 μm.
1.2 Fish body samples
The fish samples were obtained from yellow sea in Shandong province or purchased in the market. The characteristics of the digestive tract (lipid characteristics, thickness) of each fish are different; in addition, the types and degree of digestion of intestinal contents vary greatly depending on the eating habits. In the early testing stage, we found that the digestion effect was very different even though we used the same experimental protocol due to the above differences. To eliminate errors as much as possible, the tissues used in this study were derived from a mixture of all fish gut and stored at-20 ℃.
1.3 materials, equipment details
TABLE 1 Experimental materials
TABLE 2 Experimental Equipment
Results of the experiment
1. Experimental results with a single reagent
Step (ii) of
Note that: in order to prevent the pollution to the experimental sample, cotton experiment clothes, nitrile gloves and a mask are worn in the whole experimental process, all glassware is washed for 3 times by using ultrapure water, and all operations are carried out in a fume hood. Digestion reagents of each concentration in the study comprise 3 groups of parallel experiments, so that errors caused by different samples and temperatures are avoided. The beaker was sealed with tin foil paper and left at room temperature for 12 hours, and the experimental phenomenon was observed
1) Taking one plastic particle, cutting a cross nick at the center of the plastic by using a scalpel, washing for 3 times by using deionized water, and air-drying for later use
2) 3.0g of fish sample is weighed by a balance and placed in a 200mL beaker, 60mL of deionized water is added, and after photographing and recording the initial state of the sample, excessive water is drained.
3) After 60mL of digestive reagent is added into the beaker (mixed or added in several times), the mouth of the beaker is sealed by tinfoil paper to prevent impurities from entering, and after the beaker is kept stand for 12 hours, a picture is taken to record the digestive effect.
3) The mixture in the beaker is made to pass through a nitrocellulose membrane with the aperture of 5 mu m by a suction filter, then the filter membrane is taken down, plastic particles are clamped by tweezers, the mixture is washed and dried by a dryer to constant weight, and the surface morphology is observed by naked eyes.
Nitric acid alone
(1) Description of phenomena
Under the action of high concentration of nitric acid, the digestive juice is clear and transparent, however all kinds of plastics are affected, wherein PA disappears and ABS melts. The rest kinds of plastics become soft to different degrees. With the decrease of the concentration, the digestion effect and the corrosion effect on the fish body are gradually weakened, but the morphological change of PA is not ignored. No macroscopic change of the PA occurred until the nitric acid concentration dropped below 12%. However, the digestion effect of the fish is general and the residual quantity is large.
(2) Conclusion
The high-concentration nitric acid has obvious corrosion to plastic particles, wherein PA changes most severely, and the digestion effect of the fish body is good; from the surface characteristics observed by naked eyes, the low concentration of nitric acid has no influence on plastic particles basically, but the fish digestion effect is poor, and the improvement is suggested.
Independent action of hydrogen peroxide
(1) Description of phenomena
We have studied the effect of hydrogen peroxide in 8 groups of concentrations, and the concentrations of 30% and 24% have better effect on fish digestion. The effect then diminishes as the concentration decreases. None of the concentrations produced macroscopic corrosion of the plastic.
(2) Conclusion
The results of this study showed that different concentrations of H 2 O 2 The use of the solution has certain application prospect and almost no harmful effect on plastics. The results of the hydrogen peroxide treatment are relatively mild compared to the acid treatment. High concentrations of hydrogen peroxide have a certain effect on the digestion of fish tissue. But low concentration of H 2 O 2 Has poor digestion effect on fish tissues, particularly on digestive tracts. Thus, H 2 O 2 The use of micro-plastics as digestive juices from fish tissue is limited and improvements have been suggested.
2. Reagent combination experiment
Due to digestive agent (HNO) 3 And H 2 O 2 ) When added alone, the digestive effect is not very desirable while maintaining retention of the plastic. According to the experimental result under a single condition, the nitric acid digestion effect is better, but the corrosion to plastics is stronger, and 11.5 percent of nitric acid does not influence the plastics, so 11.5 percent of nitric acid and H are selected 2 O 2 Combinatorial experiments were performed and further studies were continued.
Research on direct mixing ratio effect of 11.5% nitric acid and 30% hydrogen peroxide
(1) Description of phenomena
11.5% of HNO in FIGS. 1 and 2, respectively 3 And 30% of H 2 O 2 Experimental figures before and after direct mixing digestion. Wherein the reagents in the a-h pictures are respectively 11.5% HNO 3 ：30％H 2 O 2 1, 2.
After the mixture of the 11.5 percent nitric acid and the 30 percent hydrogen peroxide is mixed, the digestion effect on fish bodies is not improved compared with that of a single reagent, and in a mixed system with all the proportions, the digestion effect is reduced along with the reduction of the proportion of the nitric acid.
(2) Conclusion
Compared with a single digestion scheme, the method has the advantage that the addition of nitric acid and hydrogen peroxide at the same time is not obviously improved. We speculate that this may be due to HNO 3 And H 2 O 2 A chemical reaction takes place, after the reaction H 2 O 2 Or HNO 3 May be reduced, resulting in a poor digestion of the tissue. Therefore, the next verification is performed.
11.5% nitric acid and 30% hydrogen peroxide were added in portions
(1) Description of phenomena
FIGS. 3 and 4 are graphs of the digestion effect before and after digestion with batch additions of 11.5% nitric acid and 30% hydrogen peroxide, respectively, and a-h graphs representing the content of HNO at 11.5% 3 With 30% of H 2 O 2 Digestion in the batch addition protocol of volume ratio =1, 2.
The 11.5 percent nitric acid and the 30 percent hydrogen peroxide are added in sequence, the digestion effect is obviously better than that of a single reagent and a mixed solution with a corresponding proportion, and the plastic is not influenced. The effect improves with increasing hydrogen peroxide ratio. But as the nitric acid ratio decreases, the digestion effect decreases, when 11.5% HNO 3 And 30% of H 2 O 2 The ratio is 2.
(2) Conclusion
Two reagents are selected to be added in batches, after the hydrogen peroxide is digested, the residual hydrogen peroxide is removed by utilizing the catalysis of sodium hydroxide and ferrous sulfate solution, and then 11.5% nitric acid is added into the system to further digest the fish body tissue, so that the digestion capacity is improved.
Adding sodium hydroxide and Fe 2+ Then the reaction is violent, a large amount of bubbles are generated to float on the liquid surface,after standing for a few minutes, the bubbles disappeared. The digestion result is slightly better than that of single H 2 O 2 Solution, probably due to NaOH and Fe 2+ A catalyzed reaction. The experimental results show that the reaction is carried out by NaOH and Fe 2+ After the action, HNO is added again 3 The digestion effect is obviously better than that of directly adding HNO 3 The digestion experiment group, namely the digestion effect of adding the catalytic system is obviously better than that of directly adding HNO 3 Digestion experimental group. Also, the optimized reagent combination still has no effect on plastics.
3. Plan optimization
3.1 background
Because fat is difficult to remove, the filtration speed is slowed down during filtration, the observation of the plastic is influenced by the existence of grease, and the subsequent identification and identification of the plastic are not facilitated, the removal by adopting a surfactant (such as sodium dodecyl sulfate) is considered, and in order to ensure full mixing, an ultrasonic method is provided for assistance.
3.2 conclusion
The results show that the use of the surfactant alone has a limited effect on grease removal with ultrasound alone. When the surfactant and the ultrasonic method are combined, the grease is well removed. The lipid-containing matter in the digestive tract is put into a beaker, and in the process of observation and treatment, the lipid is gradually dispersed, the volume is reduced, and the foam of a reaction system is increased. After about 40min, the state of the substance had hardly changed. After standing for 6h, the amount of foam was reduced and the lipid particles were no longer increased. Therefore, the optimized method of fat is determined to be that after all the inorganic reagents are acted, saturated sodium dodecyl sulfate solution is added into a beaker, and the ultrasound is carried out for 1h after the foam quantity is reduced.
4. Determination of digestion protocols
In conclusion, the optimal binary system digestion scheme is as follows: at the beginning of the tissue digestion process, 30% H was added to the beaker 2 O 2 Standing for 1h; then 0.5M NaOH and 0.005M Fe were added 2+ Standing for 4h; final addition of 11.5% HNO 3 Put into a beaker and stand for 6 hours. 150g/L SDS solution was added further, followed by sonication for 1h.
Step (ii) of
1) A3.0 g fish sample was weighed using a balance and placed in a 200mL beaker.
2) Adding 20mL of 30% H 2 O 2 And standing for 1h.
3) To the beaker were added 10mL of 0.5M NaOH solution and 1mL of 0.005M FeSO 4 The solution was allowed to stand for 4h.
4) Adding 40mL11.5% HNO to the beaker 3 And standing for 6 hours.
5) Measuring 20ml,150g/L sodium dodecyl sulfate, adding into a beaker, and after the foam disappears, carrying out ultrasonic treatment for 1h at the temperature of 30 ℃.
The flow chart is shown in figure 5.
5. Scheme verification
(1) Morphological contrast
1) Before the optimal digestion scheme is used for digestion, a Raman spectrometer is used for carrying out microscopic shooting and spectrogram test on scored plastics (the optimal test parameters of various plastics are determined in the pre-experiment process);
2) After the optimal digestion scheme, the plastic particles are taken out of the beaker, washed 3 times with deionized water to remove impurities attached to the surface, dried to constant weight at normal temperature, and the plastic sample is scanned again under the same parameter setting.
(2) Conclusion
The test results are shown in fig. 6-25, and the change of the circumference of the cross mark on the surfaces of 10 plastic particles is not obvious by comparing before and after digestion. The 10 plastics have no great difference in peak position before and after reaction, and the plastic spectrogram after digestion has strong identifiability. Indicating that the digestive reagent has no significant effect on the molecular structure of the plastic.
4.3 recovery validation
(1) The experimental steps are as follows:
1) The plastic particles are crushed by a crusher under the condition that the temperature is controlled to be lower than 40 ℃, and the crushed mixed sample is divided into three particle size intervals of 60-100 mu m, 100-200 mu m and 200-500 mu m by a metal sieve with the aperture of 500 mu m, 200 mu m, 100 mu m and 60 mu m.
2) For each plastic, 30 granules per size interval were picked up by means of a microscope and placed in a beaker and digested according to a defined optimal protocol.
3) After suction filtration, the filter was removed, the particles were visually identified by microscopy and the values recorded.
4) Recovery = number of particles after digestion/number of particles before digestion × 100%.
(2) Conclusion
The results are shown in FIGS. 26-28, and the recovery rates for 10 plastic particles were between 80% and 120% for particle size studies greater than 60 μm. The digestion scheme adopted by the experiment has little influence on the recovery rate of the micro-plastic, and can be used for detecting environmental samples at present.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (15)
1. A method of detecting micro-plastics in a fish, the method comprising:
digestion: adding hydrogen peroxide, sodium hydroxide, ferrous sulfate and acid liquor into a fish body sample to be detected in sequence for digestion treatment;
degreasing: treating the fish body sample to be detected after the digestion is finished by adopting a surfactant and ultrasound;
the method also comprises the steps of washing and filtering the degreased fish body sample to be detected to obtain micro plastic;
the fish body sample to be detected is selected from the digestive tract of the fish body;
the acid liquor is HNO 3 Said HNO 3 Concentration of 11.5%, HNO 3 The treatment time is 5-6h;
the concentration of the hydrogen peroxide is controlled to be 24-30 percent; the treatment time of the hydrogen peroxide is 1-2h;
the concentration of the NaOH is 0.1-1M;
the FeSO 4 The concentration of (A) is 0.001-0.01M; the treatment time of the ferrous sulfate and the sodium hydroxide is 3-5h.
2. The method according to claim 1, wherein the filtration is in particular a filtration with a microfiltration membrane.
3. The method of claim 2, wherein the microfiltration membrane has a pore size of 5 μm.
4. The method of claim 1, wherein the hydrogen peroxide concentration is controlled to be 30%.
5. The method of claim 2, wherein the concentration of NaOH is 0.5M.
6. The method of claim 1, wherein the FeSO4 concentration is 0.005M; the treatment time of ferrous sulfate and sodium hydroxide is 4h.
7. The method according to claim 1, wherein the digestion treatment is performed by standing.
8. The method of claim 1, wherein the surfactant comprises an anionic surfactant, a cationic surfactant, a zwitterionic surfactant, and a nonionic surfactant.
9. The method of claim 8, wherein the surfactant is one or more of stearic acid, sodium lauryl sulfate, lecithin, polysorbate (tween).
10. The method of claim 8, wherein the surfactant is sodium lauryl sulfate.
11. The method according to claim 1, wherein the degreasing step is in particular: after the sodium dodecyl sulfate is added, ultrasonic treatment is carried out after the foam disappears.
12. The method of claim 11, wherein the sonication is carried out at room temperature for 1-2 hours.
13. The method of claim 11, wherein sonication is carried out at 30 ℃ for 1 hour.
14. Use of the detection method according to any one of claims 1 to 13 for the qualitative and/or quantitative detection of microplastics in fish;
the micro-plastics include micro-plastic samples of polyamide, polypropylene, polyethylene terephthalate, acrylonitrile-butadiene-styrene plastic, polystyrene plastic, styrene-acrylonitrile copolymer, polyethylene, high density polyethylene, low density polyethylene, high impact polystyrene.
15. Use of the detection method according to any one of claims 1 to 13 for the qualitative and/or quantitative detection of microplastics in fish; qualitative and/or quantitative detection methods include detection using electron microscopy, raman spectroscopy, and fourier-infrared spectroscopy.
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