CN113358623A - Method for quantitatively analyzing micro-plastics in leaf vegetables - Google Patents
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Abstract
The invention provides a method for quantitatively analyzing micro-plastics in leaf vegetables. The method specifically comprises the steps of crushing leaf vegetables, mixing the crushed leaf vegetables with a digesting agent for 3-5 hours at 40-60 ℃ to obtain a digesting solution, measuring the concentration of the digesting solution, and calculating to obtain the content of the micro-plastics in the leaf vegetables. According to the method, the micro-plastics in the leaf vegetables can be completely digested by the specific digestion method suitable for the micro-plastics of the leaf vegetables, and the structure of the micro-plastics cannot be damaged, so that the content of the micro-plastics in the leaf vegetables can be efficiently and accurately determined, and the method has considerable necessity for the technical field of quantitative analysis of leaf vegetable pollutants.
Description
Technical Field
The invention belongs to the technical field of quantitative analysis of leaf vegetable pollutants. More particularly, the invention relates to a method for quantitatively analyzing the micro-plastics in the bodies of leafy vegetables.
Background
By 2019, the total amount of plastic products produced in China exceeds 10 hundred million tons, which becomes the first major country of global plastic production and consumption, but the total recovery rate of plastics is less than 20%, a large amount of waste plastics enter plant bodies, and researches show that the micro plastics have obvious influence on the growth of various plants at present, for example, when the broad bean root tip cells contain a large amount of 0.1 mu m micro plastics, the normal growth of the plants is obviously inhibited, and the oxidative damage is caused; as another example, a clear growth inhibitory effect was also observed in studies of the effect of microplastics on wheat growth. However, most of the existing researches only explain the influence of the micro-plastics on the growth of plants, but do not aim at quantitative analysis research of the micro-plastics in the plants, and limit the research progress of the micro-plastics in the aspects of absorption pathways, distribution rules and toxicity response mechanisms in the plants.
However, the present inventors have conducted a great deal of research in the early stage, and as a result, it has been shown that since the structure and components of leaf vegetable cells are greatly different from those of animal cells, when a microplastic digesting agent for most animals such as fish is used to digest microplastic in leaf vegetables, the structure of microplastic can be destroyed, or microplastic is not completely digested, resulting in excessively high or excessively low microplastic content in the finally determined leaf vegetables, the digestion method applicable to the micro-plastics in the bodies of mammals is not necessarily applicable to the micro-plastics in the bodies of leaf vegetables.
Therefore, a digestion and extraction method suitable for quantitative analysis of micro-plastics in leaf vegetables is urgently needed to be found, the content of the micro-plastics in the leaf vegetables is accurately determined, and the method has considerable necessity for the technical field of quantitative analysis of leaf vegetable pollutants.
Disclosure of Invention
The invention provides a method for quantitatively analyzing micro-plastics in leaf vegetables aiming at the defects of the conventional method for quantitatively analyzing the micro-plastics in the leaf vegetables. According to the method, the micro-plastics in the leaf vegetables can be completely digested by the specific digestion method suitable for the micro-plastics in the leaf vegetables, and the structure of the micro-plastics cannot be damaged, so that the content of the micro-plastics in the leaf vegetables can be efficiently and accurately determined.
The above purpose of the invention is realized by the following technical scheme:
the invention provides a method for quantitatively analyzing micro-plastics in leaf vegetables, which comprises the following steps:
s1, crushing leaf vegetables, and mixing the crushed leaf vegetables with a digesting agent at the temperature of 40-60 ℃ for 3-5 hours to obtain a digesting solution;
s2, measuring the concentration of the micro-plastic in the digestion solution obtained in the step S1, and calculating to obtain the content of the micro-plastic in the leaf vegetables;
wherein the digesting agent consists of H2O2Aqueous solution and HNO3The composition of aqueous solution; the HNO3The concentration of the aqueous solution is 60-70% (w/w), H2O2The concentration of the aqueous solution is 25-35% (w/w); oven-dried quality of leaf vegetables, HNO3Volume of aqueous solution, H2O2The volume ratio of the aqueous solution is 5-20 mg: 2.8-3.6 mL: 0.6-1.0 mL.
When HNO3Aqueous solution and H2O2When the concentration of the aqueous solution is too high, the aqueous solution has strong oxidizing property and is easy to damage the structure of the micro plastic, so that the quantitative result is too high; when HNO3Aqueous solution and H2O2When the concentration of the aqueous solution is too low, the digestion of the micro-plastic is incomplete, so that the quantitative result is too low.
Preferably, the leaf vegetables of step S1 include one or more of leaf vegetables, lettuce, shanghai green or spinach.
Most preferably, the HNO3The concentration of the aqueous solution was 65% (w/w), H2O2The concentration of the aqueous solution was 30% (w/w), see example 3.
Most preferably, the oven dried quality, HNO, of the leafy vegetables3Volume of aqueous solution, H2O2The volume ratio of the aqueous solution is 10 mg: 3.2 mL: 0.8mL, see example 3.
Preferably, the mixing in step S1 is mixing with digesting agent at 50 ℃ for 4h, see example 3.
Preferably, the leafy vegetables are further dried before being pulverized in step S1.
Further preferably, the drying in step S1 is drying in an oven at 40-50 ℃.
Further preferably, the drying in step S1 is drying in an oven at 45 ℃, see example 3.
Preferably, the concentration of the micro-plastic is obtained by measuring the fluorescence intensity of the digestion solution by an ultramicro fluorescence spectrophotometer and then calculating according to a standard curve.
The invention has the following beneficial effects:
according to the method, the micro-plastics in the leaf vegetables can be completely digested by the specific digestion method suitable for the micro-plastics of the leaf vegetables, and the structure of the micro-plastics cannot be damaged, so that the content of the micro-plastics in the leaf vegetables can be efficiently and accurately determined, and the method has considerable necessity for the technical field of quantitative analysis of leaf vegetable pollutants. .
Drawings
FIG. 1 is a photograph of a digestion solution of example 2.
Figure 2 is the micro plastic recovery of example 2. Wherein NaOH is "NaOH (10 mol/L)"; KOH means "KOH (2.5 mol/L)"; HNO3Refers to "HNO3(65～70％；w/w)”；H2O2Means "H2O2(30％；w/w)”；1HNO3: 1HCl means "HNO3(15.9mol/L)：HCl(12.1mol/L)＝1：1；v/v”；4HNO3：1H2O2Refers to "HNO3(65％；w/w)：H2O2(30％；w/w)＝4：1；v/v”；4HNO3：1HClO4Refers to "HNO3(65％；w/w)：HClO4(68％；w/w)＝4：1；v/v”；1HNO3: 10NaClO means "HNO3(65％；w/w)：NaClO(9％；w/w)＝1：10；v/v”。
FIG. 3 is a scanning electron micrograph of the microplastic spheres of example 2.
FIG. 4 shows the observation results of the micro plastic laser confocal microscope of example 2.
FIG. 5 is a photograph of a digestion solution of example 3.
FIG. 6 is a scanning electron micrograph of the microplastic spheres of example 3.
FIG. 7 shows the observation results of the micro plastic laser confocal microscope of example 3.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
EXAMPLE 1 hydroponic cultivation of Microplastic-enriched leaf lettuce
S1, selecting micro plastic: polystyrene micro plastic spheres (micro plastic) with the particle size of 0.2 μm, which are purchased from Shanghai chitin Biotechnology Co., Ltd, are used as test materials, and green fluorescent dye is wrapped at the sphere center of the polystyrene micro plastic spheres and is not easy to damage and generate fluorescence quenching.
S2, obtaining the leaf lettuce rich in fluorescent micro-plastic: 300mL of Hoagland's solution is used as a hydroponic solution, the leaf lettuce is hydroponically cultured, polystyrene micro plastic balls with the concentration of 30mg/L are added, the concentration of the micro plastic in the Hoagland's solution is 20mg/L, and 6 parallel samples are set; continuously culturing for 10 days, wherein the illuminance is kept at 15000lux in the culture process, the temperature is kept at 22 ℃ in the daytime and 16 ℃ at night, nutrient solution is appropriately supplemented midway to maintain the growth requirement of the leaf lettuce, the fallen leaves are kept for subsequent content analysis, and the harvested leaf lettuce is enriched with micro-plastics; then carrying out ultrasonic treatment on the leaf lettuce for 20 minutes to desorb the micro-plastics adsorbed on the surface of the leaf lettuce, and finally pouring the desorbed solution back into the water culture solution, wherein the concentration C of the micro-plastics in the water culture solution is1Measured by a NanoDrop 3300 ultramicro fluorescence spectrophotometer at 488nm wavelength.
Example 2 quantitative analysis of leaf lettuce micro-plastics with different digesting agents
The first experiment method comprises the following steps:
s1, placing the ultrasonic leaf lettuce and the leaf lettuce fallen off in the water culture process in a 45 ℃ oven for drying and crushing to obtain 3.2g of leaf lettuce powder, then respectively taking 10mg of the leaf lettuce powder according to the composition, the volume, the digestion temperature and the digestion time of a digestion agent shown in the table 1, mixing and digesting the leaf lettuce and the digestion agent to obtain a digestion solution (photographing to obtain a picture 1);
s2, measuring the fluorescence intensity of the digestion solution at the position of 488nm wavelength by using a NanoDrop 3300 ultra-micro fluorescence spectrophotometer, and calculating according to a standard curve to obtain the concentration C of the micro-plastic in the digestion solution2And further calculating to obtain the content of the micro-plastics in the leaf lettuce.
TABLE 1
II, experimental results:
calculating the recovery rate of the micro-plastic according to the following formula, and drawing the calculation result into a histogram to obtain a graph shown in figure 2:
recovery of microplastic (%) - (V)2*C2*320+V1*C1)/M0*100％
Wherein, V2Represents the volume of digestion solution; c2Indicating the concentration of the micro-plastic in the digestion solution; 320 is the ratio of 3.2g of the total weight of the leaf lettuce obtained after the crushing in the step (2) S1 to 10mg of the leaf lettuce powder subjected to digestion; v1Represents the volume of the hydroponic solution after adding the desorption solution to the hydroponic solution; c1Indicating the micro-plastic concentration in the hydroponic solution after the desorption solution is added to the hydroponic solution; m0The mass of polystyrene micro-plastic spheres initially added to the hydroponic solution is indicated.
Filtering the digestion solution with a nitrocellulose filter membrane, scanning the micro plastic particles obtained by filtering with a scanning electron microscope to obtain a spherical scanning electron microscope image (figure 3), and observing the fluorescence dispersion degree of the micro plastic with a laser confocal microscope (figure 4).
As can be seen from FIG. 1, the use of "NaOH (10 mol/L)", "KOH (2.5 mol/L)" and "H2O2(30%; w/w) "as a digesting agent to obtain a digestion solution after digestion, and also a large amount of green leaf lettuce residues; as can be seen from FIG. 2, when the digesting agents are "NaOH (10 mol/L)", "KOH (2.5 mol/L)" and "H2O2(30%; w/w) "the highest recovery rate of the leaf lettuce micro-plastics, which exceeds 100%; in addition, as can be seen from fig. 3 and 4, the profile of the micro plastic particles obtained after digestion by the three digesting agents is unclear, the fluorescent light spots are incomplete, and green fuzzy lumps exist, because under the three digesting agents, the micro plastic particles in the leaf lettuce body are broken and deformed, the green fluorescent dye leaks, so that the fluorescence intensity measured by the NanoDrop 3300 ultramicro fluorescence spectrophotometer is inaccurate, and the finally calculated recovery rate is higher than 100%, so that the three digesting agents are not suitable for quantitatively analyzing the micro plastic in the leaf lettuce body.
As can be seen from FIG. 2, the digesting agent "HNO3(65％；w/w)：H2O2(30%; w/w) 4: 1; the recovery rate of the micro plastic at v/v' reaches 86.05 percent; as can be seen from the combination of FIGS. 3 and 4, when the digesting agent is "HNO3(65％；w/w)：H2O2(30%; w/w) 4: 1; v/v', the digested micro plastic particles present clear particles, and the green fluorescence is complete and not destroyed, which indicates that when the digesting agent is used for digesting the micro plastic in the leaf lettuce, the structure of the micro plastic can not be damaged, and the micro plastic in the leaf lettuce can be quantitatively analyzed more accurately.
As can also be seen in FIG. 2, other digesting agents ("HNO") are employed3(65～70％；w/w)”、“HNO3(15.9mol/L)：HCl(12.1mol/L)＝1：1；v/v”、“HNO3(65％；w/w)：HClO4(68％；w/w)＝4：1；v/v”、“HNO3(65%; w/w): NaClO (9%; w/w) ═ 1: 10; v/v') the recovery rate of the micro-plastic obtained by digestion is only 67.69-79.64%, and the digestion effect is not good.
Visible counteractant "HNO3(65％；w/w)：H2O2(30%; w/w) 4: 1; v/v' can quantitatively analyze the micro-plastics in the leaf lettuce more accurately.
Example 3 method for quantitative analysis of microplastics in leaf of Oedalea sativa
First, experiment method
S1, placing the ultrasonic leaf lettuce and the leaf lettuce fallen off in the water culture process in a 45 ℃ oven for drying and crushing to obtain 3.2g of leaf lettuce powder, and mixing and digesting 10mg of leaf lettuce powder with 4mL of digesting agent at 50 ℃ for 4 hours to obtain a digestion solution;
s2, measuring the fluorescence intensity of the digestion solution at the wavelength of 488nm by using a NanoDrop 3300 ultramicro fluorescence spectrophotometer, calculating the concentration of the micro-plastics in the digestion solution according to a standard curve, and further calculating the content of the micro-plastics in the leaf lettuce;
wherein the digesting agent consists of H2O2Aqueous solution and HNO3The composition of aqueous solution; the HNO3The concentration of the aqueous solution was 65% (w/w), H2O2The concentration of the aqueous solution was 30% (w/w), HNO3Volume of aqueous solution and H2O2The volume ratio of the aqueous solution is 4: 1.
second, experimental results
The micro-plastic recovery was calculated to be 97.31%.
Example 4 method for quantitative analysis of microplastics in leaf of Oedalea sativa
First, experiment method
The experimental procedure of example 3 was followed except that the digestion time of the mixture in step S1 was 3 hours.
Second, experimental results
The micro-plastic recovery was calculated to be 90.15%.
Example 5A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The experimental procedure of example 3 was followed except that the digestion time of the mixture in step S1 was 5 hours.
Second, experimental results
The micro-plastic recovery was calculated to be 96.81%.
Example 6A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The same experimental procedure as in example 3, except that the HNO3The concentration of the aqueous solution was 70% (w/w), H2O2The concentration of the aqueous solution was 25% (w/w).
Second, experimental results
The micro-plastic recovery was calculated to be 92.36%.
Example 7A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The same experimental procedure as in example 3, except that the HNO3The concentration of the aqueous solution was 60% (w/w), H2O2The concentration of the aqueous solution was 35% (w/w).
Second, experimental results
The micro-plastic recovery was calculated to be 91.31%.
Example 8A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The experimental procedure of example 3 was followed except that the temperature of the mixed digestion in step S1 was 40 ℃.
Second, experimental results
The micro-plastic recovery was calculated to be 91.22%.
Example 9A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The experimental procedure of example 3 was followed except that the temperature of the mixed digestion in step S1 was 60 ℃.
Second, experimental results
The micro-plastic recovery was calculated to be 92.44%.
Example 10A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The experimental method of example 3 was repeated except that the leaf lettuce powder of step S1 was 20mg in mass and HNO was added3Volume of aqueous solution 3.6mL, H2O2The volume of the aqueous solution was 0.6 mL.
Second, experimental results
The micro-plastic recovery was calculated to be 93.17%.
Example 11A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The experimental method of example 3 was repeated except that the leaf lettuce powder of step S1 was 5mg in mass and HNO was added3Volume of aqueous solution 2.8mL, H2O2The volume of the aqueous solution was 1.0 mL.
Second, experimental results
The micro-plastic recovery was calculated to be 95.62%.
Example 12A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The experimental method of example 3 is different in that the drying in step S1 is oven drying at 50 ℃.
Second, experimental results
The micro-plastic recovery was calculated to be 96.22%.
Example 13A method for quantitative analysis of microplastics in leaf of Oedalia oleifera
First, experiment method
The experimental method of example 3 is different in that the drying in step S1 is oven drying at 40 ℃.
Second, experimental results
The micro-plastic recovery was calculated to be 94.57%.
Example 14A method for quantitative analysis of microplastics in lettuce
First, experiment method
The experimental procedure of example 3 was followed except that lettuce was replaced with lettuce.
Second, experimental results
The micro-plastic recovery was calculated to be 98.11%.
Example 15A method for quantitative analysis of Microplastics in Shanghai Qingre
First, experiment method
The experimental procedure of example 3 was followed except that leaf lettuce was replaced with Shanghai green.
Second, experimental results
The micro-plastic recovery was calculated to be 97.23%.
Example 16A method for quantitatively analyzing in vivo microplastic of spinach
First, experiment method
The experimental procedure of example 3 was followed except that lettuce was replaced with spinach.
Second, experimental results
The micro-plastic recovery was calculated to be 96.97%.
Comparative example 1
First, experiment method
The experimental procedure of example 3 was followed, except that the time for the mixed digestion in step S1 was 2 hours.
Second, experimental results
The micro-plastic recovery was calculated to be 54.85%.
Comparative example 2
First, experiment method
The experimental procedure of example 3 was followed, except that the time for the mixed digestion in step S1 was 8 hours.
Second, experimental results
The micro-plastic recovery was calculated to be 108.83%.
Comparative example 3
First, experiment method
The same experimental procedure as in example 3, except that the HNO3The concentration of the aqueous solution was 50% (w/w), H2O2The concentration of the aqueous solution was 15% (w/w).
Second, experimental results
The micro-plastic recovery was calculated to be 65.26%.
Comparative example 4
First, experiment method
The experimental procedure of example 3 was followed except that the temperature of the mixed digestion in step S1 was 20 ℃.
Second, experimental results
The micro-plastic recovery was calculated to be 20.25%.
Comparative example 5
First, experiment method
The experimental procedure of example 3 was followed except that the temperature of the mixed digestion in step S1 was 70 ℃.
Second, experimental results
The micro-plastic recovery was calculated to be 73.56%.
Comparative example 6
First, experiment method
The experimental method of example 3 was repeated except that the leaf lettuce powder of step S1 was 40mg in mass and HNO was added3Volume of aqueous solution 4.5mL, H2O2The volume of the aqueous solution was 0.3 mL.
Second, experimental results
The micro-plastic recovery was calculated to be 86.54%.
Comparative example 7
First, experiment method
The experimental method of example 3 was repeated except that the leaf lettuce powder of step S1 was 5mg in mass and HNO was added3Volume of aqueous solution 1.2mL, H2O2The volume of the aqueous solution was 1.5 mL.
Second, experimental results
The micro-plastic recovery was calculated to be 84.89%.
Comparative example 8
First, experiment method
The experimental procedure of example 3 was followed except that lettuce was replaced with potato.
Second, experimental results
The micro-plastic recovery was calculated to be 76.33%.
Comparative example 9
First, experiment method
The experimental procedure of example 3 was followed except that lettuce was replaced with carrot.
Second, experimental results
The micro-plastic recovery was calculated to be 82.33%.
Comparative example 10
First, experiment method
The experimental procedure of example 3 was followed except that lettuce was replaced with white radish.
Second, experimental results
The micro-plastic recovery was calculated to be 84.87%.
Comparative example 11
First, experiment method
The experimental procedure of example 3 was followed except that leaf lettuce was replaced with rice grain.
Second, experimental results
The micro-plastic recovery was calculated to be 74.44%.
In conclusion, the recovery rates of the micro-plastics in the examples 3 to 16 are all above 90%, which shows that the micro-plastics in the leaf vegetables can be accurately and quantitatively analyzed by the methods in the examples 3 to 16.
The recovery rate of the micro-plastic in the comparative example 2 is more than 100%, which is probably because the micro-plastic particles in the leaf lettuce body are broken and deformed, the green fluorescent dye in the leaf lettuce body leaks, the accuracy of the fluorescence intensity result of the NanoDrop 3300 ultramicro fluorescence spectrophotometer is influenced, and the calculated recovery rate is higher and even exceeds 100%, so that the method in the comparative example 2 is not suitable for quantitatively analyzing the micro-plastic in the leaf lettuce body.
The recovery rate of the micro-plastics of comparative examples 1 and 3-7 is below 90%, which shows that the digestion effect is not good, and the method is not suitable for quantitative analysis of the micro-plastics in the leaf vegetables.
The recovery rate of the micro-plastics of the comparative examples 8-11 is below 90%, and the digestion effect is poor, so that the method is not suitable for quantitative analysis of the micro-plastics in the non-leafy vegetables.
The digestion solution of example 3 was photographed (fig. 5), and after filtration with a nitrocellulose filter, the microplastic particles obtained by filtration were scanned with a scanning electron microscope to obtain a scanning electron microscope image of a sphere (fig. 6), and the degree of fluorescence diffusion of the microplastic was observed with a confocal laser microscope (fig. 7). It can be seen from the figure that the digestion solution obtained by digesting the micro-plastics in the leaf lettuce by the method of the embodiment 3 is clear and has no residue, the fluorescence of the digested micro-plastics is not destroyed, and the surface contour of the micro-plastic particles is clear, which shows that the micro-plastics in the leaf lettuce can be completely digested by the method of the present invention without damaging the structure of the micro-plastics, so that the content of the micro-plastics in the leaf lettuce can be efficiently and accurately determined, and the method has considerable necessity for the technical field of quantitative analysis of the leaf vegetable pollutants.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A method for quantitatively analyzing micro-plastics in leaf vegetables is characterized by comprising the following steps:
s1, crushing leaf vegetables, and mixing the crushed leaf vegetables with a digesting agent at the temperature of 40-60 ℃ for 3-5 hours to obtain a digesting solution;
s2, measuring the concentration of the micro-plastic in the digestion solution obtained in the step S1, and calculating to obtain the content of the micro-plastic in the leaf vegetables;
wherein the digesting agent consists of H2O2Aqueous solution and HNO3The composition of aqueous solution; the HNO3The concentration of the aqueous solution is 60-70% (w/w), H2O2The concentration of the aqueous solution is 25-35% (w/w); oven-dried quality of leaf vegetables, HNO3Volume of aqueous solution, H2O2The volume ratio of the aqueous solution is 5-20 mg: 2.8-3.6 mL: 0.6-1.0 mL.
2. The method of claim 1, wherein the leaf vegetables of step S1 comprise one or more of leaf vegetables selected from the group consisting of leaf lettuce, green sea weed, and spinach.
3. According to claimThe method of claim 1, wherein the HNO is3The concentration of the aqueous solution was 65% (w/w), H2O2The concentration of the aqueous solution was 30% (w/w).
4. The method according to claim 1, wherein the quality of the leaf vegetables is oven dried, HNO3Volume of aqueous solution, H2O2The volume ratio of the aqueous solution is 10 mg: 3.2 mL: 0.8 mL.
5. The method according to claim 1, wherein the mixing of step S1 is mixing with digesting agent at 50 ℃ for 4 h.
6. The method of claim 1, wherein the leaf vegetables are further dried before being pulverized in step S1.
7. The method according to claim 6, wherein the drying in step S1 is drying in an oven at 40-50 ℃.
8. The method of claim 7, wherein the drying of step S1 is drying in an oven at 45 ℃.
9. The method according to claim 1, wherein the concentration of the micro plastic is calculated from a standard curve after measuring the fluorescence intensity of the digestion solution by an ultramicro fluorescence spectrophotometer.
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