CN108344818A - The remaining detection method of Multiple Pesticides in a kind of soil - Google Patents
The remaining detection method of Multiple Pesticides in a kind of soil Download PDFInfo
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- CN108344818A CN108344818A CN201810159507.XA CN201810159507A CN108344818A CN 108344818 A CN108344818 A CN 108344818A CN 201810159507 A CN201810159507 A CN 201810159507A CN 108344818 A CN108344818 A CN 108344818A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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Abstract
The invention discloses the remaining detection methods of Multiple Pesticides in a kind of soil, belong to Soil K+adsorption technical field.The remaining detection method of Multiple Pesticides in the soil, including：(1) deionized water is added into pedotheque to impregnate, glacial acetic acid acetonitrile solution, anhydrous magnesium sulfate, sodium chloride and sodium acetate is then added, carry out vortex and centrifugal treating successively；(2) supernatant of step (1) is taken, anhydrous magnesium sulfate and multi-walled carbon nanotube is added, carries out vortex and centrifugal treating successively；(3) it takes the supernatant of step (2) in being concentrated in Rotary Evaporators, with being filtered after n-hexane acetone mixed solvent constant volume, filtrate is measured and is confirmed.The detection method of the present invention is efficiently simple, greatly reduce amount of reagent compared to conventional pre-treating method, reduce the use of toxic organic solvent, not only reduces cost but also environmentally friendly, the clean-up effect for improving extraction efficiency and matrix realizes requirement that is quick, easy, accurately and simultaneously analyzing.
Description
Technical field
The present invention relates to Soil K+adsorption technical fields, and in particular to the remaining detection method of Multiple Pesticides in a kind of soil.
Background technology
The use of pesticide is the primary leap in agricultural production, to prevent pest and disease damage from threatening, promoting crop growth, China
Pesticide use is more extensive so that Pesticide-Polluted Soil content is higher, easily causes animal body pesticide residue savings or pesticide poisoning thing
Part endangers public's health.Therefore, the remaining detection of Pesticide Residue in Soil becomes the pith of environment measuring.Soil matrix
Complexity, pre-treatment is extremely important, and the residual common pre-treating method of detection of agriculture at present includes：Soxhlet extraction, adds liquid-liquid extraction method
Quick-dissolving agent extraction method, ultrasonic extraction, microwave extraction method, gel permeation, solid phase extraction, matrix solid phase dispersion extraction
Deng.The type that these methods detect pesticide residue simultaneously is few, and efficiency is low, chemical levels are big, of high cost.
Invention content
The purpose of the present invention is to provide the remaining detection methods of Multiple Pesticides in a kind of soil, to solve existing detection side
The type that method detects pesticide residue simultaneously is few, the problem that efficiency is low, chemical levels are big, of high cost.
The technical solution that the present invention solves above-mentioned technical problem is as follows：
The remaining detection method of Multiple Pesticides in a kind of soil, including：
(1) deionized water is added into pedotheque to impregnate, glacial acetic acid-acetonitrile solution, anhydrous magnesium sulfate, chlorine is then added
Change sodium and sodium acetate, carries out vortex and centrifugal treating successively；
(2) supernatant of step (1) is taken, anhydrous magnesium sulfate and multi-walled carbon nanotube is added, is vortexed and is centrifuged successively
Processing；
(3) take the supernatant of step (2) in being concentrated in Rotary Evaporators, with mistake after n-hexane-acetone mixed solvent constant volume
Filter, is measured filtrate and confirms.
The present invention screens the type that adsorbent uses on the basis of existing QuEChERS methods, makes it more
Purification suitable for soil matrix；Compared with traditional QuEChERS methods, in order to improve the rate of recovery of object, it is also simultaneously
In order to ensure the stability of Pesticide Residue in Soil, appropriate acetic acid is added in Extraction solvent of the invention, the rate of recovery is good and stablizes.This reality
The QuEChERS methods for testing use are that cleanser multi-walled carbon nanotube is added directly into extracting solution, with traditional Solid Phase Extraction
Method compares the solvent that can be saved needed for a large amount of column activation and elution, and can save the time.With classical second eyeball extraction, Fu Luoli silicon
The earth pillar method of purification compares, and solvent can be saved by making extractant with glacial acetic acid-acetonitrile, be reduced environmental pollution.Meanwhile multi wall carbon is added
Can be with the ability of adsorpting pigment after nanotube, while also there is certain clean-up effect.Because it is with excellent adsorption energy
A small amount of multi-walled carbon nanotube is added in power, so that it may reach good clean-up effect, greatly reduce miscellaneous in soil extract
Matter.The result shows that this method has the good rate of recovery and repeatability, and simplify operation sequence.
It for existing QuEChERS methods, is extracted with extractant, is directly after taking supernatant to cross film after cleanser purification
Upper machine, the present invention is converted to glacial acetic acid-acetonitrile of addition with n-hexane+acetone, using n-hexane+acetone as upper machine
Solvent can substantially reduce the damage to pillar, and small to the pollution of instrument, improve instrument compared to glacial acetic acid-acetonitrile
Sensitivity, peak shape is more preferable, and the rate of recovery is also more stable.The present invention has the advantages that many using acetonitrile as extractant.Acetonitrile itself is
Polar solvent, can be miscible with water, and so as to effectively extract water-soluble pesticide, and acetonitrile can dissolve most of chemical combination
Object, dissolving power is relatively good, is not easy band impurity, disclosure satisfy that the analysis for extracting requirement in pesticide residue analysis, pesticide after extracting
The rate of recovery can reach the standard of Pesticides Testing, the boiling point of acetonitrile is 81~82 DEG C, thus not volatile.
In addition, present invention introduces multi-walled carbon nanotubes as new type purification material, as a result accurately, the rate of recovery is high.The present invention
On the basis of sample pre-treatments and GC-MC conditions, the novel QuEChERS/GC-MS detection methods of a variety of drugs are established, are made
While it can meet a variety of drugs and quantifies testing requirements, the sensitivity with tandem mass spectrum.
Further, in this experiment in novel preferred embodiment, in step (1), glacial acetic acid-acetonitrile solution it is dense
It is 0.8-1.2wt% to spend, and the volume ratio of glacial acetic acid and acetonitrile is (0.8-1.2)：(98.8-99.2).
The present invention selects 0.8-1.2wt% glacial acetic acid-acetonitrile not only to have the higher rate of recovery, Er Qieyi to pesticide extraction
The more other solvents of nitrile can more effectively reduce the interference of wax, fat, protein, lipophilic pigment and other leachables, wherein ice
Acetic acid can form buffer salt with sodium acetate, so that pH value range is maintained at 6~7, enhance the stability of pesticide.
Further, in preferred embodiments of the present invention, in step (1), glacial acetic acid-acetonitrile solution, anhydrous slufuric acid
The mass ratio (9-11) of magnesium, sodium chloride and sodium acetate：(3.9-4.1)：(0.9-1.1)：(0.9-1.1).
Further, in preferred embodiments of the present invention, in step (1), vortex time 1-2min, centrifugal rotational speed
For 7800-8200r/min, centrifugation time 4-6min.
Further, in preferred embodiments of the present invention, in step (2), supernatant, anhydrous magnesium sulfate and multi wall carbon
The mass ratio of nanotube is (5-7)：(0.5-1)：(0.005-0.007).
Further, in preferred embodiments of the present invention, in step (2), vortex time 1-2min, centrifugal rotational speed
For 7800-8200r/min, centrifugation time 4-6min.
Further, in preferred embodiments of the present invention, in step (3), supernatant mixes molten with n-hexane-acetone
The volume ratio of agent is (1.5-2.5)：1.
Further, in preferred embodiments of the present invention, in n-hexane-acetone mixed solvent, n-hexane and acetone
Volume ratio is (8.8-9.2)：(0.8-1.2).
Further, in preferred embodiments of the present invention, the temperature of Rotary Evaporators is 35-45 DEG C.
Further, in preferred embodiments of the present invention, in step (3), filtrate is measured in GC-MS and
Confirmation, determination condition are：SH-Rxi-5Sil MS capillary columns (30m × 0.25mm × 0.25 μm), injector temperature：250 DEG C,
Carrier gas：High-pure helium (He), purity>99.999%, column flow rate：1.69mL/min, chromatographic column post case temperature programming pattern：Initial temperature
50 DEG C of degree keeps 1min, rises to 150 DEG C with 25 DEG C/min rates, then rise to 300 DEG C with 10 DEG C/min, keeps 5min, sample introduction
Amount：1ul, input mode：Splitless injecting samples；Detector ionizes mode：EI, ion source temperature：230 DEG C, electron energy：70eV,
Transmission line temperature：300 DEG C, solvent delay time 1.5min, quantification of MRM scan patterns, tuning manner is automatic tuning, is used
Highly sensitive pattern.
The invention has the advantages that：
The present invention handles pedotheque using QuEChERS methods, has and is applicable in wide, efficient, easy to operate, solvent use
Measure the advantages such as small, the rate of recovery is high.The present invention is based on traditional QuEChERS methods of purification to propose novel QuEChERS/GC-MS detections
Method has the more stable rate of recovery, disclosure satisfy that the testing requirements of soil drug residue, and the present invention uses multi wall carbon
Nanotube, absorption property is similar with C18, and chemical stability is high, and large specific surface area, adsorption capacity are big, the suction for not only having GCB to have
The ability of attached pigment, but also there is certain impurity-eliminating effect.Multi-walled carbon nanotube, which is added, can reach good purification simultaneously
Effect can reach same even preferably clean-up effect, and plant compared with the combination of adsorbents of common PSA, GCB, C18
Class and the opposite reduction of dosage, can not only save analysis cost, and reduce the influence to the rate of recovery to a certain extent.
The present invention establishes QuEChERS- gas chromatography mass spectrometry methods and quickly measures the remaining method of Multiple Pesticides in soil.The party
The characteristics of method, is efficiently simple, greatly reduces amount of reagent compared to conventional pre-treating method, reduces the use of toxic organic solvent,
Not only reduced cost but also environmentally friendly, and improved the clean-up effect of extraction efficiency and matrix, realize it is quick, easy, accurate and
The requirement of analysis simultaneously.
Description of the drawings
Fig. 1 is the soil blank sample chromatogram of the embodiment of the present invention 1；
Fig. 2 is that the soil blank sample of the embodiment of the present invention 1 adds the chromatography of 131 kinds of pesticide standard solution (0.25mg/kg)
Figure；
Fig. 3 is that 131 kinds of pesticide soil matrixes of the embodiment of the present invention 1 match the chromatogram of standard solution (0.1mg/L).
Specific implementation mode
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.The person that is not specified actual conditions in embodiment, the item suggested according to normal condition or manufacturer
Part carries out.Reagents or instruments used without specified manufacturer is the conventional products that can be obtained by commercially available purchase.
The pedotheque of the use of the embodiment of the present invention is made by the following method：
It will be uniformly layered on brown paper from the collected pedotheque of the Pixian County towns the An De organic farm in West Lake island, by soil
In rubble, grass and various other sundries rejected.Then it allows soil after the local natural air drying of ventilation, uses mortar
Pedotheque is ground, is sieved again with 60 mesh sieve after crushing, it is for use that the soil after sieving is packed into valve bag.
The embodiment of the present invention is measured and confirms in GC-MS, and determination condition is：SH-Rxi-5SilMS capillary columns
(30m × 0.25mm × 0.25 μm), injector temperature：250 DEG C, carrier gas：High-pure helium (He), purity>99.999%, column flow rate：
1.69mL/min, chromatographic column post case temperature programming pattern：50 DEG C of initial temperature keeps 1min, 150 is risen to 25 DEG C/min rates
DEG C, then 300 DEG C are risen to 10 DEG C/min, keep 5min, sample size：1ul, input mode：Splitless injecting samples；Detector ionization side
Formula：EI, ion source temperature：230 DEG C, electron energy：70eV, transmission line temperature：It is 300 DEG C, solvent delay time 1.5min, quantitative
For MRM scan patterns, tuning manner is automatic tuning, using highly sensitive pattern.
Standard solution preparation includes the following steps：
131 kinds of pesticide standard sample solutions are accurately measured in 50mL volumetric flasks, with acetone constant volume, are made into the mixed of 1.0mg/L
Standardization storing solution, in -18 DEG C of storages.
The pedotheque of blank is taken, (1)-(3) carry out pre-treatment as steps described below.Solution is made after taking blank sample to handle
For matrix, hybrid standard storing solution is made into the matrix standard specimen of 0.1mg/L, for machine on GC-MS, in this, as quantified by external standard method.
Embodiment 1：
The remaining detection method of Multiple Pesticides in the soil of the present embodiment, including：
(1) deionized water is added into pedotheque to impregnate, impregnates 30min, glacial acetic acid-acetonitrile solution, nothing is then added
Water magnesium sulfate, sodium chloride and sodium acetate carry out being vortexed successively and centrifugal treating, vortex time 1min, centrifugal rotational speed are
8000r/min, centrifugation time 5min.The mass ratio 10 of glacial acetic acid-acetonitrile solution, anhydrous magnesium sulfate, sodium chloride and sodium acetate：
4：1：1.The volume ratio of a concentration of 1wt% of glacial acetic acid-acetonitrile solution, glacial acetic acid and acetonitrile is 1：99.
(2) supernatant of step (1) is taken, anhydrous magnesium sulfate and multi-walled carbon nanotube is added, is vortexed and is centrifuged successively
Processing, vortex time 1min, centrifugal rotational speed 8000r/min, centrifugation time 5min, supernatant, anhydrous magnesium sulfate and more
The mass ratio of wall carbon nano tube is 6：0.75：0.006.
(3) take the supernatant of step (2) in being concentrated in Rotary Evaporators, with mistake after n-hexane-acetone mixed solvent constant volume
Filter, is measured filtrate and confirms.The volume ratio of supernatant and n-hexane-acetone mixed solvent is 2：1.N-hexane-acetone
The volume ratio of in the mixed solvent, n-hexane and acetone is 9:1.The temperature of Rotary Evaporators is 40 DEG C.
Embodiment 2：
The remaining detection method of Multiple Pesticides in the soil of the present embodiment, including：
(1) deionized water is added into pedotheque to impregnate, impregnates 45min, glacial acetic acid-acetonitrile solution, nothing is then added
Water magnesium sulfate, sodium chloride and sodium acetate carry out being vortexed successively and centrifugal treating, vortex time 2min, centrifugal rotational speed are
8200r/min, centrifugation time 6min.The mass ratio 11 of glacial acetic acid-acetonitrile solution, anhydrous magnesium sulfate, sodium chloride and sodium acetate:
4.1:1.1:1.1.The volume ratio of a concentration of 1.2wt% of glacial acetic acid-acetonitrile solution, glacial acetic acid and acetonitrile is 1.2：98.8.
(2) supernatant of step (1) is taken, anhydrous magnesium sulfate and multi-walled carbon nanotube is added, is vortexed and is centrifuged successively
Processing, vortex time 2min, centrifugal rotational speed 8200r/min, centrifugation time 6min, supernatant, anhydrous magnesium sulfate and more
The mass ratio of wall carbon nano tube is 7：1：0.007.
(3) take the supernatant of step (2) in being concentrated in Rotary Evaporators, with mistake after n-hexane-acetone mixed solvent constant volume
Filter, is measured filtrate and confirms.The volume ratio of supernatant and n-hexane-acetone mixed solvent is 2.5：1.N-hexane-the third
The volume ratio of ketone in the mixed solvent, n-hexane and acetone is 8.8:1.2.The temperature of Rotary Evaporators is 45 DEG C.
Embodiment 3：
The remaining detection method of Multiple Pesticides in the soil of the present embodiment, including：
(1) deionized water is added into pedotheque to impregnate, impregnates 40min, glacial acetic acid-acetonitrile solution, nothing is then added
Water magnesium sulfate, sodium chloride and sodium acetate carry out being vortexed successively and centrifugal treating, vortex time 1.5min, centrifugal rotational speed are
7800r/min, centrifugation time 4min.The mass ratio 9 of glacial acetic acid-acetonitrile solution, anhydrous magnesium sulfate, sodium chloride and sodium acetate:
3.9:0.9:0.9.The volume ratio of a concentration of 0.8wt% of glacial acetic acid-acetonitrile solution, glacial acetic acid and acetonitrile is 0.8：99.2.
(2) supernatant of step (1) is taken, anhydrous magnesium sulfate and multi-walled carbon nanotube is added, is vortexed and is centrifuged successively
Processing, vortex time 1.5min, centrifugal rotational speed 7800r/min, centrifugation time 4min, supernatant, anhydrous magnesium sulfate and
The mass ratio of multi-walled carbon nanotube is 5：0.5：0.005.
(3) take the supernatant of step (2) in being concentrated in Rotary Evaporators, with mistake after n-hexane-acetone mixed solvent constant volume
Filter, is measured filtrate and confirms.The volume ratio of supernatant and n-hexane-acetone mixed solvent is 1.5：1.N-hexane-the third
The volume ratio of ketone in the mixed solvent, n-hexane and acetone is 9.2:0.8.The temperature of Rotary Evaporators is 35 DEG C.
By taking the test result of above-described embodiment 1 as an example, Fig. 1 is soil blank sample chromatogram, and Fig. 2 is soil blank sample
Add the chromatogram of pesticide standard solution.
It adds a certain amount of pesticide standard solution respectively in blank sample, makes a concentration of 0.25mg/kg of addition, according to upper
The detecting step and chromatographic condition for stating embodiment 1 are measured, and addition concentration repeats experiment 6 times, show that the average of pesticide returns
Yield and relative standard deviation, are shown in Table 1.
1 rate of recovery of table and precision
From table 1 it follows that mark-on pesticide to be determined shares 131 kinds of pesticides, wherein 9 kinds of pesticide rate of recovery are relatively low, a kind
The pesticide rate of recovery is higher.Relatively low pesticide has clofentezine, acephatemet, orthene, omethoate, Azodrin, Bravo, antibacterial
Spirit, cyprodinil, Resistox；Higher pesticide is fenhexamid；Remaining pesticide rate of recovery within the allowable range, and is tested
The relative standard deviation of gained is between 0.22%~12.65%.
From the point of view of the blank of Fig. 1 and Fig. 2's plus 131 kinds of pesticide standard liquid chromatogram comparison, 131 kinds of agricultures in mark-on spectrogram
Medicine can be detached preferably, illustrate that chromatographic condition has obtained preferable optimization.Blank spectrogram shows to be baseline, shows blank
It is the pesticide without being measured in sample.From the point of view of Fig. 2 matches standard solution comparison with 131 kinds of pesticide soil matrixes of Fig. 3, they
Peak shape and appearance time be all identical, show the present invention detection method be it is accurate and stablize.
In conclusion the detection method accuracy of the present invention is high, stability is good, the rate of recovery and reproducibility can meet quantitatively
The requirement of analysis also meets a kind of detection of Multiple Pesticides in soil, and is not necessarily to special installation, at low cost, organic reagent simultaneously
Dosage is few, is a kind of simple, quick and environmentally friendly method.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (10)
1. the remaining detection method of Multiple Pesticides in a kind of soil, which is characterized in that including：
(1) deionized water is added into pedotheque to impregnate, glacial acetic acid-acetonitrile solution, anhydrous magnesium sulfate, sodium chloride is then added
And sodium acetate, vortex and centrifugal treating are carried out successively；
(2) supernatant of step (1) is taken, anhydrous magnesium sulfate and multi-walled carbon nanotube is added, carries out vortex and centrifugal treating successively；
(3) take the supernatant of step (2) in being concentrated in Rotary Evaporators, it is right with being filtered after n-hexane-acetone mixed solvent constant volume
Filtrate is measured and confirms.
2. the remaining detection method of Multiple Pesticides in soil according to claim 1, which is characterized in that in step (1),
The volume ratio of a concentration of 0.8-1.2wt% of glacial acetic acid-acetonitrile solution, glacial acetic acid and acetonitrile is (0.8-1.2)：(98.8-
99.2)。
3. the remaining detection method of Multiple Pesticides in soil according to claim 2, which is characterized in that in step (1),
The mass ratio (9-11) of glacial acetic acid-acetonitrile solution, anhydrous magnesium sulfate, sodium chloride and sodium acetate：(3.9~4.1)：(0.9-1.1)：
(0.9-1.1)。
4. the remaining detection method of Multiple Pesticides in soil according to claim 3, which is characterized in that in step (1),
Vortex time is 1-2min, centrifugal rotational speed 7800-8200r/min, centrifugation time 4-6min.
5. the remaining detection method of Multiple Pesticides in soil according to claim 1, which is characterized in that in step (2),
The mass ratio of supernatant, anhydrous magnesium sulfate and multi-walled carbon nanotube is (5-7)：(0.5-1)：(0.005-0.007).
6. the remaining detection method of Multiple Pesticides in soil according to claim 5, which is characterized in that in step (2),
Vortex time is 1-2min, centrifugal rotational speed 7800-8200r/min, centrifugation time 4-6min.
7. the remaining detection method of Multiple Pesticides in soil according to claim 1, which is characterized in that in step (3),
The volume ratio of supernatant and n-hexane-acetone mixed solvent is (1.5-2.5)：1.
8. the remaining detection method of Multiple Pesticides in soil according to claim 7, which is characterized in that n-hexane-acetone
The volume ratio of in the mixed solvent, n-hexane and acetone is (8.8-9.2)：(0.8-1.2).
9. the remaining detection method of Multiple Pesticides in soil according to claim 8, which is characterized in that Rotary Evaporators
Temperature is 35-45 DEG C.
10. the remaining detection method of Multiple Pesticides in soil according to claim 9, which is characterized in that in step (3)
In, filtrate is measured and is confirmed in GC-MS, determination condition is：SH-Rxi-5Sil MS capillary columns, 30m ×
0.25mm × 0.25 μm, injector temperature：250 DEG C, carrier gas：High-pure helium, purity>99.999%, column flow rate：1.69mL/min
Chromatographic column post case temperature programming pattern：50 DEG C of initial temperature keeps 1min, rises to 150 DEG C with 25 DEG C/min rates, then with 10
DEG C/min rises to 300 DEG C, keep 5min, sample size：1ul, input mode：Splitless injecting samples；Detector ionizes mode：EI, from
Source temperature：230 DEG C, electron energy：70eV, transmission line temperature：300 DEG C, solvent delay time 1.5min, quantification of MRM are swept
Pattern is retouched, tuning manner is automatic tuning, using highly sensitive pattern.
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| CN109239174A (en) * | 2018-09-30 | 2019-01-18 | 广西乐业康辉生态养殖专业合作社 | A kind of Fast Determination of Pesticide Residue method of organic agricultural products |
| CN113238064A (en) * | 2021-04-16 | 2021-08-10 | 中国人民解放军总医院第三医学中心 | Application of full-automatic biochemical analyzer in chemical poisoning serum sample detection |
| CN113325119A (en) * | 2021-06-11 | 2021-08-31 | 中国热带农业科学院南亚热带作物研究所 | Pesticide residue sample pretreatment concentration method |
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