CN103604880A - Method for detecting triazophos pesticide in environmental samples of different types - Google Patents
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Abstract
The invention relates to a method for detecting a triazophos pesticide in environmental samples of different types. The method comprises the following steps: (1), preparing a triazophos standard solution, carrying out high performance liquid chromatography detection, quantitatively measuring the concentration of the standard solution by adopting an external standard peak area method, and making a linear regression curve of a chromatographic peak area to the triazophos concentration; (2), preprocessing the environmental samples of different types, namely extracting triazophos and carrying out solid-phase extraction; and (3), carrying out high performance liquid chromatography detection on the processed samples obtained in the step (2), thus obtaining the concentration of the triazophos in the samples by combining the linear regression curve obtained in the step (1). Compared with the prior art, the method has the advantages of convenience and accuracy in operation, stability and reliability, high recovery rate, less consumption of an organic solvent in a preprocessing process, little secondary pollution to the environment, and the like.
Description
Technical field
The present invention relates to a kind of detection method of persticide residue, especially relate to the detection method of Hostathion agricultural chemicals in a kind of dissimilar environmental sample.
Background technology
Along with the growing interest of people to environmental protection and self health, the high malicious high residue organophosphorus pesticide of part is successively disabled, and the middle low-toxin farm chemicals that Hostathion is recommended as China Ministry of Agriculture, has started to be widely used in agricultural production.Hostathion (Triazophos, TAP), a kind of efficient, poisoning, the broad spectrum organic phosphorus insecticidal/acaricidal agent of the exploitation of 20 century 70 Germany Hoechst companies, it agricultural pests (mite) are had tag, stomach poison function, have concurrently in certain and ooze effect, be applicable to prevent and treat the insect pest in paddy rice, cotton, corn, beans, vegetables, in aquaculture, also adopt in addition Hostathion sterilization and eliminate harmful animal.In China, produce and long-term use because Hostathion agricultural chemicals is a large amount of, the residual quantity in some areas water body, soil, plant surpasses national safety standard equally, and environment, biology and health are constituted a serious threat.Therefore, set up the analytical approach of Hostathion residues of pesticides in the surrounding medium of efficiently and accurately, be significant.
For Triazophos residue, detect, Liu Shuzhao etc. once invention Hostathion competitive ELISA absorption method for the fast detecting of Triazophos residue in agricultural product and environment.Immunoassay has high specificity, highly sensitive, fast and easy, analysis capacity is large, analysis cost is low, the advantage such as safe and reliable.But also there is certain limitation in sufficient immunoassay, as: the coefficient of variation is large, needs the post of disposable dress film, and antibody and enzyme target haptens use amount are large, once can only detect a sample; Performance history need to drop into more fund and time, obtains high-quality antigen more difficult, high to the selectivity of reagent, is difficult to analyze Multiple components simultaneously, and the similar compound of structure is had to cross reaction to a certain degree etc.Instrumental method is one of technology classical, the most the most frequently used in Detecting Pesticide, has the advantages such as highly sensitive, accuracy is good.The instrumental analysis process of residues of pesticides is for extracting-purify-detection at present.Because Triazophos residue amount in surrounding medium is low and extract components is too complicated, in sample, Hostathion need to pass through the pretreatment process such as extraction, enrichment and purification and just can detect.Compare with traditional liquid-liquid extraction, solid phase extraction techniques have easy and simple to handle fast, consumption of organic solvent is few, can effectively remove impurity, to object recovery advantages of higher.
Summary of the invention
Object of the present invention is exactly that the detection method of Hostathion agricultural chemicals in a kind of dissimilar environmental sample is provided in order to overcome the defect of above-mentioned prior art existence.
The present invention is directed to water sample, plant sample and matrix sample in the artificial swamp that adds Hostathion agricultural chemicals, adopt Solid-Phase Extraction (SPE) pretreatment technology, by operation conditions optimization, significantly improved the recovery of Hostathion in three kinds of a little media of main environment of artificial swamp.Because high performance liquid chromatography has high score from advantages such as, high sensitivity compared with vapor-phase chromatography, the present invention adopts high performance liquid chromatography (HPLC) to detect through the Hostathion residues of pesticides in pretreatment sample.
Object of the present invention can be achieved through the following technical solutions:
A detection method for Hostathion agricultural chemicals in dissimilar environmental sample, the method comprises the following steps:
(1) configuration Hostathion standard solution, carries out high performance liquid chromatography detection, adopts the concentration of external standard peak area method quantitative measurement standard solution, with chromatographic peak area, Hostathion concentration is done to linear regression curve;
(2) dissimilar environmental sample is carried out to pre-treatment, pre-treatment comprises extraction and the Solid-Phase Extraction of Hostathion;
(3) sample after step (2) is processed carries out high performance liquid chromatography detection, and the linear regression curve of integrating step (1) gained, obtains the concentration of Hostathion in sample.
Described dissimilar environmental sample comprises artificial swamp water sample, plant sample and artificial swamp matrix sample;
Pre-treating method for water sample is as follows:
Water sample is crossed the filter membrane of 0.45 μ m, filters water sample continuously by SPE post, and flow velocity is by regulating the vacuum tightness of extraction equipment to control as 3-5mL/min; After water sample all passes through, with ultrapure water, rinse SPE column wall, then with the suction of air-flow continuation stably 10 minutes; Finally, with eluant, eluent wash-out at twice, collect eluent as the test liquid of liquid chromatography;
Pre-treating method to plant sample is as follows:
Get constructed wetland plant sample, pure water is cleaned, and root, stem, leaf are evenly pulverized after freeze drying respectively, add extraction solvent, and ultrasonication, standing, incline and supernatant; Add again extraction solvent, ultrasonication, filtration, filtrate merges the supernatant that inclines before to and revolves steams near doing, and then gets extract extraction constant volume; Finally extract is crossed to SPE post, and with eluant, eluent wash-out at twice, collected eluent as the test liquid of liquid chromatography;
Pre-treating method to artificial swamp matrix sample is as follows:
Get more than artificial swamp 3 places matrix haydite and mix, after natural air drying, remove impurity, haydite is pulverized, cross 100 mesh sieves, add after extracting solvent and vibrate in constant temperature oscillator, and ultrasonication, standing, incline and supernatant; Add again extraction solvent, ultrasonication, filtration, filtrate merges the supernatant that inclines before to and revolves steams near doing, and then gets extract extraction constant volume; Finally extract is crossed to SPE post, and with eluant, eluent wash-out at twice, collected eluent as the test liquid of liquid chromatography.
Further, described eluant, eluent is selected from methyl alcohol, ethyl acetate, acetone or acetonitrile; Described extraction solvent is selected from acetonitrile, ethyl acetate or methylene chloride; Described extract is methyl alcohol.
Further, described eluant, eluent is acetonitrile, and described extraction solvent is methylene chloride.
Described SPE post activates before using, and concrete grammar is: before using, 5mL ethyl acetate and 5mL methyl alcohol are passed through to SPE post successively lentamente, wash away interference impurity, then use 2 drip washing SPE posts of the ultrapure moisture of 10mL.
In following ratio proportioning, feed in raw material: described water sample sampling 200ml, described constructed wetland plant sample samples 0.50g after pulverizing, described haydite pulverizes and sieves rear sampling 5.0g, the total amount of described extraction solvent is 50ml, add 25ml at every turn, described extract adds 5ml, and the amount of described eluant, eluent is 5ml.
The condition of carrying out high performance liquid chromatography detection in step (1) and step (3) is as follows:
Chromatographic column: internal diameter 250mm * 4.6mm, stainless steel chromatogram post, interior filling AlltechApollo C185um filler;
Mobile phase: the potpourri of methyl alcohol and water, wherein, the volume ratio of methyl alcohol and water is 80:20;
Flow velocity: 1.0mL/min;
Column temperature: 30 ℃;
Detect wavelength: 246nm;
Sample size: 10 μ L.
In step (1), the concentration of the Hostathion standard solution of configuration is respectively 0.5mg/L, 1mg/L, 2mg/L, 4mg/L, 6mg/L and 8mg/L.
Compared with prior art, the present invention adopts Solid-Phase Extraction-high performance liquid chromatography, and after Solid-Phase Extraction, the Hostathion in sample is separated good in chromatographic column, and non-target analytes can be by effectively washing removal, and target analytes obtains highly purified.High efficiency liquid phase method is simple to operate, and detection limit can reach 1.7 μ g/L.The average recovery of standard addition of the inventive method mark-on actual sample detection display water sample, constructed wetland plant sample (canna), haydite is respectively 95.7% ± 4.7%, 88.8% ± 8.1%, 86.5% ± 7.2%, can promote the use of the detection of Hostathion residues of pesticides in other surrounding mediums.
Meanwhile, the present invention have easy to operate, accurate, reliable and stable, the recovery is high, in pretreatment process organic solvent use less, to advantages such as the secondary pollution of environment are few.
Accompanying drawing explanation
Fig. 1 is the chromatogram of Hostathion standard model;
Fig. 2 is that in surrounding medium, Hostathion agricultural chemicals passes through eluent ethyl acetate chromatogram;
Fig. 3 is that in surrounding medium, Hostathion agricultural chemicals passes through acetonitrile elution chromatography figure;
Fig. 4 is that eluant, eluent volume affects figure to the Hostathion recovery;
Fig. 5 was that SPE post volume of water sample affects figure to the Hostathion recovery;
Fig. 6 is Hostathion canonical plotting.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The instrument using in following examples, reagent and sample are as follows:
Instrument
Agilent1200 type high performance liquid chromatograph (Agilent Technologies, the U.S.), has diode array and detects; 250mm x4.6mm (i, d) stainless steel chromatogram post, interior filling AlltechApollo C185um filler; KQ-200VDV type ultrasonic cleaner (Kunshan ultrasonic instrument company limited); The multiplex vacuum pump of SHB-IIIA circulating water type (Shanghai Yu Kang Science & Teaching Instrument equipment company limited); RE-3000A type Rotary Evaporators (Shanghai Yarong Biochemical Instrument Plant); High speed Universalpulverizer (Tianjin Stettlen Instrument Ltd.); Constant temperature oscillator (Shanghai Yiheng Scientific Instruments Co., Ltd); Germany's CHRIST freeze drier (Beijing Shanghai branch office of Bo Maihang Instrument Ltd.); U.S. Supelco12 manages anti-cross staining solid-phase extraction device and people's capacity sampling pipe, and GM-0.33A is without oily vacuum diaphragm pump, CNWBOND LC-C18SPE pillar (Town in Shanghai spectrum scientific instrument company limited).
Reagent and medicine
Hostathion standard model purity >=98.5%; 85% triazophos emulsifiable solution (chemical reagent company limited of Shanghai Johnson & Johnson provides); Ultrapure water; Methyl alcohol is chromatographically pure, and ethyl acetate, acetone, acetonitrile, methylene chloride are for analyzing pure (Shanghai traditional Chinese medicines reagent provides).The chromatogram of Hostathion standard model as shown in Figure 1.
Standard solution configuration
Accurately take 0.0508g Hostathion (98.5%) standard items and in 100mL volumetric flask, with methyl alcohol, dissolve and be diluted to scale, shake up.Compound concentration is the storing solution of 50mg/L, and precision pipettes appropriate storing solution respectively, and with methyl alcohol stepwise dilution, becoming concentration is the Hostathion standard solution of 0.5mg/L, 1mg/L, 2mg/L, 4mg/L, 6mg/1,8mg/L.
Sample preparation
Quadruplet horizontal drowned flow artificial wet land small testing device is positioned at Tongji University experiment greenhouse, water inlet Hostathion agricultural chemicals (be 0,0.1,1,5mg/L, hydraulic load is 100mm/d.Constructed wetland plant is that (planting density is 20 strains/m to canna (Canna indica)
2), wet land filler is the haydite of 3-5mm particle diameter.
Water sample: 500mL water sample is got in artificial wetland effluent district, water sample, through the filter membrane of 0.45 μ m, is collected filtrate and is stored in reefer standby.
Plant sample: get each strain pure water of canna of holding before, during and after artificial swamp and clean, root, stem, leaf are evenly pulverized after freeze drying respectively, are stored in reefer standby.
Matrix sample: get constructed wetland plant root district haydite 500g and be placed in fuming cupboard natural air drying, remove the impurity such as root system, haydite is pulverized, cross 100 mesh sieves, be stored in reefer standby.
Sample pre-treatments
Water sample: get 200mL water sample continuously by SPE pillar, flow velocity is by regulating the vacuum tightness of extraction equipment to control as 3-5mL/min; After water sample all passes through, with 5mL ultrapure water, rinse the little column wall of SPE, then with the suction of air-flow continuation stably 10 minutes; Finally use 5mL acetonitrile wash-out at twice, collect eluent as the test liquid of liquid chromatography.
Plant sample: get the triangular flask that the canna 0.5000g (being accurate to 0.0002g) preparing is placed in 150mL, add 25mL methylene chloride, ultrasonication 20min, standing, incline and supernatant; Add 25mL methylene chloride, ultrasonication 20min, filters again, and the supernatant that leans forward out filtrate merging revolves and steams near doing, and then gets 5mL methanol extraction constant volume; Finally extract is crossed to SPE post, and with 5mL acetonitrile wash-out at twice, collected eluent as the test liquid of liquid chromatography.
Matrix sample: get the triangular flask that the haydite 5.00g (being accurate to 0.02g) preparing is placed in 150mL, add the 30min that vibrates in 25mL methylene chloride constant temperature oscillator, subsequent processes is with canna sample.
One, determine Operating parameters
1, extract the selection of solvent
Extraction solvent for plant and matrix residues of organophosphate pesticides mainly contains acetonitrile, ethyl acetate, acetone and methylene chloride etc.Acetone and water are miscible, not easily separated.Comparative analysis of the present invention acetonitrile, ethyl acetate and the methylene chloride percentage extraction (in Table 1) to Hostathion residues of pesticides in canna.Result shows, the percentage extraction of methylene chloride is significantly higher than acetonitrile and ethyl acetate, and percentage extraction is 90.7%, and standard deviation is 7.3%, therefore selects methylene chloride as preferred extractant.
Table 1 extracts the impact of solvent on Hostathion extraction ratio
2, SPE post activation
Before using, 5 mL ethyl acetate and 5mL methyl alcohol are passed through to SPE post successively lentamente, with moistening, activation, balance filler, wash away interference impurity,, then use 2 drip washing pillars of the ultrapure moisture of 10 mL.
3, eluant, eluent is selected
Eluant, eluent is the key factor of impact analysis thing SPE wash-out behavior.The present embodiment is analyzed the impact of four kinds of opposed polarity eluant, eluents such as methyl alcohol, ethyl acetate, acetone, acetonitrile on the Hostathion SPE recovery, show that the eluant, eluent that the recovery is relatively high is ethyl acetate (95.6%-101.3%) and acetonitrile (93.2%-97.5%).But in conjunction with chromatogram, on eluent ethyl acetate chromatogram, eluant, eluent goes out peak before object, and peak area very people covered the peak (Fig. 2) of object; In acetonitrile elution chromatography figure (Fig. 3), eluant, eluent goes out peak after object, and object detachment process and peak spectrum are not produced and disturbed.It is preferred eluant, eluent that sample preparation therefore of the present invention is selected acetonitrile.
4, eluant, eluent volume is selected
Fig. 4 is shown in the impact that eluant, eluent volume detects the recovery to Hostathion.When the volume of eluant, eluent is less than 5 mL, the recovery obviously improves with the increase of eluant, eluent volume; And when the volume of eluant, eluent is greater than 5 mL to 10 mL, the recovery is along with the increase of eluant, eluent volume does not have much variations substantially.Therefore to select effluent volume be 5 mL to sample preparation of the present invention, and wash-out at twice, and then obtain the higher recovery.
5, crossing SPE post volume of water sample selects
In environment water, Hostathion residues of pesticides are very low, and liquid phase peak spectrum is very little even not to be had, and are difficult for detecting, and need very high enrichment times just can detect.In order to be applicable to Hostathion analysis in surrounding medium, need to select suitable processing volume.The artificial swamp Inlet and outlet water that adds Hostathion operation of take is water sample, and 100mL is initial volume, and every increase by 50 mL process once, measure the recovery, until 250 mL cross post volume of water sample on the impact of the Hostathion recovery as shown in Figure 5.Result shows, when crossing column volume and being 200 mL, average recovery rate is the highest, is 97.5%.Therefore,, in order to obtain larger enrichment times, it is 200 mL that the present invention selected post volume of water sample.
6, chromatography condition
Mobile phase, methyl alcohol+ultrapure water=80+20 (V+V); Flow 1.0 mL/min; 30 ℃ of column temperatures; Detect wavelength 246nm; Sample size 10uL.
Two, sample is measured
1, the typical curve of Hostathion
Configuration concentration is the Hostathion standard solution of 0.5mg/L, 1mg/L, 2mg/L, 4mg/L, 6mg/1,8mg/L, under above-mentioned chromatographic condition, adopts the quantitative measurement of external standard peak area method.With chromatographic peak area (X), Hostathion concentration (Y) is done to linear regression curve, as shown in Figure 6.Equation of linear regression is Y=0.04381*X-0.03008 (R
2=0.9999).According to detecting of calculation by extrapolation the method, be limited to 1.7 μ g/L.
2, instrument and method stability
The present invention adopts pre-treating method that above-mentioned optimization selects to the water sample content replication 5 times (in Table 2) containing Hostathion residues of pesticides, and result shows, the method detects and meets national residues of pesticides trace analysis requirement.
Table 2 apparatus suitability test result
3, recovery experiment
The samples such as water sample, canna and haydite are carried out to mark-on and reclaim detection test, calculate the average recovery rate of 3 results, list in table 3, table 4, table 5.Result shows that the average recovery of standard addition of water sample is that 95.7% (± 4.7%), the average recovery of standard addition of canna are that 88.8% (± 8.1%), the average recovery of standard addition of haydite are 86.5% (± 7.2%).
Table 3 water sample recovery test result (n=3)
Table 4 canna sample recovery test result (n=3)
Table 5 haydite sample recovery test result (n=3)
4, sample determination
Get Hostathion and add water outlet water sample, canna and the haydite sample that concentration is the artificial swamp of 0.1mg/L, carry out high performance liquid chromatography detection, and in conjunction with linear regression curve, result shows that in water outlet water sample, Hostathion concentration is 6 μ g/L; In India Canna Rhizome cauline leaf, Hostathion average content is 0.12mg/kg; Hostathion amount 0.114mg/kg in haydite.
Embodiment 2
A detection method for Hostathion agricultural chemicals in dissimilar environmental sample, the method comprises the following steps:
(1) configuration concentration is respectively the Hostathion standard solution of 0.5mg/L, 1mg/L, 2mg/L, 4mg/L, 6mg/L and 8mg/L, carry out high performance liquid chromatography detection, adopt the concentration of external standard peak area method quantitative measurement standard solution, with chromatographic peak area, Hostathion concentration is done to linear regression curve, as shown in Figure 6, equation of linear regression is Y=0.04381*X-0.03008 (R
2=0.9999).
(2) dissimilar environmental sample is carried out to pre-treatment, pre-treatment comprises extraction and the Solid-Phase Extraction of Hostathion:
Pre-treating method for water sample is as follows:
Water sample is crossed the filter membrane of 0.45 μ m, filtration water sample is continuously by SPE post, and SPE post activates before using, and concrete grammar is: before using, 5mL ethyl acetate and 5mL methyl alcohol are passed through to SPE post successively lentamente, wash away interference impurity, then use 2 drip washing SPE posts of the ultrapure moisture of 10mL.Flow velocity is by regulating the vacuum tightness of extraction equipment to control as 3-5mL/min; After water sample all passes through, with ultrapure water, rinse SPE column wall, then with the suction of air-flow continuation stably 10 minutes; Finally use eluant, eluent (being acetonitrile in the present embodiment) wash-out at twice, collect eluent as the test liquid of liquid chromatography;
Pre-treating method to plant sample is as follows:
Get constructed wetland plant sample (canna three strains), pure water is cleaned, root, stem, leaf are evenly pulverized after freeze drying respectively, and add and extract solvent (being methylene chloride in the present embodiment), and ultrasonication, standing, incline and supernatant: add extraction solvent, ultrasonication, filters again, filtrate merges the supernatant that inclines before to and revolves steams near doing, and then gets extract extraction constant volume; Finally extract (being methyl alcohol in the present embodiment) is crossed to SPE post, and with eluant, eluent wash-out at twice, collected eluent as the test liquid of liquid chromatography;
Pre-treating method to artificial swamp matrix sample is as follows:
Get more than artificial swamp 3 places matrix haydite and mix, after natural air drying, remove the impurity such as root system, haydite is pulverized, cross 100 mesh sieves, add after extracting solvent and vibrate in constant temperature oscillator, and ultrasonication, standing, incline and supernatant; Add again extraction solvent, ultrasonication, filtration, filtrate merges the supernatant that inclines before to and revolves steams near doing, and then gets extract extraction constant volume; Finally extract is crossed to SPE post, and with eluant, eluent wash-out at twice, collected eluent as the test liquid of liquid chromatography.
The feed ratio of each material is closed: water sample sampling 200ml, constructed wetland plant sample pulverize after sampling 0.50g, haydite pulverizes and sieves rear sampling 5.0g, the total amount of extraction solvent is 50ml, adds 25ml at every turn, extract adds 5ml, the amount of eluant, eluent is 5ml.
(3) sample after step (2) is processed carries out high performance liquid chromatography detection, and the linear regression curve of integrating step (1) gained, obtains the concentration of Hostathion in sample.
The condition of carrying out high performance liquid chromatography detection in step (1) and step (3) is as follows:
Chromatographic column: internal diameter 250mm * 4.6mm, stainless steel chromatogram post, interior filling AlltechApollo C185um filler; Mobile phase: the potpourri of methyl alcohol and water, wherein, the volume ratio of methyl alcohol and water is 80:20; Flow velocity: 1.0mL/min; Column temperature: 30 ℃; Detect wavelength: 246nm; Sample size: 10 μ L.
Claims (7)
1. a detection method for Hostathion agricultural chemicals in dissimilar environmental sample, is characterized in that, the method comprises the following steps:
(1) configuration Hostathion standard solution, carries out high performance liquid chromatography detection, adopts the concentration of external standard peak area method quantitative measurement standard solution, with chromatographic peak area, Hostathion concentration is done to linear regression curve;
(2) dissimilar environmental sample is carried out to pre-treatment, pre-treatment comprises extraction and the Solid-Phase Extraction of Hostathion;
(3) sample after step (2) is processed carries out high performance liquid chromatography detection, and the linear regression curve of integrating step (1) gained, obtains the concentration of Hostathion in sample.
2. the detection method of Hostathion agricultural chemicals in a kind of dissimilar environmental sample according to claim 1, is characterized in that, described dissimilar environmental sample comprises artificial swamp water sample, plant sample and artificial swamp matrix sample;
Pre-treating method for water sample is as follows:
Water sample is crossed the filter membrane of 0.45 μ m, filters water sample continuously by SPE post, and flow control is 3-5mL/min; After water sample all passes through, with ultrapure water, rinse SPE column wall, then with the suction of air-flow continuation stably 10 minutes; Finally, with eluant, eluent wash-out at twice, collect eluent as the test liquid of liquid chromatography;
Pre-treating method to plant sample is as follows:
Get constructed wetland plant sample, pure water is cleaned, and root, stem, leaf are evenly pulverized after freeze drying respectively, add extraction solvent, and ultrasonication, standing, incline and supernatant; Add again extraction solvent, ultrasonication, filtration, filtrate merges the supernatant that inclines before to and revolves steams near doing, and then gets extract extraction constant volume; Finally extract is crossed to SPE post, and with eluant, eluent wash-out at twice, collected eluent as the test liquid of liquid chromatography;
Pre-treating method to artificial swamp matrix sample is as follows:
Get more than artificial swamp 3 places matrix haydite and mix, after natural air drying, remove impurity, haydite is pulverized, cross 100 mesh sieves, add after extracting solvent and vibrate in constant temperature oscillator, and ultrasonication, standing, incline and supernatant; Add again extraction solvent, ultrasonication, filtration, filtrate merges the supernatant that inclines before to and revolves steams near doing, and then gets extract extraction constant volume; Finally extract is crossed to SPE post, and with eluant, eluent wash-out at twice, collected eluent as the test liquid of liquid chromatography.
3. the detection method of Hostathion agricultural chemicals in a kind of dissimilar environmental sample according to claim 2, is characterized in that, described eluant, eluent is selected from methyl alcohol, ethyl acetate, acetone or acetonitrile; Described extraction solvent is selected from acetonitrile, ethyl acetate or methylene chloride; Described extract is methyl alcohol.
4. the detection method of Hostathion agricultural chemicals in a kind of dissimilar environmental sample according to claim 3, is characterized in that, described eluant, eluent is acetonitrile, and described extraction solvent is methylene chloride.
5. the detection method of Hostathion agricultural chemicals in a kind of dissimilar environmental sample according to claim 2, it is characterized in that, described SPE post activates before using, concrete grammar is: before using, 5mL ethyl acetate and 5mL methyl alcohol are passed through to SPE post successively lentamente, wash away interference impurity, then use 2 drip washing SPE posts of the ultrapure moisture of 10mL.
6. the detection method of Hostathion agricultural chemicals in a kind of dissimilar environmental sample according to claim 2, it is characterized in that, in following ratio proportioning, feed in raw material: described water sample sampling 200ml, described constructed wetland plant sample samples 0.50g after pulverizing, described haydite pulverizes and sieves rear sampling 5.0g, and the total amount of described extraction solvent is 50ml, adds 25ml at every turn, described extract adds 5ml, and the amount of described eluant, eluent is 5ml.
7. the detection method of Hostathion agricultural chemicals in a kind of dissimilar environmental sample according to claim 1, is characterized in that, the condition of carrying out high performance liquid chromatography detection in step (1) and step (3) is as follows:
Chromatographic column: internal diameter 250mm * 4.6mm, stainless steel chromatogram post, interior filling Alltech Apollo C185um filler;
Mobile phase: the potpourri of methyl alcohol and water, wherein, the volume ratio of methyl alcohol and water is 80:20;
Flow velocity: 2.0mL/mim
Column temperature: 30 ℃;
Detect wavelength: 246nm;
Sample introduction is dizzy: 10 μ L.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115796366A (en) * | 2022-12-02 | 2023-03-14 | 同济大学 | Forest pest prediction method and forest pest prediction map system |
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