CN108287203A - A kind of ultrasonic wave and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues method - Google Patents
A kind of ultrasonic wave and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues method Download PDFInfo
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- CN108287203A CN108287203A CN201711326775.8A CN201711326775A CN108287203A CN 108287203 A CN108287203 A CN 108287203A CN 201711326775 A CN201711326775 A CN 201711326775A CN 108287203 A CN108287203 A CN 108287203A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of ultrasonic waves and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues method, include the following steps, S1, sampling, S2, sample blending processing, S3 extract, saltout, S4 shakes batch mixing, S5, the primary extraction of ultrasound, S6, ultrasonic second extraction, S7, primary concentration, purification, S8, secondary concentration, purification, S9 make determinand, S10 is measured, this method have many advantages, such as it is qualitative accurately, it is high sensitivity, easy to operate.This experiment has also carried out the chromatographic behavior research of DDT and its metabolin on nonpolar chromatographic column HP 5, substantially increases accuracy.
Description
Technical field
The present invention relates to Agricultural Soil Environments to detect correlative technology field, specially a kind of ultrasonic wave and gas-chromatography knot
It closes and measures agricultural land soil Organochlorine Pesticide Residues method.
Background technology
Six six six (BHCs) and DDT (DDTs) are organo-chlorine pesticide (OCPs), are representative lasting organic contaminations
Object (POPs), due to its good disinsection effect and lasting medicine, once extensive use in the world.Though in China already in 80
Age part disables, but since organo-chlorine pesticide has half volatile and high persistence, can for a long time exist in atmospheric environment,
And [3] are propagated by distillation effect over long distances, it finally falls in soil, therefore densely populated area is it is still necessary to research
Its pollution situation.Pearl River Delta area was once a large amount of territory of use of organo-chlorine pesticide, in recent years studies have shown that soil in the area
Earth can still detect Organochlorine Pesticide Residues, therefore the organochlorine contamination situation in agricultural land soil can not be ignored.
China has worked out OPCs assay methods standard in soil at present《Six six six and drop in GB/T 14550-2003 soil
The gas chromatography that DDT measures》, pre-treatment extracting method is Soxhlet extraction in the standard, and extraction side common at present
Method also has accelerated solvent extraction and microwave abstracting etc., but these methods, in the presence of time-consuming, solvent-oil ratio is big, such as above-mentioned GB/
T14550 Extraction solvent amounts be 110mL, need to there is special messenger to keep an eye on, and need using special equipment the shortcomings of.
Pre-treatment purification method is concentrated sulfuric acid cleanup method or the chromatographic column method of purification in national standard, the former uses the concentrated sulfuric acid, operation
There is larger danger；The latter need to voluntarily fill chromatographic column before experiment, and production method is cumbersome.For this purpose, proposing a kind of ultrasonic wave
With gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues method.
Invention content
The purpose of the present invention is to provide a kind of ultrasonic wave and gas-chromatography binding assay agricultural land soil organo-chlorine pesticide are residual
Method is stayed, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides the following technical solutions：
A kind of ultrasonic wave and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues method, include the following steps：
S1, sampling：The soil sample for taking the topsoil soils and topsoil of depth about 15cm or less (15-30) cm, by soil profile layer
Secondary clearing samples, and on each sampled point, soil is cut vertically downward by layer, and each point takes the soil of thickness about 10cm, and every
The soil amount taken on a point is equal, is uniformly mixed the soil sample of each point after sampling, then pedotheque is placed on interior
Ventilation after natural air drying, is ground soil using grinder, and crosses 80 mesh sieve；
S2, sample blending processing：50mL centrifuge tubes are placed on electronic balance, are weighed the soil sample 20.0g obtained in S1 and are used
In subsequent analysis, 5.O0mL deionized waters are measured using liquid-transfering gun, is added in 50mL centrifuge tubes, is rocked 1 minute, shake manually
It is even；
S3 extracts, saltouts：Using one division pipette, measures 20mL acetonitriles and above-mentioned 50mL is added as extractant
In centrifuge tube, then, measuring sodium chloride 5-7g with electronic balance, (sodium chloride is put into drying box by experiment the previous day, is set
The temperature of drying box is 140 DEG C, is dried through 140 DEG C) it is added in 50mL centrifuge tubes, the salting out of sodium chloride improves acetonitrile
Extraction efficiency；
S4 shakes batch mixing：50mL centrifuge tubes are covered tightly into lid, are placed in shaking table, setup parameter shakes 30min,
300rpm；
S5, the primary extraction of ultrasound：50mL centrifuge tubes are set in supersonic wave cleaning machine, ultrasonic extraction 20min is stood overnight；
S6, ultrasonic second extraction：Next day, 50mL centrifuge tubes, are then placed in a centrifuge by ultrasonic extraction 20min again,
Set 5000r/min, time 5min, centrifugal treating；
S7, concentration：The liquid that will be centrifuged in S6, taking 10mL supernatants nitrogen at a temperature of 40 DEG C to blow, concentration is close to be done, so
Afterwards, add hexane 2mL to be clean；
S8, purification：Fu Luoli silicon Solid phase extraction pillars (1.0g, 6mL) are placed in 24 solid phases of Vac Elut SPS extraction
It takes in instrument, uses 5mL hexane acetones mixed liquor (volume ratio 1: 9) that S7 sample concentrations are added after the activation of 5mL n-hexanes successively
Liquid is eluted with 5mL hexane acetones mixed liquor (volume ratio 1: 9), is repeated 1 times, obtains mixed liquor A；
S9 makes determinand：The mixed liquor A that S8 is obtained is placed in nitrogen evaporator, and 40 DEG C of temperature is arranged, and nitrogen blows close dry, use
N-hexane is settled to 1mL, obtains determinand B；
S10 is measured：The determinand B in above-mentioned S9 is taken out, chromatography column condition is HP-5 capillary columns, 30m × 0.25mm
× 0.25 μm, carrier gas is high pure nitrogen；Temperature programming：100 DEG C of holding 3min rise to 250 DEG C of holding 5min with 120 DEG C/min,
260 DEG C of holding 3.4min are risen to 120 DEG C/min again；Injector temperature：200 DEG C, input mode：Split sampling, 1 μ of sample size
L, split ratio 10: 1, column flow rate 1.5mL/min, electron capture detector, 300 DEG C of temperature had its 8 kinds in 13 minutes
Machine chloro pesticide detaches.
Preferably, batch mixing is shaken：The 50mL centrifuge tubes for having weighed up sample, addition Extraction solvent are covered tightly into lid, are placed in shaking table
In, setup parameter shakes 30min, 300rpm.
Preferably, the primary extraction of ultrasound：50mL centrifuge tubes are set in supersonic wave cleaning machine, ultrasonic extraction 20min, is placed
Overnight；Ultrasonic second extraction：Next day, 50mL centrifuge tubes, are then placed in a centrifuge by ultrasonic extraction 20min again, setting
5000r/min, time 5min, centrifugal treating.
Preferably, commodity in use Fu Luoli silicon Solid phase extraction pillar (1.0g, 6mL), is placed in solid-phase extracting instrument
In, it uses 5mL hexane acetones mixed liquor (volume ratio 1: 9) that S7 sample concentration liquid is added after the activation of 5mL n-hexanes successively, uses
5mL hexane acetones mixed liquor (volume ratio 1: 9) elutes, and repeats 1 time, obtains mixed liquor A.
Preferably, mixed liquor A S8 obtained is placed in nitrogen evaporator, and 40 DEG C of temperature is arranged, and nitrogen, which is blown, closely to be done, fixed with n-hexane
Hold to 1mL, obtains determinand B.
Preferably, gas-chromatography instrument method：Chromatography column condition is HP-5 capillary columns, the μ of 30m × 0.25mm × 0.25
M, carrier gas are high pure nitrogen；Temperature programming：100 DEG C of holding 3min rise to 250 DEG C of holding 5min with 120 DEG C/min, then with 120
DEG C/min rise to 260 DEG C holding 3.4min；Injector temperature：200 DEG C, input mode：Split sampling, 1 μ L of sample size, shunting
Than 10: 1, column flow rate 1.5mL/min, electron capture detector, 300 DEG C of temperature, in 13 minutes, by 8 kinds of organo-chlorine pesticides
Separation.
Compared with prior art, the beneficial effects of the invention are as follows：Using the ultrasonic extraction of relative ease, put overnight
Pre-treating method, compared with GB/T14550-2003 uses Soxhlet extraction, the workload of single sample reduces more than half,
Organic solvent usage amount reduces to 20mL from 110mL, and entire extraction process greatly reduces organic molten without being again turned on lid
The injury that agent is volatilized to experimenter purifies (Florisil SPE) in conjunction with Fu Luoli silicon solid phase extraction columns, eliminates preceding place
Manage the tedious steps of the glassware cleaned after the completion.Compared with GB/T14550-2003, the workload of single sample is at most only
For its a quarter, batch processing is then more efficient.Use the high gas chromatograph-electron capture detector of popularity rate
(GC-ECD) method for measuring Organochlorine Pesticides In Soil, accuracy is good, precision is high.
This experiment uses ultrasonic extraction, and extraction efficiency is high, simple and efficient to handle, and consumption of organic solvent is few, to environment
It is friendly；The small column extracting of purification method SPE solid phases can remove the interfering substance in soil matrix, use gas-chromatography skill substantially
Art establishes 8 kinds of organochlorine detection methods in agricultural land soil, and entire analytic process realizes that automation equipment operates substantially, significantly
Human error is reduced, the accuracy of detection method is good, precision is high, is suitable for the quick detection of organochlorine in agricultural land soil.
This method has many advantages, such as qualitative accurate, high sensitivity, easy to operate.This experiment has also carried out DDT and its metabolism
Chromatographic behavior research of the object on nonpolar chromatographic column HP-5, substantially increases accuracy.
Description of the drawings
Fig. 1 is the method flow schematic diagram of the present invention；
Fig. 2 is that three kinds of extracting method recovery of standard addition compare；
Fig. 3 is three kinds of purification method recovery of standard addition comparison schematic diagrams；
Fig. 4 is that initial temperature is high, the lower 8 kinds of organochlorine chromatograms of the slow temperature program of heating rate；
Fig. 5 is that initial temperature is low, the lower 8 kinds of organochlorine chromatograms of the slow temperature program of heating rate；
Fig. 6 is that initial temperature is high, the lower 8 kinds of organochlorine chromatograms of the fast temperature program of heating rate.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
His embodiment, shall fall within the protection scope of the present invention.
- 6 are please referred to Fig.1, the present invention provides a kind of technical solution：
A kind of ultrasonic wave and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues method, include the following steps：
S1, sampling：The soil sample for taking the topsoil soils and topsoil of depth about 15cm or less (15-30) cm, by soil profile layer
Secondary clearing samples, and on each sampled point, soil is cut vertically downward by layer, and each point takes the soil of thickness about 10cm, and every
The soil amount taken on a point is equal, is uniformly mixed the soil sample of each point after sampling, then pedotheque is placed on interior
Ventilation after natural air drying, is ground soil using grinder, and crosses 80 mesh sieve；
S2, sample blending processing：50mL centrifuge tubes are placed on electronic balance, are weighed the soil sample 20.0g obtained in S1 and are used
In subsequent analysis, 5.00mL deionized waters are measured using liquid-transfering gun, is added in 50mL centrifuge tubes, is rocked 1 minute, shake manually
It is even；
S3 extracts, saltouts：Using one division pipette, measures 20mL acetonitriles and above-mentioned 50mL is added as extractant
In centrifuge tube, then, measuring sodium chloride 5-7g with electronic balance, (sodium chloride is put into drying box by experiment the previous day, is set
The temperature of drying box is 140 DEG C, is dried through 140 DEG C) it is added in 50mL centrifuge tubes, the salting out of sodium chloride improves acetonitrile
Extraction efficiency；
S4 shakes batch mixing：50mL centrifuge tubes are covered tightly into lid, are placed in shaking table, setup parameter shakes 30min,
300rpm；
S5, the primary extraction of ultrasound：50mL centrifuge tubes are set in supersonic wave cleaning machine, ultrasonic extraction 20min is stood overnight；
S6, ultrasonic second extraction：Next day, 50mL centrifuge tubes, are then placed in a centrifuge by ultrasonic extraction 20min again,
Set 5000r/min, time 5min, centrifugal treating；
S7, concentration：The liquid that will be centrifuged in S6, taking 10mL supernatants nitrogen at a temperature of 40 DEG C to blow, concentration is close to be done, so
Afterwards, add hexane 2mL to be clean；
S8, purification：Fu Luoli silicon Solid phase extraction pillars (1.0g, 6mL) are placed in 24 solid phases of Vac Elut SPS extraction
It takes in instrument, uses 5mL hexane acetones mixed liquor (volume ratio 1: 9) that S7 sample concentrations are added after the activation of 5mL n-hexanes successively
Liquid is eluted with 5mL hexane acetones mixed liquor (volume ratio 1: 9), is repeated 1 times, obtains mixed liquor A；
S9 makes determinand：The mixed liquor A that S8 is obtained is placed in nitrogen evaporator, and 40 DEG C of temperature is arranged, and nitrogen blows close dry, use
N-hexane is settled to 1mL, obtains determinand B；
S10 is measured：The determinand B in above-mentioned S9 is taken out, chromatography column condition is HP-5 capillary columns, 30m × 0.25mm
× 0.25 μm, carrier gas is high pure nitrogen；Temperature programming：100 DEG C of holding 3min rise to 250 DEG C of holding 5min with 120 DEG C/min,
260 DEG C of holding 3.4min are risen to 120 DEG C/min again；Injector temperature：200 DEG C, input mode：Split sampling, 1 μ of sample size
L, split ratio 10: 1, column flow rate 1.5mL/min, electron capture detector, 300 DEG C of temperature had its 8 kinds in 13 minutes
Machine chloro pesticide detaches.
As a result with analysis
One, the selection of extracting method
Compare 3 kinds of extracting methods：
A is the Soxhlet extraction mentioned in background technology；
B is handled by the method for the present invention；
C is to be handled by the method for the present invention, but will stand overnight and be changed to place 20min.
All with the small column purifications of SPE after extraction.The extraction efficiency of 3 kinds of extracting methods is with the recycling knot of mark-on 0.01mg/kg
Fruit calculates, and sees Fig. 1, as seen in figures：For the rate of recovery of method A and B without significant difference, the C rate of recovery is relatively low.Method A takes that surpass 24 small
When, organic solvent 110mL is consumed, special instrument need to be purchased, needs to clean a large amount of glasswares after the completion of experiment, human hand operation
Time is also longer, and the workload of single sample is twice or more of method B, and method B's is more efficient when batch processing, selects B
Extracting method as this experiment.
Two, the selection of purification method
3 kinds of purification methods have been investigated in this experiment：
D is the concentrated sulfuric acid cleanup method by GB/T14550,
E is the concentrated sulfuric acid cleanup method of the offers such as Liu Hongmei,
F is purified using Florisil commercialization pillars SPE by the method for the present invention.
See Fig. 4-6, the purification of 3 kinds of methods by the method extraction in the present invention, the chromatogram of 3 kinds of purification methods before purification
Effect is suitable, and chromatogram is interfered without apparent miscellaneous peak.The recycling result of mark-on 0.01mg/kg is shown in Fig. 3, and the rate of recovery is without apparent
Variation, but the operation of method D is extremely complex, needs the glassware of cleaning also most after experiment, the workload of each sample
It is twice or more of method F；Method E's is easy to operate, but dangerous big, breaks pipe rate height, generally surpasses 10%, once broken pipe needs
Pre-treatment is re-started, workload is also increased, delays the time for providing experimental result；Method F is extremely suitable at batch
It sets, this experimental selection F is as purification method.
Three, the selection of gas-chromatography temperature program
OCPs is a kind of low pole compound, and the chromatographic column of nonpolarity or low pole stationary phase may be selected to reach ideal
Separating effect and obtain higher response.This experiment compares a variety of temperature programs using HP-5 capillary columns, every time
The mixed standard solution that equal implantation concentration is 0.1mg/L：
Using the temperature program of the offers such as Liu Hongmei, P, P '-DDD and 0, P '-DDT 2 can not be made in this experiment
A component separates, and sees the chromatographic peak of serial number 7 (12.486min) in Fig. 4.Temperature program：It is risen to from 190 DEG C with 5 DEG C/min
210 DEG C of holding 5min, then 220 DEG C of holding 1min are risen to 2 DEG C/min, then 270 DEG C of holding 5min are risen to 10 DEG C/min, entirely
Cheng Yunhang takes 20min.
To detach 2 components of P, P '-DDD and 0, P '-DDT, using initial temperature is reduced, the side of heating rate is reduced
Method, enabling initial temperature every time reduces by 10 DEG C, rises to 210 DEG C of holding 5min later with 5 DEG C/min, then rise to 220 DEG C of guarantors with 2 DEG C/min
1min is held, then 270 DEG C of holding 3min are risen to 10 DEG C/min.11 temperature program methods are tested in this way, and the time of operation is not
It is disconnected to extend, but two components of P, P '-DDD and 0, P '-DDT can not be efficiently separated always, and sensitivity is greatly reduced, and sees figure
5, the temperature program of this method：From 80 DEG C of holding 5min, 210 DEG C are risen to 2 DEG C/min, then 270 DEG C are risen to 50 DEG C/min
Keep 3min.210 DEG C are risen to 2 DEG C/min, then 270 DEG C of holding 3min are risen to 50 DEG C/min.
Lower initial temperature is selected, faster heating rate, as a result P, P '-DDD and 0, P '-DDT are efficiently separated：It rises
Warm program is as follows：From 90 DEG C of holding 3min, 250 DEG C of holding 5min are risen to 120 DEG C/min, then 260 are risen to 100 DEG C/min
DEG C keep 3.4min, run time 12.83min, Fig. 6.Under this instrumental method, 8 components realize good separation, response
Testing requirements are fully achieved in height, sensitivity.
Analysis：Under normal circumstances, using low polar HP-5 chromatographic columns or slow down heating rate and can be increased with certain procedures
Separating degree between difficult separation component, but while the relative retention value of this two component increases, the peak width of component is also increasing
Add, when the increase for increasing above relative retention value of peak width, overlapping for two components is even more serious, such as serial number 7 in Fig. 4
In (12.486min) and Fig. 5 shown in the chromatographic peak of serial number 6 (63.284min).Use the slightly higher DB- of stationary phase polarity
1701P reduces reservation of the chromatographic column liquid film to nonpolar component, the peak width of component is made to narrow；Or the heating using 2.3.3
Program, heating rate are accelerated, and increase molecular diffusion rate, the constriction peak width of component, so as to improve the separating degree of compound,
The principle of both methods is close, and has all reached and make P, the purpose that P '-DDD is clearly separated with 0, P '-DDT, two components.
Four, the linear detection range of quantitative approach
With a concentration of abscissa of mixed standard solution, the peak area of each target compound chromatographic peak is ordinate, is drawn
Standard curve, property sexual intercourse related coefficient, regression equation are shown in Table 1.8 kinds of organochlorines are linear within the scope of 0.01-0.2 μ g/mL
Relationship is good, r2Value is all higher than 0.999.
Five, method detection limit
Minimum detectability is by 3 times of calculating of the response of 0.01 μ g/mL of minimum concentration point and the noise response of baseline, inspection
Rising limit the results are shown in Table 1.The method detection of 8 kinds of organochlorines is limited to 0.012~0.059ng/g, can meet trace organic chlorine in soil
Detection.
The regression equation of 8 kinds of organochlorines, related coefficient, detection limit, the rate of recovery and relative standard are inclined in 1 agricultural land soil of table
Difference
Six, the method rate of recovery and precision
Under identical experiment condition, 8 kinds of organochlorines that 6 blank pedotheques are added with a concentration of 0.005 μ g/g are mixed
Standard specimen is closed, mark-on reclaims and precision test are carried out, test result is shown in Table 1.The recovery of standard addition of 8 kinds of organochlorines is：92.1%
~105.3%, relative standard deviation：2.7%~6.9%.Method has the preferable rate of recovery and precision.
This experiment uses ultrasonic extraction, and extraction efficiency is high, simple and efficient to handle, and consumption of organic solvent is few, to environment
It is friendly；The small column extracting of purification method SPE solid phases can remove the interfering substance in soil matrix, use gas-chromatography skill substantially
Art establishes 8 kinds of organochlorine detection methods in agricultural land soil, and entire analytic process realizes that automation equipment operates substantially, significantly
Human error is reduced, the accuracy of detection method is good, precision is high, is suitable for the quick detection of organochlorine in agricultural land soil, has
There are substantive distinguishing features outstanding and significant progress.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of ultrasonic wave and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues method, which is characterized in that including
Following steps：
S1, sampling：The soil sample for taking the topsoil soils and topsoil of depth about 15cm or less (15-30) cm, by soil profile layer point
Layer sampling, on each sampled point, soil is cut by layer vertically downward, and each point takes the soil of thickness about 10cm, and in each point
On the soil amount that is taken it is equal, the soil sample of each point is uniformly mixed after sampling, then pedotheque is placed on room ventilation
Locate, after natural air drying, ground soil using grinder, and crosses 80 mesh sieve；
S2, sample blending processing：50mL centrifuge tubes are placed on electronic balance, are weighed after the soil sample 20.0g obtained in S1 is used for
Continuous analysis measures 5.00mL deionized waters using liquid-transfering gun, is added in 50mL centrifuge tubes, rocks 1 minute, shake up manually；
S3 extracts, saltouts：Using one division pipette, 20mL acetonitriles are measured, as extractant, above-mentioned 50mL centrifugations are added
Guan Zhong, then, measuring sodium chloride 5-7g with electronic balance, (sodium chloride is put into drying box by experiment the previous day, setting drying
The temperature of case is 140 DEG C, is dried through 140 DEG C) it is added in 50mL centrifuge tubes, the salting out of sodium chloride improves the extraction effect of acetonitrile
Rate；
S4 shakes batch mixing：50mL centrifuge tubes are covered tightly into lid, are placed in shaking table, setup parameter shakes 30min, 300rpm；
S5, the primary extraction of ultrasound：50mL centrifuge tubes are set in supersonic wave cleaning machine, ultrasonic extraction 20min is stood overnight；
S6, ultrasonic second extraction：Next day, 50mL centrifuge tubes, are then placed in a centrifuge by ultrasonic extraction 20min again, setting
5000r/min, time 5min, centrifugal treating；
S7, concentration：The liquid that will be centrifuged in S6, taking 10mL supernatants nitrogen at a temperature of 40 DEG C to blow, concentration is close to be done, and then, is added
Hexane 2mL is to be clean；
S8, purification：Fu Luoli silicon Solid phase extraction pillars (1.0g, 6mL) are placed in 24 solid-phase extracting instruments of Vac Elut SPS
In, it uses 5mL hexane acetones mixed liquor (volume ratio 1: 9) that S7 sample concentration liquid is added after the activation of 5mL n-hexanes successively, uses
5mL acetone normal hexanes mixed liquor (volume ratio 1: 9) elutes, and is repeated 1 times, obtains mixed liquor A；
S9 makes determinand：The mixed liquor A that S8 is obtained is placed in nitrogen evaporator, and 40 DEG C of temperature is arranged, and nitrogen, which is blown, closely to be done, and n-hexane is used
It is settled to 1mL, obtains determinand B；
S10 is measured：The determinand B in above-mentioned S9 is taken out, chromatography column condition is HP-5 capillary columns, 30m × 0.25mm ×
0.25 μm, carrier gas is high pure nitrogen；Temperature programming：100 DEG C of holding 3min rise to 250 DEG C of holding 5min with 120 DEG C/min, then
260 DEG C of holding 3.4min are risen to 120 DEG C/min；Injector temperature：200 DEG C, input mode：Split sampling, 1 μ L of sample size,
Split ratio 10: 1, column flow rate 1.5mL/min, electron capture detector, 300 DEG C of temperature are organic by its 8 kinds in 13 minutes
Chloro pesticide detaches.
2. a kind of ultrasonic wave according to claim 1 and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues side
Method, it is characterised in that：Shake batch mixing：The 50mL centrifuge tubes for having weighed up sample, addition Extraction solvent are covered tightly into lid, are placed in shaking table
In, setup parameter shakes 30min, 300rpm.
3. a kind of ultrasonic wave according to claim 1 and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues side
Method, it is characterised in that：Ultrasonic primary extraction：50mL centrifuge tubes are set in supersonic wave cleaning machine, ultrasonic extraction 20min was placed
Night；Ultrasonic second extraction：Next day, 50mL centrifuge tubes, are then placed in a centrifuge by ultrasonic extraction 20min again, setting
5000r/min, time 5min, centrifugal treating.
4. a kind of ultrasonic wave according to claim 1 and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues side
Method, it is characterised in that：Commodity in use Fu Luoli silicon Solid phase extraction pillars (1.0g, 6mL), are placed in solid-phase extracting instrument,
5mL hexane acetones mixed liquor (volume ratio 1: 9) is used S7 sample concentration liquid to be added, with 5mL third after the activation of 5mL n-hexanes successively
Ketone n-hexane mixed liquor (volume ratio 1: 9) elutes, and is repeated 1 times, obtains mixed liquor A.
5. a kind of ultrasonic wave according to claim 4 and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues side
Method, it is characterised in that：The mixed liquor A that S8 is obtained is placed in nitrogen evaporator, and 40 DEG C of temperature is arranged, and nitrogen, which is blown, closely to be done, with n-hexane constant volume
To 1mL, determinand B is obtained.
6. a kind of ultrasonic wave according to claim 1 and gas-chromatography binding assay agricultural land soil Organochlorine Pesticide Residues side
Method, it is characterised in that：Gas-chromatography instrument method：Chromatography column condition is HP-5 capillary columns, 30m × 0.25mm × 0.25 μm,
Carrier gas is high pure nitrogen；Temperature programming：100 DEG C holding 3min, with 120 DEG C/min rise to 250 DEG C holding 5min, then with 120 DEG C/
Min rises to 260 DEG C of holding 3.4min；Injector temperature：200 DEG C, input mode：Split sampling, 1 μ L of sample size, split ratio 10:
1, column flow rate 1.5mL/min, electron capture detector, 300 DEG C of temperature detached 8 kinds of organo-chlorine pesticides in 13 minutes.
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| CN110681180A (en) * | 2019-10-10 | 2020-01-14 | 深圳市龙华区中心医院 | Method for extracting endocrine disruptors |
| CN110865135A (en) * | 2019-10-30 | 2020-03-06 | 河南大学 | Method for measuring capacity of micro plastic for adsorbing soil organic chlorine pesticide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110681180A (en) * | 2019-10-10 | 2020-01-14 | 深圳市龙华区中心医院 | Method for extracting endocrine disruptors |
| CN110865135A (en) * | 2019-10-30 | 2020-03-06 | 河南大学 | Method for measuring capacity of micro plastic for adsorbing soil organic chlorine pesticide |
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