CN109991358A - Measure chloroacetic method in soil - Google Patents
Measure chloroacetic method in soil Download PDFInfo
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- CN109991358A CN109991358A CN201910279924.2A CN201910279924A CN109991358A CN 109991358 A CN109991358 A CN 109991358A CN 201910279924 A CN201910279924 A CN 201910279924A CN 109991358 A CN109991358 A CN 109991358A
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- chloroacetic
- mobile phase
- solution
- monoxone
- soil according
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Classifications
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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
-
- 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
-
- 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
- G01N30/89—Inverse chromatography
-
- 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
- G01N2030/042—Standards
- G01N2030/047—Standards external
-
- 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
- G01N2030/146—Preparation by elimination of some components using membranes
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
- G01N2030/8845—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds involving halogenated organic compounds
Abstract
The present invention relates to chloroacetic methods in measurement soil comprising step: prepares mobile phase and monoxone standard solution；Pedotheque is added in mobile phase and extracts testing sample solution；Monoxone standard solution and testing sample solution are tested and analyzed respectively using rp-hplc；Chloroacetic concentration in testing sample solution is calculated according to the result of detection and analysis.In measurement pedotheque provided by the invention in chloroacetic method, sample treatment is simple, and detection process is easy to operate, and the high sensitivity of the method for the present invention, detection limit are low, it can be achieved that chloroacetic quick detection in practical pedotheque.
Description
Technical field
The present invention relates to chloroacetic methods in measurement soil.
Background technique
Monoxone, also referred to as chloroacetic acid (English name: Chloroacetic acid, No. CAS: 79-11-8), it is a kind of
Important industrial chemicals is a kind of important intermediate in organic synthesis, pesticide, medicine, dyestuff, daily use chemicals, surfactant,
Chemical reagent, papermaking chemical product, oilfield chemistry, textile auxiliary, rubber chemicals, plating and spices and essence etc. have extensive
Application.
Chloroethene acids is extremely toxic substance, and monoxone belongs to one of chloroethene acids, has potential carcinogenic work to human body
With toxicity constantly obtains toxicology and physiological confirmation, causes the extensive concern of people.Chloroethene acids in water
There are many kinds of analysis determining methods, such as colorimetric method, high performance liquid chromatography, gas chromatography, the chromatography of ions.Wherein, than
Color method sensitivity is low, poor selectivity, is easy the interference etc. by other similar compounds such as dichloroacetic acid；High performance liquid chromatography
Although interfering substance can be separated effectively, analysis time is short and high sensitivity, reagent cost are relatively high；In GB/T5750.10-
Gas chromatography is used in 2006 " the drinking water standard methods of inspection ", but needs to carry out monoxone esterification derivative, is operated
Step is more, and analysis time is longer；The chromatography of ions can be used for analyzing monoxone in water, but be often limited by the complexity of matrix,
And to prevent the interference of the high concentration ions such as chloride ion in water.However, being pesticide in the chloroacetic major consumers field in China
And pesticide industry, monoxone can synthesize more than 20 common desinsection, weeding and plant growth regulations, this results in chloroethene
Acid can also pollute in the soil, and monoxone also moves in soil in Chang Huicong water body, further makes chlorine in soil
The pollution problem of acetic acid is more serious and threatens to human health.In contrast, in soil chloroacetic analysis method compared with
Understatement road, or even such contamination accident once occur can generate and lack coherent detection analysis foundation, be unable to judge accurately etc. and to ask
Topic.
Summary of the invention
An object of the present invention is for overcome the deficiencies in the prior art, to provide chloroacetic side in a kind of measurement soil
Method.
In order to achieve the above object, the invention is realized by the following technical scheme:
Measure chloroacetic method in soil, which is characterized in that comprising steps of
A, mobile phase and monoxone standard solution are prepared；
B, pedotheque is added in mobile phase and extracts testing sample solution；
C, using rp-hplc respectively to be measured in the monoxone standard solution and step B in step A
Sample solution tests and analyzes；
D, chloroacetic concentration in testing sample solution is calculated according to the detection and analysis result in step C.
According to one embodiment of present invention, the mobile phase is made of by volume for 10:90 acetonitrile with phosphoric acid solution,
Wherein the volume fraction of phosphoric acid solution is 0.1%；After acetonitrile and phosphoric acid solution are mixed according to the above mentioned proportion, using 0.45 μm
Organic phase filter membrane filtering and at least 20min ultrasonic treatment.
According to one embodiment of present invention, in step A, a series of various concentrations are prepared by solvent of the mobile phase
Monoxone standard solution, concentration range are 1.0~20.0 μ g/ml.
According to one embodiment of present invention, in step B, soil weight and mobile phase volume ratio are 1:(2-5), wherein weighing
Amount unit is g, volume unit mL.
According to one embodiment of present invention, in step B, soil weight and mobile phase volume ratio are 1:4, wherein weight list
Position is g, volume unit mL.
According to one embodiment of present invention, it in step B, weighs after the mobile phase is added in soil and carries out ultrasound twice,
Each at least 15min, then stand 30min.
According to one embodiment of present invention, take the supernatant liquor after standing in centrifuge tube, at revolving speed 4000r/min
It is centrifuged 5min, the supernatant after collecting centrifugation passes through 0.22 μm of water phase pin hole membrane filtration again.
According to one embodiment of present invention, in step C, detection and analysis use the size of Zorbax SB-C8 chromatographic column for
4.6 × 250mm, 5.0 μm.
According to one embodiment of present invention, the rp-hplc is detected according to following condition: column
Temperature is 30 DEG C, and sampling volume is 20.0 μ l, flow rate of mobile phase 1.0ml/min；Detector is two poles that function is acquired with 3D
Pipe array detector, acquisition wavelength are 214nm, scanning range 200-400nm, frequency acquisition 5Hz, and acquisition time is
15min。
According to one embodiment of present invention, in step D, the monoxone standard that is detected with rp-hplc
The chromatographic peak peak area of solution and corresponding concentration draw standard curve, in conjunction with the chromatographic peak peak area in testing sample solution
Calculate chloroethene acid concentration.
Compared with the prior art, the invention has the advantages that:
1, the present invention provides chloroacetic method in measurement pedotheque, sample treatment is simple, detection process behaviour
Facilitate, and the high sensitivity of the method for the present invention, detection limit are low, it can be achieved that chloroacetic quick inspection in practical pedotheque
It surveys；
2, chromatographic test strip part is optimized, target components is made to generate stronger stick effect and is kept completely separate out with matrix,
And chromatographic column is damaged smaller；
3, the pre-treating method of soil is developed, and has carried out the comparison of sample mark-on, it was demonstrated that the feasibility of this method；
4, the soil sample amount for optimizing pre-treatment both ensure that the sensitivity of measurement in turn simplified pre-treatment step, also
It ensure that the safety of entire measurement operation.
Detailed description of the invention
Fig. 1 is chloroacetic standard solution chromatogram in embodiment 1 (by taking 10 μ g/ml as an example).
Fig. 2 is chloroacetic standard curve in embodiment 1.
Specific embodiment
The present invention is described in detail below with reference to embodiment:
Embodiment 1
In order to achieve the above object, being achieved through the following technical solutions chloroacetic method in measurement soil, which is characterized in that
The following steps are included:
A, according to acetonitrile: phosphoric acid is the volume ratio of 10:90, takes volume fraction offline for 0.1% phosphoric acid solution and acetonitrile
Mixing, mixed solution obtain mobile phase using 0.45 μm of organic phase filter membrane filtering and the ultrasonic treatment of 20min；
Using above-mentioned prepared mobile phase as solvent, a series of monoxone standard solution of various concentrations is prepared, chloroethene acid concentration is successively
For 1.0 μ g/ml, 2.0 μ g/ml, 5.0 μ g/ml, 10.0 μ g/ml, 20.0 μ g/ml.
B, 5.0g pedotheque is accurately weighed, is placed in 20mL Brown Glass Brown glass bottles and jars only, the above-mentioned prepared flowing of 10mL is added
Phase, then the vial after addition mobile phase is placed in supersonic wave cleaning machine and is ultrasonically treated in two times, each ultrasound 15min surpasses
30min is stood after sound, obtains testing sample solution；If there are also more suspended matters in the supernatant liquor after standing, take upper layer clear
Liquid is centrifuged 5min in centrifuge tube at revolving speed 4000r/min, and the supernatant after collecting centrifugation passes through 0.22 μm of water phase pin hole
Membrane filtration obtains testing sample solution；The testing sample solution for finally taking 1mL to obtain is in sample injection bottle to sample introduction.
C, using rp-hplc respectively in a series of monoxone standard solution and step B in step A
Testing sample solution test and analyze, detect chromatographic condition are as follows:
Use the size of Zorbax SB-C8 chromatographic column for 4.6 × 250mm, 5.0 μm；
Column temperature is 30 DEG C, and sampling volume is 20.0 μ l, flow rate of mobile phase 1.0ml/min；
Detector is the diode array detector that function is acquired with 3D, and acquisition wavelength is 214nm, and scanning range is
200-400nm, frequency acquisition 5Hz, acquisition time 15min.
D, using a series of chromatographic peak peak area of the monoxone standard solution detected in step C as ordinate Y-axis, chlorine
The concentration of acetic acid standard solution is abscissa X-axis, draws standard curve, calculates slope and intercept, obtain equation of linear regression
Are as follows: Y=3.54X+0.036；Wherein R2=0.9993, illustrate that the peak area of the monoxone standard solution detected and its concentration have
There is good linear relationship.As shown in Figure 1, the retention time of 10 μ g/ml chloroacetic acid solutions is 5.295min.According to above-mentioned linear
The calculated by peak area for the testing sample solution that regression equation and detection obtain obtains chloroethene acid concentration in testing sample solution.
For the accuracy of judgment method, the monoxone of known quantity is added in the pedotheque of blank, is carried out with embodiment 1
Sample treatment operation and detection and analysis operation, measure chloroacetic peak area, substitute into above-mentioned standard curve, acquire above-mentioned soil-like
Chloroacetic content in product according to known magnitude and acquires content value comparison discovery, the detection error of the method for the present invention be 5% with
It is interior.
Embodiment 2
In order to achieve the above object, being achieved through the following technical solutions chloroacetic method in measurement soil, which is characterized in that
The following steps are included:
Step A, the operation of C, D only change the step the sampling amount of sample in B with embodiment 1.
Scheme one: B accurately weighs 6.0g pedotheque, is placed in 20mL Brown Glass Brown glass bottles and jars only, and the prepared stream of 15mL is added
Dynamic phase, then the vial after addition mobile phase is placed in supersonic wave cleaning machine and is ultrasonically treated in two times, each ultrasound 18min,
30min is stood after ultrasound, obtains testing sample solution；If there are also more suspended matters in the supernatant liquor after standing, upper layer is taken
Clear liquid is centrifuged 5min in centrifuge tube at revolving speed 4000r/min, and the supernatant after collecting centrifugation passes through 0.22 μm of water phase needle
Hole membrane filtration, obtains testing sample solution；The testing sample solution for finally taking 1mL to obtain is in sample injection bottle to sample introduction.
Scheme two: B accurately weighs 5.0g pedotheque, is placed in 20mL Brown Glass Brown glass bottles and jars only, and the prepared stream of 20mL is added
Dynamic phase, then the vial after addition mobile phase is placed in supersonic wave cleaning machine and is ultrasonically treated in two times, each ultrasound 20min,
30min is stood after ultrasound, obtains testing sample solution；If there are also more suspended matters in the supernatant liquor after standing, upper layer is taken
Clear liquid is centrifuged 5min in centrifuge tube at revolving speed 4000r/min, and the supernatant after collecting centrifugation passes through 0.22 μm of water phase needle
Hole membrane filtration, obtains testing sample solution；The testing sample solution for finally taking 1mL to obtain is in sample injection bottle to sample introduction.
Scheme three: B accurately weighs 5.0g pedotheque, is placed in 50mL Brown Glass Brown glass bottles and jars only, and the prepared stream of 25mL is added
Dynamic phase, then the vial after addition mobile phase is placed in supersonic wave cleaning machine and is ultrasonically treated in two times, each ultrasound 30min,
30min is stood after ultrasound, obtains testing sample solution；If there are also more suspended matters in the supernatant liquor after standing, upper layer is taken
Clear liquid is centrifuged 5min in centrifuge tube at revolving speed 4000r/min, and the supernatant after collecting centrifugation passes through 0.22 μm of water phase needle
Hole membrane filtration, obtains testing sample solution；The testing sample solution for finally taking 1mL to obtain is in sample injection bottle to sample introduction.
Chlorine in testing sample solution is calculated in the present embodiment according to the equation of linear regression that step D is obtained in embodiment 1
Acetic acid concentration.
It is found by above-mentioned experiment and the experiment of embodiment 1, before the sample of different sampling amounts is by sample in the present invention
Reason method can obtain comparatively ideal testing result during subsequent detection, it was demonstrated that the sample treatment has feasible
Property.
Embodiment 3
In order to achieve the above object, being achieved through the following technical solutions chloroacetic method in measurement soil, which is characterized in that
The following steps are included:
The operation of step B-D only changes the step the volume ratio of acetonitrile and phosphoric acid in A with embodiment 1.
Scheme one: acetonitrile: the volume ratio of phosphoric acid is 20:80；
Scheme two: acetonitrile: the volume ratio of phosphoric acid is 15:85；
Scheme three: acetonitrile: the volume ratio of phosphoric acid is 30:70；
Scheme four: acetonitrile: the volume ratio of phosphoric acid is 25:75.
It is found by above-mentioned Experimental comparison, chloroacetic chromatographic peak retention time is longer in scheme one, is more advantageous to chromatography
Separation, therefore selection scheme one carries out rp-hplc.
Chloroacetic method in the practical pedotheque of measurement in the present invention, sample treatment is simple, detection method is easy
In operation, and the high sensitivity of this method, detection limit are low, it can be achieved that chloroacetic quick detection in practical pedotheque.
Embodiment in the present invention is only used for that the present invention will be described, and is not construed as limiting the scope of claims limitation,
It may occur to persons skilled in the art that other substantially equivalent substitutions, all fall in the scope of protection of the present invention.
Claims (10)
1. measuring chloroacetic method in soil, which is characterized in that comprising steps of
A, mobile phase and monoxone standard solution are prepared；
B, pedotheque is added in mobile phase and extracts testing sample solution；
C, using rp-hplc respectively to the sample to be tested in the monoxone standard solution and step B in step A
Solution tests and analyzes；
D, chloroacetic concentration in testing sample solution is calculated according to the detection and analysis result in step C.
2. chloroacetic method in measurement soil according to claim 1, which is characterized in that the mobile phase by acetonitrile with
Phosphoric acid solution is 10:90 composition by volume, and wherein the volume fraction of phosphoric acid solution is 0.1%；Acetonitrile and phosphoric acid solution are pressed
After aforementioned proportion mixing, using 0.45 μm of organic phase filter membrane filtering and the ultrasonic treatment of at least 20min.
3. chloroacetic method in measurement soil according to claim 1, which is characterized in that in step A, with the flowing
It is mutually a series of monoxone standard solution that solvent prepares various concentrations, concentration range is 1.0~20.0 μ g/ml.
4. chloroacetic method in measurement soil according to claim 1, which is characterized in that in step B, soil weight with
Mobile phase volume ratio is 1:(2-5), wherein unit of weight is g, volume unit mL.
5. chloroacetic method in measurement soil according to claim 1, which is characterized in that in step B, soil weight with
Mobile phase volume ratio is 1:4, and wherein unit of weight is g, volume unit mL.
6. chloroacetic method in measurement soil according to claim 1, which is characterized in that in step B, weigh soil and add
Ultrasound twice is carried out after entering the mobile phase, every time at least 15min, then stands 30min.
7. chloroacetic method in measurement soil according to claim 6, which is characterized in that take the supernatant liquor after standing
In centrifuge tube, 5min is centrifuged at revolving speed 4000r/min, the supernatant after collecting centrifugation passes through 0.22 μm of water phase pin hole again
Membrane filtration.
8. chloroacetic method in measurement soil according to claim 1, which is characterized in that in step C, detection and analysis are adopted
It is 4.6 × 250mm with the size of Zorbax SB-C8 chromatographic column, 5.0 μm.
9. chloroacetic method in measurement soil according to claim 1, which is characterized in that the RP-HPLC color
Spectrometer is detected according to following condition: column temperature is 30 DEG C, and sampling volume is 20.0 μ l, flow rate of mobile phase 1.0ml/min；Inspection
Surveying device is the diode array detector that function is acquired with 3D, and acquisition wavelength is 214nm, and scanning range 200-400nm is adopted
Integrate frequency as 5Hz, acquisition time 15min.
10. chloroacetic method in measurement soil according to claim 1, which is characterized in that in step D, with reverse phase height
The chromatographic peak peak area for the monoxone standard solution that effect liquid phase chromatogram instrument detects and corresponding concentration draw standard curve, then tie
The chromatographic peak calculated by peak area closed in testing sample solution goes out chloroethene acid concentration.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111103387A (en) * | 2020-01-09 | 2020-05-05 | 实朴检测技术(上海)股份有限公司 | Method for measuring chloroacetic acid, dichloroacetic acid and trichloroacetic acid in soil |
| CN112014510A (en) * | 2020-09-07 | 2020-12-01 | 瀚盟测试科技（天津）有限公司 | Detection method for determining chloroacetic acid residue in cinepazide maleate intermediate by HPLC (high performance liquid chromatography) method |
| CN112881545A (en) * | 2021-01-12 | 2021-06-01 | 山东省药学科学院 | Method for detecting residual quantity of monochloroacetic acid in modified starch styptic powder |
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| CN112014510B (en) * | 2020-09-07 | 2022-07-05 | 瀚盟测试科技（天津）有限公司 | Detection method for determining chloroacetic acid residue in cinepazide maleate intermediate by HPLC (high performance liquid chromatography) method |
| CN112881545A (en) * | 2021-01-12 | 2021-06-01 | 山东省药学科学院 | Method for detecting residual quantity of monochloroacetic acid in modified starch styptic powder |
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