CN108732293A - The high performance liquid chromatography tandem mass spectrum analysis method of indenes piperazine benfluralin and its metabolin - Google Patents
The high performance liquid chromatography tandem mass spectrum analysis method of indenes piperazine benfluralin and its metabolin Download PDFInfo
- Publication number
- CN108732293A CN108732293A CN201810521114.9A CN201810521114A CN108732293A CN 108732293 A CN108732293 A CN 108732293A CN 201810521114 A CN201810521114 A CN 201810521114A CN 108732293 A CN108732293 A CN 108732293A
- Authority
- CN
- China
- Prior art keywords
- kinds
- indenes piperazine
- piperazine benfluralin
- metabolins
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- G01N30/96—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 using ion-exchange
-
- 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
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses the high performance liquid chromatography tandem mass spectrum analysis methods of indenes piperazine benfluralin and its metabolin, and this approach includes the following steps：The indenes piperazine benfluralin of known concentration gradient and its soil matrix standard working curve of four kinds of metabolins are established with high performance liquid chromatography tandem mass spectrometry, the indenes piperazine benfluralin and its four kinds of metabolite residue amounts in pedotheque extraction and cleaning liquid are measured with high performance liquid chromatography tandem mass spectrometry, record extraction ion chromatography peak area, matrix quantified by external standard method obtains the measured value of indenes piperazine benfluralin and its four kinds of metabolins in the pedotheque extraction and cleaning liquid；The measured value is brought into quantitative calculation formula again, finally obtains indenes piperazine benfluralin to be measured and four kinds of metabolite residue amounts in pedotheque.The method of the present invention, sample pre-treatments are simple to operate, and consumption of organic solvent is few, and target pesticide recovery rate is high, good purification, and the Instrumental Analysis time is short.In addition, the instrument detection limit and method detection limit of the method for the present invention are very low.
Description
Technical field
The invention belongs to analytical chemistry fields, more particularly to the high-efficient liquid phase color of indenes piperazine benfluralin and its metabolin in soil
Tandem Mass Spectrometry Analysis method is composed, this method simplicity, quick, sensitivity and accuracy are high.
Background technology
Triazine herbicide (triazine herbicides) occupies second in herbicide, in world's agricultural production
Played great function, however since its dosage is big, the residence time is long, weeds caused to easy to produce resistance, and can to soil,
Table water and other drinking water sources pollute, and there is an urgent need for research and development new herbicides to substitute traditional triazine herbicide kind.Therefore, have
There are few dosage, broad weed-killing spectrum, longevity of residure length, the Novel alkyl triazines highy potent herbicide indenes to weeds control effect the features such as good
Piperazine benfluralin comes into being, and Beyer Co., Ltd in 2010 releases in the U.S. and emerges.
The indenes piperazine benfluralin mechanism of action is by inhibiting cellulose biosynthesis (CBI), inhibiting the life of plant meristem
Long next effective management of weeds, the herbicide as soil treatment are played by the germination and emergence (hypocotyl absorption) for inhibiting weeds
Effect.Indenes piperazine benfluralin be suitable for the unifacial leaves such as citrus, grape, lawn, ornamental plant and broadleaf weed (it is annual, 2 years
It is raw, perennial) prevention, have the characteristics that longevity of residure length, be not likely to produce drug resistance.
Indenes piperazine benfluralin in the environment using it is rear it is degradable be four kinds of different metabolins (indaziflam ketone, diamino three
Piperazine class, olefines and carboxylic acid compound), the physicochemical properties such as water solubility, octanol water partition coefficient of each metabolin are different, cause
The behaviors such as their degradation characteristic, mobility in the environment have differences.Temporarily have no indenes piperazine benfluralin and four kinds both at home and abroad at present
The relevant report of metabolite analysis method.
The chemistry of four kinds of metabolins such as indenes piperazine benfluralin and indaziflam ketone, diamino triazines, olefines and carboxylic acids
Structural formula is as follows：
Invention content
For the present situation that current indenes piperazine benfluralin and its four kinds of metabolite analysis methods lack, it is an object of the invention to carry
For the high performance liquid chromatography tandem mass spectrum analysis method of a kind of indenes piperazine benfluralin and its metabolin.
The purpose of the invention is achieved by the following technical solution：
The high performance liquid chromatography tandem mass spectrum analysis method of indenes piperazine benfluralin and its four kinds of metabolins in a kind of soil, including
Following steps：
One, the indenes piperazine benfluralin and its four kinds of metabolins of known concentration gradient are established with high performance liquid chromatography tandem mass spectrometry
Soil matrix standard working curve, the foundation of the standard working curve includes the following steps：
(1) soil bare substrate extraction and cleaning liquid is prepared
The blank pedotheque that 2.00g is free of indenes piperazine benfluralin and its four kinds of metabolins after measured is weighed, 10mL water is added
With 10mL acetonitriles, mixing is added anhydrous magnesium sulfate 4g and sodium chloride 1g, mixing, after mechanical shaking extraction 30min, 5000rmp centrifugations
5min takes supernatant；
The above-mentioned supernatants of 5mL are taken, are put into advance added with 50mg silica gel and 150mg octadecyl silane adsorbents (C18)
In the centrifuge tube of powder, mixing, 10000rmp centrifuges 2min, is pipetted after centrifugation in 2mL supernatants to scale test tube, in 40 DEG C of water
Supernatant is slowly blown to 50 μ L in bath with nitrogen, acetonitrile is added and is settled to 1mL, cross 0.22 μm of filter membrane, obtain for preparing
The soil bare substrate extraction and cleaning liquid of indenes piperazine benfluralin and its four kinds of metabolins；
(2) indenes piperazine benfluralin and its four kinds of metabolins are prepared by solvent of obtained soil bare substrate extraction and cleaning liquid
Matrix hybrid standard working solution；
(3) soil matrix of the indenes piperazine benfluralin and its four kinds of metabolins is measured with high performance liquid chromatography tandem mass spectrometry
The extraction ion peak areas of each pesticide composition in hybrid standard working solution, with a concentration of abscissa, to extract ion peak areas
The standard working curve of indenes piperazine benfluralin and four kinds of metabolin pesticides is drawn out for ordinate；
Wherein determination condition is：Using electron spray (ESI) positive ion source, multiple-reaction monitoring pattern is quantified；Gas curtain gas
Press 30psi, 550 DEG C, capillary voltage 5500V, atomization gas pressure 50psi of ion source temperature, heating assist gas pressure power 50psi；
Chromatographic column uses the reverse phase C18 chromatographic columns of 2.7 μm of grain size；With 100% acetonitrile for A phases, 0.1% aqueous formic acid is B phases, by A
Mutually with B phases by volume 70：30 mixing are used as mobile phase；Flow velocity is set as 0.4mL/min, 35 DEG C of column temperature, sample size 5 μ L, other
Specific Mass Spectrometry Conditions are shown in Table 1；
The Mass Spectrometry Conditions of 1 indenes piperazine benfluralin of table and its four kinds of metabolins
Two, the residual quantity of indenes piperazine benfluralin and its four kinds of metabolins in pedotheque is measured, detection method includes following step
Suddenly：
(1) pedotheque is extracted；2.00g pedotheques are weighed, 10mL water is added, adds 10mL acetonitriles, are mixed
It is even；Add 4g anhydrous magnesium sulfates and 1g sodium chloride, mixing, after mechanical shaking extraction 30min, 5000rmp centrifuges 5min, takes supernatant
Liquid；
(2) the pedotheque extracting solution to be clean is purified；Take the above-mentioned supernatants of 5mL be put into advance added with
50mg silica gel and 150mg octadecyl silane adsorbents (C18) powder centrifuge tube in, mixing, 10000rmp centrifugation
2min is pipetted after centrifugation in 2mL supernatants to scale test tube, and supernatant is slowly blown to about 50 μ in 40 DEG C of water-baths with nitrogen
L adds acetonitrile and is settled to 1mL, after supernatant crosses 0.22 μm of filter membrane, obtains for measuring indenes piperazine benfluralin and its four kinds of metabolism
The pedotheque extraction and cleaning liquid of object residual quantity；
(3) with high performance liquid chromatography tandem mass spectrometry measure indenes piperazine benfluralin in the pedotheque extraction and cleaning liquid and
Its four kinds of metabolite residue amounts, record extraction ion chromatography peak area, matrix quantified by external standard method obtain the pedotheque extraction
The measured value of indenes piperazine benfluralin and its four kinds of metabolins in scavenging solution；The measured value is brought into quantitative calculation formula again,
Finally obtain indenes piperazine benfluralin to be measured and four kinds of metabolite residue amounts in pedotheque；
Quantitative calculation formula：W=(p × v × f)/m, in formula：W is indenes piperazine benfluralin to be measured and four kinds of metabolins in sample
Residual quantity, unit mg/kg；P is measured value, unit mg/L；M is the sample size weighed, unit g；V is constant volume,
Unit is mL；F is extension rate；
The chromatographic condition of indenes piperazine benfluralin and four kinds of metabolins in the wherein described pedotheque extraction and cleaning liquid with it is described
The chromatographic condition of indenes piperazine benfluralin and four kinds of metabolins in (3) of first part is identical.
The present invention has the following advantages and effects with respect to the prior art
1, the method for the present invention, sample pre-treatments are simple to operate, and consumption of organic solvent is few, and target pesticide recovery rate is high,
Good purification, and the Instrumental Analysis time is short.This method uses matrix solid phase dispersion abstraction technique and is carried out to target compound
Purification, then carries out Instrumental Analysis with high performance liquid chromatography tandem mass spectrometry and short chromatographic column, can be complete in 5min
At the measurement of sample, it is suitable for the quick detection and analysis of batch samples.
2, the instrument detection limit of the method for the present invention and method detection limit are very low.This method has used tandem mass spectrum detection
Device carries out quantitative detection using the electron spray ion source (ESI) and multiple-reaction monitoring pattern (MRM) and is looked for by optimizing parameters
Optimal quota ion pair is sought to obtain minimum instrument detection limit (LODs) and method detection limit (LOQs).
3, the present invention is by establishing the analysis method of indenes piperazine benfluralin and its four kinds of metabolins in the soil, can specify its
Transport And Transformation feature in Different Soil prevents from generating pollution to underground water.This method have quickly, conveniently, sensitivity
High feature.
Description of the drawings
Fig. 1 is the extraction chromatography of ions figure of 0.1mg/kg indenes piperazine benfluralin (Indaziflam) in soil matrix solution.
Fig. 2 is 0.1mg/kg indaziflams ketone metabolin (Indaziflam-triazine in soil matrix solution
Indanone extraction chromatography of ions figure).
Fig. 3 is 0.1mg/kg diamino triazine metabolite (Indaziflam- in soil matrix solution
Triazinediamine extraction chromatography of ions figure).
Fig. 4 is the extraction ion of 0.1mg/kg alkene metabolite (Indaziflam-olefin) in soil matrix solution
Chromatogram.
Fig. 5 is 0.1mg/kg carboxylic acids metabolite (Indaziflam-carnoxylic acid) in soil matrix solution
Extract chromatography of ions figure.
Fig. 6 is the extraction chromatography of ions figure of indenes piperazine benfluralin (Indaziflam) in pedotheque.
Specific implementation mode
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment
Pedotheque (picking up from Guangzhou, Guangdong Fanyu District Lan Hezhen) is acquired, with Liquid Chromatography-Tandem Mass Spectrometry method point
Indenes piperazine benfluralin and four kinds of metabolites in soil are analysed, are included the following steps：
One, the indenes piperazine benfluralin and its four kinds of metabolins of known concentration gradient are established with high performance liquid chromatography tandem mass spectrometry
Standard working curve, the foundation of the standard working curve comprises the steps of：
Indenes piperazine benfluralin (indaziflam, purity 99.5%), indaziflam ketone metabolin (indaziflam-
Triazine indanone, purity 94.9%), diamino triazine metabolite (indaziflam-triazinediamine,
Purity 96.4%), alkene metabolite (indaziflam-olefin, purity 94.8%) and carboxylic acid metabolite
(indaziflam-carnoxylic acid, purity 96.6%) metabolin is purchased from CHEM SERVICE companies.
(1) soil bare substrate extraction and cleaning liquid is prepared
It weighs 2.00g and is free of the blank pedotheque of tested indenes piperazine benfluralin and its four kinds of metabolins after measured in 50mL
Tool plug centrifuge tube in, be added 10mL water, 10mL acetonitriles, vortex mixing 2min, be added anhydrous magnesium sulfate 4g, sodium chloride 1g, whirlpool
After rotation mixing 2min, mechanical shaking extraction 30min, 5000rmp centrifuges 5min, takes supernatant；
The above-mentioned supernatants of 5mL are taken to be put into advance added with 50mg silica gel and 150mg octadecyl silane adsorbents (C18)
In the centrifuge tube of powder, vortex mixing 2min, 10000rmp centrifugation 2min is pipetted after centrifugation in 2mL supernatants to scale test tube,
Supernatant is slowly blown to 50 μ L in 40 DEG C of water-baths with nitrogen；Acetonitrile is added in supernatant again and is settled to 1mL, crosses 0.22 μm
Filter membrane obtains the soil bare substrate extraction and cleaning liquid for preparing indenes piperazine benfluralin and its four kinds of metabolins.
(2) indenes piperazine benfluralin and its four kinds are prepared as solvent using the bare substrate extraction and cleaning liquid obtained in the first step
The matrix hybrid standard working solution of metabolin, the wherein concentration range of indenes piperazine benfluralin and its four kinds of metabolins are 1-100 μ g/
L；
(3) matrix that the indenes piperazine benfluralin and its four kinds of metabolins are measured with high performance liquid chromatography tandem mass spectrometry mixes
The extraction ion peak areas of each pesticide composition in standard working solution is vertical to extract ion peak areas with a concentration of abscissa
Coordinate draws out the standard working curve of indenes piperazine benfluralin and four kinds of metabolins, and wherein determination condition is：Using electron spray (ESI)
Positive ion source, multiple-reaction monitoring pattern are quantified；Gas curtain air pressure 30psi, 550 DEG C of ion source temperature, capillary voltage
5500V, atomization gas pressure 50psi, heating assist gas pressure power 50psi；Chromatographic column uses the reverse phase C18 chromatographic columns of 2.7 μm of grain size；
With 100% acetonitrile for A phases, 0.1% aqueous formic acid is B phases, by A phases and B phases by volume 70：30 mixing are used as mobile phase；
Flow velocity is set as 0.4mL/min, 35 DEG C of column temperature, 5 μ L of sample size, and other specific Mass Spectrometry Conditions are shown in Table 1.
The standard working curve and quantification range of each compound, instrument detection limit (LODs) and method detection limit
(LOQs) 2 are shown in Table.
In matrix hybrid standard working solution, the chromatogram of indenes piperazine benfluralin parent and each metabolite is shown in Fig. 1-5.
Two, the indenes piperazine benfluralin in measurement pedotheque and its four kinds of metabolite residue amounts, detection method include following step
Suddenly：
(1) pedotheque is extracted：Pedotheque 2g is weighed, is placed in the tool plug centrifuge tube of 50mL, 10mL is added
Water adds 10mL acetonitriles, vortex mixing 2min；Add 4g anhydrous magnesium sulfates and 1g sodium chloride, vortex mixing 2min, oscillation
After extracting 30min, 5000rmp centrifuges 5min, takes supernatant；
(2) the pedotheque extracting solution to be clean is purified；Take the above-mentioned supernatants of 5mL be put into advance added with
50mg silica gel and 150mg octadecyl silane adsorbents (C18) powder centrifuge tube in, vortex mixing 2min, 10000rmp
2min is centrifuged, pipettes after centrifugation in 2mL supernatants to scale test tube, is slowly blown to supernatant about with nitrogen in 40 DEG C of water-baths
50μL；Acetonitrile is added in supernatant again and is settled to 1mL, after supernatant crosses 0.22 μm of filter membrane, obtains for measuring indenes piperazine fluorine grass
The pedotheque extraction and cleaning liquid of amine and four kinds of metabolite residues；
Silica gel described in step (2) and octadecyl silane adsorbent (C18) it is purchased from Town in Shanghai spectrum experiment high-tech stock
Part Co., Ltd.
(3) with high performance liquid chromatography tandem mass spectrometry measure indenes piperazine benfluralin in the pedotheque extraction and cleaning liquid and
Four kinds of metabolite residue amounts, record extraction ion chromatography peak area, quantified by external standard method obtain the pedotheque extraction and cleaning liquid
The measured value of middle indenes piperazine benfluralin and four kinds of metabolins；The measured value is brought into quantitative calculation formula again, is finally obtained
Indenes piperazine benfluralin to be measured and four kinds of metabolite residue amounts in pedotheque；
Quantitative calculation formula：W=(p × v × f)/m, in formula：W is indenes piperazine benfluralin to be measured and four kinds of metabolins in sample
Persticide residue, unit mg/kg；P is measured value, unit mg/L；M is the sample size weighed, unit g；V is constant volume body
Product, unit mL；F is extension rate；
The chromatographic condition of indenes piperazine benfluralin and four kinds of metabolins in the wherein described pedotheque extraction and cleaning liquid with it is described
The chromatographic condition of indenes piperazine benfluralin and four kinds of metabolins in (3) of first part is identical.
Fig. 6 is the extraction chromatography of ions figure of indenes piperazine benfluralin (Indaziflam) in pedotheque.
(4) according to the measured value of indenes piperazine benfluralin and four kinds of metabolins, according to quantitative equation, the indenes in pedotheque is found out
A concentration of 0.0422mg/kg of piperazine benfluralin, indaziflam ketone metabolin are not detected, and diamino triazine metabolite is not detected, alkene
Hydro carbons metabolin is not detected, and carboxylic acid metabolite is not detected.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (3)
1. the high performance liquid chromatography tandem mass spectrum analysis method of indenes piperazine benfluralin and its four kinds of metabolins, feature in a kind of soil
It is to include the following steps：
One, the indenes piperazine benfluralin of known concentration gradient and its soil of four kinds of metabolins are established with high performance liquid chromatography tandem mass spectrometry
Earth extraction standard working curve, the foundation of the standard working curve include the following steps：
(1) soil bare substrate extraction and cleaning liquid is prepared
Weigh the blank pedotheque that 2.00g is free of indenes piperazine benfluralin and its four kinds of metabolins after measured, be added 10mL water and
10mL acetonitriles, mixing are added anhydrous magnesium sulfate 4g and sodium chloride 1g, mixing, after mechanical shaking extraction 30min, 5000rmp centrifugations
5min takes supernatant；
Take the above-mentioned supernatants of 5mL, be put into advance added with 50mg silica gel and 150mg octadecyl silane absorbent powders from
In heart pipe, mixing, 10000rmp centrifuges 2min, is pipetted after centrifugation in 2mL supernatants to scale test tube, will be upper in 40 DEG C of water-baths
Clear liquid is slowly blown to 50 μ L with nitrogen, adds acetonitrile and is settled to 1mL, crosses 0.22 μm of filter membrane, obtains for preparing indenes piperazine fluorine grass
The soil bare substrate extraction and cleaning liquid of amine and its four kinds of metabolins；
(2) matrix of indenes piperazine benfluralin and its four kinds of metabolins is prepared using obtained soil bare substrate extraction and cleaning liquid as solvent
Hybrid standard working solution；
(3) soil matrix that the indenes piperazine benfluralin and its four kinds of metabolins are measured with high performance liquid chromatography tandem mass spectrometry mixes
The extraction ion peak areas of each pesticide composition in standard working solution is vertical to extract ion peak areas with a concentration of abscissa
Coordinate draws out the standard working curve of indenes piperazine benfluralin and four kinds of metabolin pesticides；
Two, the residual quantity of indenes piperazine benfluralin and its four kinds of metabolins in pedotheque is measured, detection method includes the following steps：
(1) pedotheque is extracted；2.00g pedotheques are weighed, 10mL water is added, adds 10mL acetonitriles, mixing；Again
It is added 4g anhydrous magnesium sulfates and 1g sodium chloride, mixing, after mechanical shaking extraction 30min, 5000rmp centrifuges 5min, takes supernatant；
(2) the pedotheque extracting solution to be clean is purified；The above-mentioned supernatants of 5mL are taken to be put into advance added with 50mg silicon
In the centrifuge tube of glue and 150mg octadecyl silane absorbent powders, mixing, 10000rmp centrifuges 2min, is moved after centrifugation
It takes in 2mL supernatants to scale test tube, supernatant is slowly blown to about 50 μ L in 40 DEG C of water-baths with nitrogen, it is fixed to add acetonitrile
Hold to 1mL, after supernatant crosses 0.22 μm of filter membrane, obtains the soil for measuring indenes piperazine benfluralin and its four kinds of metabolite residue amounts
Sample extraction scavenging solution；
(3) the indenes piperazine benfluralin and its four in the pedotheque extraction and cleaning liquid is measured with high performance liquid chromatography tandem mass spectrometry
Kind metabolite residue amount, record extraction ion chromatography peak area, matrix quantified by external standard method obtain the pedotheque extraction and cleaning
The measured value of indenes piperazine benfluralin and its four kinds of metabolins in liquid；The measured value is brought into quantitative calculation formula again, finally
Obtain indenes piperazine benfluralin to be measured and four kinds of metabolite residue amounts in pedotheque；
Quantitative calculation formula：W=(p × v × f)/m, in formula：W is indenes piperazine benfluralin to be measured and four kinds of metabolite residues in sample
Amount, unit mg/kg；P is measured value, unit mg/L；M is the sample size weighed, unit g；V is constant volume, unit
For mL；F is extension rate；
Mass Spectrometry Conditions involved by step 1 its (3) and step 2 its (3) are shown in Table 1；
The Mass Spectrometry Conditions of 1 indenes piperazine benfluralin of table and its four kinds of metabolins
2. according to the method described in claim 1, it is characterized in that：Measurement involved by step 1 its (3) and step 2 its (3)
Condition is：Using electron spray (ESI) positive ion source, multiple-reaction monitoring pattern is quantified；Gas curtain air pressure 30psi, ion source temperature
550 DEG C, capillary voltage 5500V, atomization gas pressure 50psi of degree, heating assist gas pressure power 50psi；Chromatographic column uses grain size 2.7
μm reverse phase C18 chromatographic columns；With 100% acetonitrile for A phases, 0.1% aqueous formic acid is B phases, by A phases and B phases by volume 70：
30 mixing are used as mobile phase；Flow velocity is set as 0.4mL/min, 35 DEG C of column temperature, 5 μ L of sample size.
3. according to the method described in claim 1, it is characterized in that：In step 1 its (2), matrix hybrid standard work
Solution, the wherein concentration range of indenes piperazine benfluralin and its four kinds of metabolins are 1-100 μ g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810521114.9A CN108732293B (en) | 2018-05-28 | 2018-05-28 | High performance liquid chromatography tandem mass spectrometry analysis method for indexazine flumioxazin and metabolites thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810521114.9A CN108732293B (en) | 2018-05-28 | 2018-05-28 | High performance liquid chromatography tandem mass spectrometry analysis method for indexazine flumioxazin and metabolites thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108732293A true CN108732293A (en) | 2018-11-02 |
| CN108732293B CN108732293B (en) | 2020-05-05 |
Family
ID=63936347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810521114.9A Active CN108732293B (en) | 2018-05-28 | 2018-05-28 | High performance liquid chromatography tandem mass spectrometry analysis method for indexazine flumioxazin and metabolites thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108732293B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114942293A (en) * | 2022-05-23 | 2022-08-26 | 江西农业大学 | Method for detecting trifluorosaflufenacil and metabolite M-12 thereof |
| CN115267019A (en) * | 2022-06-30 | 2022-11-01 | 广东省农业科学院植物保护研究所 | Ultra-high performance liquid chromatography tandem mass spectrometry analysis method for cyhalodiamide in fruits |
| US11585790B1 (en) | 2020-07-31 | 2023-02-21 | Pace Analytical Services, LLC | Analytical herbicide detection technology |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103329931A (en) * | 2013-07-25 | 2013-10-02 | 联保作物科技有限公司 | Weeding composition and preparation thereof |
| CN107820391A (en) * | 2015-05-11 | 2018-03-20 | 拜耳作物科学股份公司 | Herbicidal combination comprising L glufosinate-ammoniums and indaziflam grass amine |
-
2018
- 2018-05-28 CN CN201810521114.9A patent/CN108732293B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103329931A (en) * | 2013-07-25 | 2013-10-02 | 联保作物科技有限公司 | Weeding composition and preparation thereof |
| CN107820391A (en) * | 2015-05-11 | 2018-03-20 | 拜耳作物科学股份公司 | Herbicidal combination comprising L glufosinate-ammoniums and indaziflam grass amine |
Non-Patent Citations (3)
| Title |
|---|
| BRITTANY HOLMES ET AL.: "Single-Laboratory Ruggedness Testing and Validation of a Modified QuEChERS Approach To Quantify 185 Pesticide Residues in Salmon by Liquid Chromatography− and Gas Chromatography-Tandem Mass Spectrometry", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
| DIEGO G. ALONSO ET AL.: "Changes in sorption of indaziflam and three transformation products in soil with aging", 《GEODERMA》 * |
| PRATHIPATI REVATHI ET AL.: "Determination of Indaziflam and its metabolite residues in black grapes", 《INTERNATIONAL JOURNAL OF CHEMICAL STUDIES》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11585790B1 (en) | 2020-07-31 | 2023-02-21 | Pace Analytical Services, LLC | Analytical herbicide detection technology |
| CN114942293A (en) * | 2022-05-23 | 2022-08-26 | 江西农业大学 | Method for detecting trifluorosaflufenacil and metabolite M-12 thereof |
| CN115267019A (en) * | 2022-06-30 | 2022-11-01 | 广东省农业科学院植物保护研究所 | Ultra-high performance liquid chromatography tandem mass spectrometry analysis method for cyhalodiamide in fruits |
| CN115267019B (en) * | 2022-06-30 | 2024-03-22 | 广东省农业科学院植物保护研究所 | Ultra-high performance liquid chromatography tandem mass spectrometry analysis method for cyhalodiamide in fruits |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108732293B (en) | 2020-05-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104730186B (en) | Precolumn derivatization-UPLC(ultra performance liquid chromatography)-ESI(electronic spray ion)+-MS/MS (mass spectrometry) detection method of glyphosate and glufosinate-ammonium pesticide residue in tea | |
| CN106053703B (en) | It is a kind of at the same detect food in various plants growth regulator method | |
| CN108732293A (en) | The high performance liquid chromatography tandem mass spectrum analysis method of indenes piperazine benfluralin and its metabolin | |
| CN104569254B (en) | One grows tobacco and the assay method of Residual Levels of Organochlorine Pesticides in tobacco product | |
| Liu et al. | Magnetic solid phase extraction coupled with in situ derivatization for the highly sensitive determination of acidic phytohormones in rice leaves by UPLC-MS/MS | |
| CN106568873B (en) | The quantitative detecting method of Rynaxypyr residual quantity in a kind of soil | |
| CN115060839B (en) | Method for determining biscarfentrazone-ethyl metabolite based on liquid chromatography mass spectrometry | |
| CN108445133A (en) | A kind of method of glufosinate-ammonium and glyphosate drug residue in detection tealeaves | |
| CN108562673A (en) | A kind of ultra performance liquid chromatography tandem mass spectrum detection method measuring Ningnanmycin content in tomato | |
| Zhu et al. | Determination of gibberellins in soybean using tertiary amine labeling and capillary electrophoresis coupled with electrochemiluminescence detection | |
| CN103308641A (en) | High performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides in tobacco and tobacco products | |
| CN107907606A (en) | The method of a variety of herbicides in a kind of while quick detection soil | |
| CN109459506B (en) | Rapid sample pretreatment method for detecting polychlorinated biphenyl in tea | |
| Benedé et al. | Carbon fibers as green and sustainable sorbent for the extraction of isoflavones from environmental waters | |
| CN108760963A (en) | The high performance liquid chromatography tandem mass spectrum analysis method of pyraclostrobin and its metabolin | |
| CN108020627B (en) | Method for determining residual quantity of three phenoxy carboxylic acid pesticides in tobacco by ultra-high performance synthetic phase chromatography-tandem mass spectrometry | |
| CN105319285B (en) | The assay method of fluorine telomeric alcohol (FTOHs) carboxylic acids catabolite in soil and plant | |
| Zhang et al. | Extraction of acetanilide herbicides in naked oat (Avena nuda L.) by using ionic‐liquid‐based matrix solid‐phase dispersion‐foam flotation solid‐phase extraction | |
| CN102944621A (en) | Method for determining residual quantity of fosetyl-aluminium in environmental sample | |
| CN106404507A (en) | Leaf vegetable gibberellins residue detection sample pretreatment method and detection method | |
| CN115166114B (en) | Method for detecting metamorphic substances of pyraclonil in water or soil | |
| CN111366659A (en) | Method for detecting trace PFOA (perfluorooctanoic acid) in powdery fluoropolymer product | |
| CN104280495A (en) | Method for detecting validamycin A in water and rice plants | |
| CN106645486A (en) | Method for measuring residual quantity of glyphosate in soil employing liquid chromatography-high-resolution mass spectrometer | |
| CN113295800B (en) | Method for determining fluorosulfonyl-Lin metabolite by combined phase chromatography tandem mass spectrometry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20181102 Assignee: Guangdong Voda Testing Technology Co.,Ltd. Assignor: PLANT PROTECTION Research Institute GUANGDONG ACADEMY OF AGRICULTURAL SCIENCES Contract record no.: X2022440000126 Denomination of invention: High performance liquid chromatography tandem mass spectrometry analysis method of indazine fluorachlor and its metabolites Granted publication date: 20200505 License type: Common License Record date: 20220909 |
|
| EE01 | Entry into force of recordation of patent licensing contract |