CN108760963A - The high performance liquid chromatography tandem mass spectrum analysis method of pyraclostrobin and its metabolin - Google Patents
The high performance liquid chromatography tandem mass spectrum analysis method of pyraclostrobin and its metabolin Download PDFInfo
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- CN108760963A CN108760963A CN201810520648.XA CN201810520648A CN108760963A CN 108760963 A CN108760963 A CN 108760963A CN 201810520648 A CN201810520648 A CN 201810520648A CN 108760963 A CN108760963 A CN 108760963A
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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
- G01N30/96—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
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—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
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Abstract
The invention discloses the high performance liquid chromatography tandem mass spectrum analysis methods of pyraclostrobin in lichee and its metabolin, and this approach includes the following steps：The lichee matrix hybrid standard working solution for preparing pyraclostrobin and its metabolin, establishes the standard working curve of pyraclostrobin and its metabolin；The pyraclostrobin and its metabolite residue amount in lichee sample extraction scavenging solution 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 pyraclostrobin and metabolin in the lichee sample extraction scavenging solution；The measured value is brought into quantitative calculation formula again, finally obtains pyraclostrobin and metabolite residue amount to be measured in lichee sample.Pyraclostrobin and its accurate qualitative, quantitative of metabolin can be improved the accuracy and sensitivity of method by the method for the present invention by the selection ion and matrix matching standard solution of second order ms.
Description
Technical field
The invention belongs to analytical chemistry fields, and in particular to the high-efficient liquid phase color of pyraclostrobin and its metabolin in lichee
Compose Tandem Mass Spectrometry Analysis method, this method simplicity, quick, favorable reproducibility, high sensitivity.
Background technology
Pyraclostrobin is a kind of methoxy acrylic bactericide of BASF Aktiengesellschaft's exploitation, is had good
Protection, treatment and conduction, downy mildew, powdery mildew, leaf spot etc. for preventing fruit tree, the mechanism of action are to pass through prevention
The electron transmission of cytochrome b c1 complexs and inhibit mitochondrial respiratory to act on.
At present about the report of pyraclostrobin, pyraclostrobin parent is concentrated mainly in works such as cucumber, apple, citruses
Research on object, temporarily without the relevant report on lichee；Its main metabolites BF 500-3 are rarely reported, and there are no on lichee
Correlative study.
Lichee is the Important Economic crop in China tropical and subtropical zone area, and China is the area of origin of lichee, Guangdong, Guangxi,
Hainan, Fujian etc. are its main producing regions.Peronophythora litchi is before and after the lichee florescence, fruiting period etc. is a large amount of occurs, and is to influence lichee production
The important disease of amount and quality.Pyraclostrobin is main chemical prevention medicament, year usage amount it is big, the master in plant
It is BF 500-3 to want metabolite.
The chemical structural formula of pyraclostrobin and its metabolin is as follows：
Litchi pulp sugar content is high, and pericarp pigment, flavones equal size are more, therefore, requires height to its pre-treating method, needs
The interference of the impurity such as carbohydrate and pigment can preferably be removed to ensure that the peak type of target compound is symmetrical, to meet analysis method
Accuracy, reproducibility requirement.
The residual quantity of pyraclostrobin is defined as pyraclostrobin parent and its metabolin by Canada and the U.S. at present
The sum of BF 500-3, Chinese residual quantity definition are still pyraclostrobin parent.Therefore, carry out pyraclostrobin and its metabolin exists
Research of residue analysis method on lichee is very necessary and urgent, and this method can be used as the prison of 2 kinds of harmful substances in the fruits and vegetables of market
It surveys, assesses its potential dietary int ake risk.
Invention content
It is largely used on lichee for current pyraclostrobin, but the present situation of analysis method missing, the purpose of the present invention
It is to provide the high performance liquid chromatography tandem mass spectrum analysis method of pyraclostrobin and its metabolin in a kind of lichee.
The purpose of the invention is achieved by the following technical solution：
The high performance liquid chromatography tandem mass spectrum analysis method of pyraclostrobin and its metabolin in lichee, including following step
Suddenly：
(1) the lichee matrix hybrid standard working solution of pyraclostrobin and its metabolin is prepared：
Weighing 2.00g, the blank lichee sample of pyraclostrobin-containing and its metabolin, addition 10mL acetonitriles do not mix after measured
It is even, anhydrous magnesium sulfate 1g and sodium chloride 1g is added, extraction of ocean eddies 5min, 5000rmp centrifugation 5min takes supernatant；
The above-mentioned supernatants of 5mL are taken to be put into advance added with ethylenediamine N- propyl silanes (PSA) and octadecyl silane
(C18) filler centrifuge tube in, mixing, 10000rmp centrifuge 2min, pipetted after centrifugation in 2mL supernatants to scale test tube, 40
Supernatant is slowly blown to 50 μ L with nitrogen in DEG C water-bath；Acetonitrile is added in supernatant again and is settled to 1mL, crosses 0.22 μm of filter
Film obtains bare substrate extraction and cleaning liquid；Pyraclostrobin and its metabolin are prepared by solvent of bare substrate extraction and cleaning liquid
Lichee matrix hybrid standard working solution；
(2) the matrix hybrid standard that pyraclostrobin and its metabolin are measured with high performance liquid chromatography tandem mass spectrometry works
The extraction ion peak areas of each pesticide composition in solution is drawn using extracting ion peak areas as ordinate with a concentration of abscissa
Go out the standard working curve of pyraclostrobin and its metabolin；
Wherein determination condition is：Using electron spray positive ion source, multiple-reaction monitoring pattern is quantified；Gas curtain air pressure
30psi, ion source temperature are 550 DEG C, capillary voltage 5500V, spray pressure power 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
Mutually with B phases by volume 75:25 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.It is other
Specific Mass Spectrometry Conditions are shown in Table 1；
The Mass Spectrometry Conditions of 1 pyraclostrobin of table and its metabolin
(3) pyraclostrobin and its metabolite residue amount in lichee sample are measured, detection method includes the following steps：
Lichee sample is extracted；Lichee sample 2.00g is weighed, 10mL acetonitriles are added, continuously add 1g anhydrous slufuric acids
Magnesium and 1g sodium chloride, extraction of ocean eddies 1min, 5000rmp centrifugation 5min, take supernatant；
The lichee sample extracting solution to be clean is purified；The above-mentioned supernatants of 5mL are taken to be put into advance added with 150mg
PSA and 150mg C18In the centrifuge tube of filler, vortex mixing 1min, 10000rmp centrifugation 2min pipettes 2mL supernatants after centrifugation
Into scale test tube, supernatant is slowly blown to about 50 μ L in 40 DEG C of water-baths with nitrogen；It is fixed that acetonitrile is added in supernatant again
Hold to 1mL, after supernatant crosses 0.22 μm of filter membrane, obtains carrying for measuring the lichee sample of pyraclostrobin and its metabolite residue
Take scavenging solution；
(4) with high performance liquid chromatography tandem mass spectrometry measure pyraclostrobin in the lichee sample extraction scavenging solution and
Its metabolite residue amount, record extraction ion chromatography peak area, matrix quantified by external standard method obtain the lichee sample extraction purification
The measured value of pyraclostrobin and metabolin in liquid；The measured value is brought into quantitative calculation formula again, finally obtains litchi
Pyraclostrobin and metabolite residue amount to be measured in branch sample；
Quantitative calculation formula：W=(p × v × f)/m, in formula：W is pyraclostrobin and metabolite residue to be measured 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；
The chromatographic condition of pyraclostrobin and its metabolin in the wherein described lichee sample extraction scavenging solution and step (2)
In pyraclostrobin and its metabolin chromatographic condition it is identical.
The present invention has the following advantages and effects with respect to the prior art：
(1) using the pre-treating method of the present invention, consumption of organic solvent is few, and the recovery rate of target pesticide is high, operating procedure
Simply, the rate of recovery of good purification, pyraclostrobin and its metabolin is high.
(2) of the invention to use instrument HPLC-MS/MS, by applying shorter chromatogram column, shorten sample detection analysis time,
Improve detection efficiency；It can be by pyraclostrobin and its metabolism by the selection ion and matrix matching standard solution of second order ms
The accurate qualitative, quantitative of object, improves the accuracy and sensitivity of method, the LOD of this method pyraclostrobin and BF 500-3 and
LOQ is below fish body (0.5 μ g/kg and 1 μ g/kg), corn (0.45-5.00 μ g/kg and 1-20 μ g/kg).
Description of the drawings
Fig. 1 is the extraction chromatography of ions figure of 0.1mg/L pyraclostrobins in matrix solution.
Fig. 2 is the extraction chromatography of ions figure of 0.1mg/L BF 500-3 in matrix solution.
Fig. 3 is the extraction chromatography of ions figure of pyraclostrobin in lichee sample.
Fig. 4 is the extraction chromatography of ions figure of BF 500-3 in lichee sample.
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
Lichee sample is acquired, analyzes pyraclostrobin and its metabolin in lichee with the method for the present invention, including following
Step：
(1) the lichee matrix hybrid standard working solution of pyraclostrobin and metabolin is prepared：
Weighing 2.00g, the blank lichee sample of pyraclostrobin-containing and its metabolin is not centrifuged in the tool plug of 50mL after measured
Guan Zhong, is added 10mL acetonitriles, and anhydrous magnesium sulfate 1g, sodium chloride 1g, extraction of ocean eddies 5min, 5000rmp is added in vortex mixing 2min
5min is centrifuged, supernatant is taken；
The above-mentioned supernatants of 5mL are taken to be put into advance added with ethylenediamine N- propyl silanes (PSA) and octadecyl silane
(C18) filler centrifuge tube in, vortex mixing 2min, 10000rmp centrifuge 2min, and 2mL supernatants to scale is pipetted after centrifugation and is tried
Supernatant is slowly blown to 50 μ L by Guan Zhong in 40 DEG C of water-baths with nitrogen；Acetonitrile is added in supernatant again and is settled to 1mL, mistake
0.22 μm of filter membrane obtains the lichee bare substrate extraction and cleaning liquid for preparing pyraclostrobin and metabolin.With lichee blank
Matrix extraction and cleaning liquid is the lichee matrix hybrid standard working solution that solvent prepares pyraclostrobin and its metabolin.
Wherein pyraclostrobin (purity 99.5%) is purchased from Chem Service companies of the U.S., BF 500-3 (purity
99.9%) Chem Service companies of the U.S. are purchased from.
In the lichee matrix hybrid standard working solution of step (1) described series concentration, concentration range is 1-100 μ g/L；
(2) the lichee matrix that the pyraclostrobin and its metabolin 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 pyraclostrobin and metabolin；
Wherein determination condition is：Using electron spray (ESI) positive ion source, multiple-reaction monitoring pattern is quantified；Nitrogen stream
Speed is 10L/min, and temperature is 300 DEG C；Nebulizer pressure is 30psi；Capillary voltage is 5500V；Chromatographic column uses grain size 2.7
μm reverse phase C18 chromatographic columns；Mobile phase is the aqueous formic acid (75/25) of acetonitrile and 0.1% (volume ratio), and flow velocity is set as
0.4mL/min, 35 DEG C of column temperature, 5 μ L of sample size, other specific Mass Spectrometry Conditions are shown in Table 1.
The lichee extraction standard solution chromatographic mass spectrometry figure of pyraclostrobin and metabolite is shown in Fig. 1 and Fig. 2.
(3) pyraclostrobin and metabolite residue amount described in lichee sample are measured, detection method includes the following steps：
Lichee sample is extracted；Lichee sample 2.00g is weighed, is placed in the tool plug centrifuge tube of 50mL, 10mL is added
Acetonitrile, continuously adds 1g anhydrous magnesium sulfates and 1g sodium chloride, and extraction of ocean eddies 1min, 5000rmp centrifugation 5min takes supernatant；
The lichee sample extracting solution to be clean is purified；The above-mentioned supernatants of 5mL are taken to be put into advance added with 150mg
PSA and 150mg C18In the centrifuge tube of filler, vortex mixing 1min, 10000rmp centrifugation 2min pipettes 2mL supernatants after centrifugation
Into scale test tube, supernatant is slowly blown to about 50 μ L in 40 DEG C of water-baths with nitrogen；It is fixed that acetonitrile is added in supernatant again
Hold to 1mL, after supernatant crosses 0.22 μm of filter membrane, obtains the lichee sample extraction for measuring pyraclostrobin and metabolite residue
Scavenging solution；
Ethylenediamine N- propyl silanes (PSA) described in step (3) and octadecyl silane (C18) adsorbent is purchased from
Town in Shanghai spectrum experiment Science and Technology Co., Ltd..
(4) with high performance liquid chromatography tandem mass spectrometry measure pyraclostrobin in the lichee sample extraction scavenging solution and
Metabolite residue amount, record extraction ion chromatography peak area, matrix quantified by external standard method obtain the lichee sample extraction scavenging solution
The measured value of middle pyraclostrobin and metabolin；The measured value is brought into quantitative calculation formula again, finally obtains lichee
Pyraclostrobin and metabolite residue amount to be measured in sample；
Quantitative calculation formula：W=(p × v × f)/m, in formula：W is pyraclostrobin and metabolite residue to be measured 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；
The chromatographic condition of pyraclostrobin and its metabolin in the wherein described lichee sample extraction scavenging solution and step (2)
In pyraclostrobin it is identical with the chromatographic condition of metabolin.
The chromatographic mass spectrometry figure of pyraclostrobin and metabolite is shown in Fig. 3 and Fig. 4 in lichee sample.
(5) according to the measured value of pyraclostrobin and metabolin, according to quantitative equation, the pyrazoles ether in lichee sample is found out
Bacterium ester concentration is 0.330mg/kg, a concentration of 0.048mg/kg of metabolin BF 500-3.
The matrix hybrid standard working curve and quantification range of each compound, instrument detection limit (LODs) and method inspection
It surveys limit (LOQs) and is shown in Table 2.
Table 2：The relevant parameters such as the matrix hybrid standard working curve of pyraclostrobin and BF 500-3
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 pyraclostrobin and its metabolin in lichee, it is characterised in that including
Following steps：
(1) the lichee matrix hybrid standard working solution of pyraclostrobin and its metabolin is prepared：
2.00g not blank lichee samples of pyraclostrobin-containing and its metabolin after measured are weighed, are added 10mL acetonitriles, mixing,
Anhydrous magnesium sulfate 1g and sodium chloride 1g is added, extraction of ocean eddies 5min, 5000rmp centrifugation 5min takes supernatant；
The above-mentioned supernatants of 5mL are taken to be put into advance added with the centrifuge tube of ethylenediamine N- propyl silanes and octadecyl silane filler
In, mixing, 10000rmp centrifuges 2min, is pipetted after centrifugation in 2mL supernatants to scale test tube, by supernatant in 40 DEG C of water-baths
50 μ L are slowly blown to nitrogen；Acetonitrile is added in supernatant again and is settled to 1mL, crosses 0.22 μm of filter membrane, obtains bare substrate and carry
Take scavenging solution；The lichee matrix hybrid standard of pyraclostrobin and its metabolin is prepared using bare substrate extraction and cleaning liquid as solvent
Working solution；
(2) the matrix hybrid standard working solution of pyraclostrobin and its metabolin is measured with high performance liquid chromatography tandem mass spectrometry
In the extraction ion peak areas of each pesticide composition pyrrole is drawn out as ordinate to extract ion peak areas with a concentration of abscissa
The standard working curve of azoles kresoxim-methyl and its metabolin；
(3) pyraclostrobin and its metabolite residue amount in lichee sample are measured, detection method includes the following steps：
Lichee sample is extracted；Weigh lichee sample 2.00g, 10mL acetonitriles be added, continuously add 1g anhydrous magnesium sulfates and
1g sodium chloride, extraction of ocean eddies 1min, 5000rmp centrifugation 5min, takes supernatant；
The lichee sample extracting solution to be clean is purified；The above-mentioned supernatants of 5mL are taken to be put into advance added with 150mg PSA
With 150mg C18In the centrifuge tube of filler, vortex mixing 1min, 10000rmp centrifugation 2min pipettes 2mL supernatants extremely after centrifugation
In scale test tube, supernatant is slowly blown to about 50 μ L in 40 DEG C of water-baths with nitrogen；Acetonitrile constant volume is added in supernatant again
To 1mL, after supernatant crosses 0.22 μm of filter membrane, the lichee sample extraction for measuring pyraclostrobin and its metabolite residue is obtained
Scavenging solution；
(4) pyraclostrobin and its generation in the lichee sample extraction scavenging solution are measured with high performance liquid chromatography tandem mass spectrometry
Object residual quantity, record extraction ion chromatography peak area are thanked, matrix quantified by external standard method obtains in the lichee sample extraction scavenging solution
The measured value of pyraclostrobin and metabolin；The measured value is brought into quantitative calculation formula again, finally obtains lichee sample
Pyraclostrobin and metabolite residue amount to be measured in product；
Quantitative calculation formula：W=(p × v × f)/m, in formula：W is pyraclostrobin and metabolite residue amount to be measured in sample, single
Position is mg/kg；P is measured value, unit mg/L；M is the sample size weighed, unit g；V is constant volume, unit mL；f
For extension rate；
In step (2) and (4), involved Mass Spectrometry Conditions are shown in Table 1；
The Mass Spectrometry Conditions of 1 pyraclostrobin of table and its metabolin
2. according to the method described in claim 1, it is characterized in that：In step (2) and (4), involved determination condition is：It adopts
With electron spray positive ion source, multiple-reaction monitoring pattern is quantified；Gas curtain air pressure 30psi, ion source temperature are 550 DEG C, capillary
Tube voltage 5500V, spray pressure power 50psi, heating assist gas pressure power 50psi；Chromatographic column uses the reverse phase C18 of 2.7 μm of grain size
Chromatographic column；With 100% acetonitrile for A phases, 0.1% aqueous formic acid is B phases, by A phases and B phases by volume 75:25 mixing conducts
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：Lichee matrix hybrid standard work described in step (1) is molten
In liquid, the concentration range of pyraclostrobin and its metabolin is 1-100 μ g/L.
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Cited By (3)
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| CN113848270A (en) * | 2021-10-12 | 2021-12-28 | 中国科学院动物研究所 | Method for detecting pyraclostrobin, fluxapyroxad and fluxad metabolite in peanut kernel and peanut straw |
| CN115201353A (en) * | 2022-06-16 | 2022-10-18 | 广州海关技术中心 | Method for detecting residual quantity of kresoxim-methyl in vegetables and fruits |
| 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 |
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| CN113848270A (en) * | 2021-10-12 | 2021-12-28 | 中国科学院动物研究所 | Method for detecting pyraclostrobin, fluxapyroxad and fluxad metabolite in peanut kernel and peanut straw |
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| 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 |
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Application publication date: 20181106 |