CN108490098A - The non-targeted quick screening method of unknown pesticide residue in a kind of white wine - Google Patents
The non-targeted quick screening method of unknown pesticide residue in a kind of white wine Download PDFInfo
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- CN108490098A CN108490098A CN201810485544.XA CN201810485544A CN108490098A CN 108490098 A CN108490098 A CN 108490098A CN 201810485544 A CN201810485544 A CN 201810485544A CN 108490098 A CN108490098 A CN 108490098A
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- G—PHYSICS
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- 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
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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
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- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
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Abstract
The invention discloses a kind of non-targeted quick screening methods of unknown pesticide residue in white wine, ethyl alcohol is removed using being concentrated in vacuo, it is concentrated again through HLB Solid Phase Extraction column purifications, UPLC Q Tof detections, it is matched using the accurate mass number of unknown object compound characteristic quasi-molecular ions, daughter fragment ion information, isotope matching, retention time and database, searches suspicious pesticide residue.Screening analysis white wine specificity of the present invention is strong, it is easy to operate, quick and precisely, analysis type it is abundant, can be that quick analyze of white wine pesticide residue provide scientific method with quality control.
Description
Technical field
The present invention relates to a kind of non-targeted quick screening methods of unknown pesticide residue in white wine, belong to analysis and detection technology
Field.
Background technology
With the popularization of agricultural production, pesticide has become in agricultural modernization production extremely important one
Point.Pesticide is most important for crops elimination insect pest, the yield of increase agricultural.But just because of this, persticide residue is exceeded tight
A series of weight, to cause environment serious problems.Pesticide residue can not only destroy natural environment, also will have a direct impact on the mankind
Health.It is in addition native since Farming process needs the drugs such as herbicide spraying, insecticide, fungicide, auxin
Earth, water source may also cause pesticide to be remained in grain by pollution by pesticides.Although the degradable part pesticide of fermentation,
Be the organic matters such as the ethyl alcohol in white wine has good dissolubility to specific pesticide, leads to pesticide residue in wine, threatens consumption
The health and life security of person.Therefore, it is very necessary to establish the remaining detection method of pesticide in white wine.
With generally answering for the technologies such as gas chromatography-mass spectrography (GC-MS), liquid chromatograph mass spectrography (LC-MS)
With detection technique is rapidly developed pesticide multi-residues simultaneously.With the height that quadrupole rod series connection flight mass spectrum (Q-Tof) is representative
There is Resolution Mass Spectrometry high resolution, accurate mass number to measure, can be to the change in complex matrices under full scan the advantages that high sensitivity
It closes object and carries out qualitative confirmation.Since Q-Tof has high sweep speed, it can not have to consider the limitation on compound amounts, realize big
Measure pesticide screening high-throughput simultaneously.It can also be by the accurate mass number of compound and retention time, isotope intensity, isotope point
The information such as cloth, secondary fragment combine, with specific compound database matching realization pesticide without standard items rapid screening.Therefore,
Q-Tof is widely used in the screening and confirmation of fruits and vegetables, soil, tealeaves and Pesticide Residues.
But the matrix of Wine Sample is complicated, contains 2,000 lot of trace ingredients, it not only can jamming target object (pesticide chemical combination
Object) analysis, and fatal damage can be caused to chromatographic column and mass spectrum, therefore how effectively extract object and to purify removal white
Interference impurity in wine becomes a problem of urgent need to resolve.
Invention content
To solve the above-mentioned problems, the present invention provides a kind of non-targeted rapid screening sides of unknown pesticide residue in white wine
Method.The method of the present invention Screening analysis white wine specificity is strong, it is easy to operate, quick and precisely, analysis type it is abundant, can be white wine pesticide
Remaining quick analysis and quality control provide scientific method.
The non-targeted quick screening method of unknown pesticide residue in white wine of the present invention removes second using vacuum concentration first
Alcohol, then concentrated through HLB Solid Phase Extraction column purifications, UPLC-Q-Tof detections utilize the essence of unknown object compound characteristic quasi-molecular ions
True mass number, daughter fragment ion information, isotope matching, retention time and database are matched, and pesticide residue information is obtained.
The non-targeted quick screening method of unknown pesticide residue, includes the following steps in white wine of the present invention：
Step 1：Sample pre-treatments
Take white wine sample 500mL in evaporative flask, 40 DEG C, rotating speed 120r/min of evaporating temperature, concentrated by rotary evaporation to 200mL,
It takes out spare；It takes the activation of 3mL methanol to balance pillar in HLB solid-phase extraction columns, then with 3mL ultra-pure waters, will then be concentrated into 200mL
White wine sample the solid-phase extraction column of activation is continued through with the speed of 5mL/min, then 2mL deionized waters is used to elute, taken out true
The dry solid-phase extraction column of sky, discards efflux, finally 5mL methanol is used to elute solid-phase extraction column, collects eluent, as to be measured
Liquid；
Step 2：UPLC-Q-Tof is detected
Prepare liquid detaches pesticide residue compound by ultra performance liquid chromatography system, using equipped with electron spray
The UPLC-Q-Tof of ion source, is respectively adopted MSEES+ and ES- both of which to the parent ion and daughter ion data of prepare liquid
Information is acquired, and is detected to pesticide residue compound；
Step 3：Pesticide screening
By MSEThe prepare liquid parent ion and daughter ion data information combination UNFI softwares that type collection obtains use science number
Screening is carried out to pesticide according to library, scientific library is according to accurate parent ion quality, retention time, fragment ion and isotope
Model and intensity are identified that rapid evaluation analysis obtains the information of unknown pesticide residue component (m/z).
The testing conditions setting of step 2 is as follows：
Chromatographic condition：
Chromatographic column：ACQUITY UPLC Ben C18Column, 2.1mm × 100mm, 1.7 μm；
Mobile phase：A phases are water, and B phases are acetonitrile, gradient elution；
Gradient elution program is：0~0.5min：95%A+5%B；0.5~5.5min：5%A+5%B；5.5min~
6.5min：5%A+95%B；6.5~6.6min：95%A+5%B；6.6~10min：95%A+5%B.
Flow velocity：0.4mL/min,
Sample size：5μL；
Column temperature：30℃；
Mass Spectrometry Conditions：
G2-S QTof mass spectrographs, acquisition mode：MSEPattern；
ESI+ ionizes mode condition：Capillary voltage：3.0kV；Sample orifice potential：40V；Ion source temperature：120℃；
Desolventizing temperature：450℃；Desolvation gas flow velocity：1000L/H；Reference mass：Leucine enkephalin [M+H] +=
556.2766；
ESI- ionizes mode condition：Capillary voltage：2.5kV；Sample orifice potential：40V；Ion source temperature：120℃；
Desolventizing temperature：450℃；Desolvation gas flow velocity：1000L/H；Reference mass：Leucine enkephalin [M-H] -=
554.2615。
Acquisition range：M/z 50~1200；Low energy collisions energy：4eV；High energy gradual change collision energy：10~45eV.
In step 3, retrieval parameter is：Retention time range of search is ± 0.02min, and accurate mass deviation is 5mDa, from
Sonization formal character+H and-H patterns.
Compared with prior art, beneficial effects of the present invention are embodied in：
The present invention, which uses, chooses to install evaporation-HLB as pretreatment mode, high to the pesticide residue rate of recovery, stability is good, Neng Gouyou
Effect removal interfering substance, while white wine middle peasant's medicine residual is carried out quickly without standard items qualitatively screening using UPLC-Q-Tof.
The method of the present invention is quick and analysis throughput is high, can be that the remaining rapid screening of pesticide and quality control carry in white wine
For important method foundation.
Description of the drawings
Fig. 1 is that chlopyrifos (Chlorpyrifos) selects ion flow graph (a) and mass spectrogram (b).
Fig. 2 is the residual total ion current figure of 18 special quality control agricultures.
Fig. 3 is the MS that blank wine sample adds MathionEPattern UNIFI composes storehouse matching the selection result sectional drawing, and wherein a is screening
As a result summarize, b is that Mathion extracts chromatography of ions figure, and c is parent ion and fragment ion hum pattern.
Specific implementation mode
Of the invention for ease of understanding, with reference to specific embodiment, the invention will be further described.
Embodiment：
1.1 reagents, drug
Trace standard of pesticide substance (purity>95%, Town in Shanghai spectrum), it is single to mark stock solution (400ug/L), matched by acetonitrile
System, -20 DEG C are kept in dark place.
1.2 instrument and equipment
Waters ACQUITYI-Class systemsG2-XS QTof mass spectrographs are furnished with electric spray ion source
(ESI)；Switzerland walks fine jade R-210 vacuum and rotates evaporimeter；CNW Poly-Sery HLB HLB solid-phase extraction columns；
1.3 sample pre-treatments
Take white wine sample 500mL in evaporative flask, 40 DEG C, rotating speed 120r/min of evaporating temperature, concentrated by rotary evaporation to 200mL,
It takes out spare；It takes the activation of 3mL methanol to balance pillar in HLB solid-phase extraction columns, then with 3mL ultra-pure waters, will then be concentrated into 200mL
White wine sample the solid-phase extraction column of activation is continued through with the speed of 5mL/min, then 2mL deionized waters is used to elute, taken out true
The dry solid-phase extraction column 5min of sky, discards efflux, finally 5mL methanol is used to elute solid-phase extraction column, collect eluent, as wait for
Liquid is surveyed, is detected for UPLC-Q-Tof；
1.4UPLC-Q-Tof detection
Prepare liquid detaches pesticide residue compound by ultra performance liquid chromatography system, using equipped with electron spray
The UPLC-Q-Tof of ion source, is respectively adopted MSEES+ and ES- both of which to the parent ion and daughter ion data of prepare liquid
Information is acquired, and is detected to pesticide residue compound；
Chromatographic condition：
Chromatographic column：ACQUITY UPLC Ben C18Column, 2.1mm × 100mm, 1.7 μm；
Mobile phase：A phases are water, and B phases are acetonitrile, gradient elution；
Gradient elution program is 0~0.5min：95%A+5%B；0.5~5.5min：5%A+5%B；5.5min~
6.5min：5%A+95%B；6.5~6.6min：95%A+5%B；6.6~10min：95%A+5%B.
Flow velocity：0.4mL/min,
Sample size：5μL；
Column temperature：30℃；
Mass Spectrometry Conditions：
G2-S QTof mass spectrographs, acquisition mode：MSEPattern；
ESI+ ionizes mode condition：Capillary voltage：3.0kV；Sample orifice potential：40V；Ion source temperature：120℃；
Desolventizing temperature：450℃；Desolvation gas flow velocity：1000L/H；Reference mass：Leucine enkephalin [M+H] +=
556.2766；
ESI- ionizes mode condition：Capillary voltage：2.5kV；Sample orifice potential：40V；Ion source temperature：120℃；
Desolventizing temperature：450℃；Desolvation gas flow velocity：1000L/H；Reference mass：Leucine enkephalin [M-H] -=
554.2615。
Acquisition range：M/z 50~1200；Low energy collisions energy：4eV；High energy gradual change collision energy：10~45eV.
1.5 screening method：Using MSEPattern acquires parent ion and daughter ion number under ES+ and ES- ionization patterns respectively
It is believed that breath, as a contrast, screening, section are carried out to pesticide using scientific library in conjunction with UNFI softwares without the residual ultra-pure water of agriculture
Database root is learned to be identified according to accurate parent ion quality, retention time, fragment ion and isotope model and intensity,
The information of rapid evaluation unknown component (m/z).
2. results and discussion
The rate of recovery and stability of 2.1 sample-pretreating methods
The matrix of Wine Sample is complicated, contains 2,000 lot of trace ingredients, not only can jamming target object (agricultural chemical compound)
Analysis, and fatal damage can be caused to chromatographic column and mass spectrum, therefore how effectively extract object and purify removal white wine
In interference impurity become urgent need to resolve a problem.This experiment is first using the overwhelming majority in being concentrated in vacuo in removal white wine
Ethyl alcohol, then extracted by CNW Poly-Sery HLB HLB Solid Phase Extraction column purifications, then to the accuracy and repeatability of this method
It is evaluated, by taking chlopyrifos as an example, MSEAppearance time is 5.05min under scanning, ES+ ionization patterns, and second order ms icon closes
+ H patterns are specifically shown in Fig. 1 (a is to select ion flow graph, b for mass spectrogram), under 100,200 and 400ug/L pitch-based spheres, recycling
Rate is in 80~115% ranges, and RSD<10% (n=5).Experimental result illustrates the accuracy and repeatability of pre-treating method
Well, the how remaining screening of pesticide and detection in white wine be can be applied to.
2.2 detecting the optimization of parameter
This method screening is used without the residual ultra-pure water of agriculture as a control group, be can remove notable false positive results, is further included
Retention time range of search is ± 0.02min, and accurate mass deviation is 5mDa, ionized form selection+H and-H patterns.
The quality control method of 2.3 non-targeted rapid screening pesticide residues
18 special quality control pesticide Acetochlor, Atrazine, Chlorpyrifos, Chlorpyrifos-methyl,
Diazinon、Dichlorvos、Dimethoate、ETHION、Machette、Malathion、Methlaxyl、MEVINPHOS、
Mocap, Phosmet, Primethanil, Quinalphos, Tetramethrin, P, P'-DDD are carried out under 1.4 experiment conditions
Experiment, the residual total ion current figure of 18 special quality control agricultures are shown in that Fig. 2, experimental data see the table below.
The spectrum analysis of 2.4 screening positives
By taking certain 50 degree commercially available white wine addition 400ug/L Mathion (malathion) interpretations of result as an example, in sample
Mathion appearance times are 4.02min, remove the false positive results in reference substance it is found that the sample only has a kind of agricultures of Mathion
Medicine remains, and as a result seeing Fig. 3, (a summarizes for screening results, and b is that Mathion extracts chromatography of ions figure, and c is parent ion and fragment ion
Hum pattern).The experimental results showed that UPLC-Q-Tof systems and related pesticide database, screening used by present invention institute are soft
The technologies such as part, retention time locking can accurately and reliably realize that pesticide residue is screened in white wine.
Claims (4)
1. the non-targeted quick screening method of unknown pesticide residue in a kind of white wine, it is characterised in that include the following steps：
Step 1：Sample pre-treatments
Take white wine sample 500mL in evaporative flask, 40 DEG C, rotating speed 120r/min of evaporating temperature, concentrated by rotary evaporation to 200mL is taken out
It is spare；It takes the activation of 3mL methanol to balance pillar in HLB solid-phase extraction columns, then with 3mL ultra-pure waters, will then be concentrated into the white of 200mL
Wine sample continues through the solid-phase extraction column of activation with the speed of 5mL/min, then 2mL deionized waters is used to elute, vacuumized dry
Dry solid-phase extraction column discards efflux, finally 5mL methanol is used to elute solid-phase extraction column, collects eluent, as prepare liquid；
Step 2：UPLC-Q-Tof is detected
Prepare liquid detaches pesticide residue compound by ultra performance liquid chromatography system, using equipped with electron spray ion
The UPLC-Q-Tof in source, is respectively adopted MSEES+ and ES- both of which to the parent ion and daughter ion data information of prepare liquid
It is acquired, pesticide residue compound is detected；
Step 3：Pesticide screening
By MSEThe prepare liquid parent ion and daughter ion data information combination UNFI softwares that type collection obtains use scientific library
Screening is carried out to pesticide, scientific library is according to accurate parent ion quality, retention time, fragment ion and isotope model
And intensity is identified, rapid evaluation analysis obtains the information of unknown pesticide residue component m/z.
2. according to the method described in claim 1, it is characterized in that：
The testing conditions setting of step 2 is as follows：
Chromatographic condition：
Chromatographic column：ACQUITY UPLC Ben C18Column, 2.1mm × 100mm, 1.7 μm；
Mobile phase：A phases are water, and B phases are acetonitrile, gradient elution；
Flow velocity：0.4mL/min,
Sample size：5μL；
Column temperature：30℃；
Mass Spectrometry Conditions：
G2-S QTof mass spectrographs, acquisition mode：MSEPattern；
ESI+ ionizes mode condition：Capillary voltage：3.0kV；Sample orifice potential：40V；Ion source temperature：120℃；Precipitation
Agent temperature：450℃；Desolvation gas flow velocity：1000L/H；Reference mass：Leucine enkephalin [M+H] +=556.2766；
ESI- ionizes mode condition：Capillary voltage：2.5kV；Sample orifice potential：40V；Ion source temperature：120℃；Precipitation
Agent temperature：450℃；Desolvation gas flow velocity：1000L/H；Reference mass：Leucine enkephalin [M-H] -=554.2615；
Acquisition range：M/z 50~1200；Low energy collisions energy：4eV；High energy gradual change collision energy：10~45eV.
3. according to the method described in claim 2, it is characterized in that：
Gradient elution program is：0~0.5min：95%A+5%B；0.5~5.5min：5%A+5%B；5.5min~6.5min：
5%A+95%B；6.5~6.6min：95%A+5%B；6.6~10min：95%A+5%B.
4. according to the method described in claim 1, it is characterized in that：
In step 3, retrieval parameter is：Retention time range of search is ± 0.02min, and accurate mass deviation is 5mDa, ionization
Formal character+H and-H patterns.
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| CN109856282A (en) * | 2019-03-11 | 2019-06-07 | 安徽瑞思威尔科技有限公司 | The quick screening method of external source hazardous material in a kind of white wine |
| CN112924590A (en) * | 2021-01-29 | 2021-06-08 | 浙江大学 | Non-targeted rapid screening method for soil pesticide by adopting GC/LC-QTOF |
| CN113574629A (en) * | 2019-03-22 | 2021-10-29 | Dh科技发展私人贸易有限公司 | Unknown Compound elution assay |
| WO2022262132A1 (en) * | 2021-06-18 | 2022-12-22 | 北京格竹生物科技有限公司 | Non-targeted analysis method for unknown component in sample by using liquid chromatography-mass spectrometry |
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| CN108490098B (en) | 2020-05-05 |
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