CN107037155A - Simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins method - Google Patents
Simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins method Download PDFInfo
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Abstract
Simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins method, it be related to it is a kind of and meanwhile in extracting and enriching water typical four kinds of Taste and odor compounds and three kinds of Algae toxins method.It is larger the invention aims to solve existing method poor reproducibility, consumption of organic solvent, occur emulsion in extraction process, it is impossible to while carrying out the technical problem of extracting and enriching.This method is as follows：First, it will be adjusted after the processing of target water sample suction filtration to acidity；2nd, solid-phase extraction column is activated and cleaned；3rd, elute and elute Taste and odor compounds；4th, elute and elute Algae toxins.5th, concentration is carried out to Taste and odor compounds and Algae toxins respectively.Emulsion will not be produced The present invention reduces the consumption of organic solvent, and in processing procedure, the time used is short, efficiency high, preci-sion and accuracy is high, filled up in water environment while the blank of extracting and enriching and quantitative Taste and odor compounds and Algae toxins.The invention belongs to the abstraction technique field of pollutant.
Description
Technical field
The present invention relates to it is a kind of and meanwhile in extracting and enriching water typical four kinds of Taste and odor compounds and three kinds of Algae toxins method.
Background technology
As body eutrophication is aggravated, planktonic organism especially algal blooms in natural water, algal grown generation
Thank to generation Taste and odor compounds, the dead rupture of algae can produce the pollutants such as Microcystin, deteriorate water quality.If being used as drink
Water water source is used, drinking water quality will be had a strong impact on by dealing with improperly.It is difficult to adapt to the water quality condition that becomes increasingly complex now and more
Strict water standard, it is difficult to ensure the safety of drinking water.And some existing method for extracting and enriching, there is poor reproducibility, have
Machine solvent load is larger, occurs emulsion in extraction process, it is impossible to while the problems such as carrying out extracting and enriching, sets up new quick
The method of contained Taste and odor compounds and Microcystin in efficient Sync enrichment extraction water environment, to ensure the environment matter of people
Amount is made efforts with safety and contribution is particularly important.
The content of the invention
It is larger the invention aims to solve existing method poor reproducibility, consumption of organic solvent, go out in extraction process
Existing emulsion, it is impossible to while carrying out the technical problem of extracting and enriching there is provided one kind while typical in extracting and enriching gauge water
Four kinds of Taste and odor compounds and three kinds of Algae toxins method.
While the method for typical four kinds of Taste and odor compounds and three kinds of Algae toxins is according to following steps in extracting and enriching gauge water
Carry out：
First, it will be adjusted after the processing of target water sample suction filtration to acidity；
2nd, solid-phase extraction column is activated and cleaned：
C18 solid-phase extraction columns are used, sampling volume is 0.1L-5L, and 500mg stationary phases, C18 solid-phase extraction columns use 5mL successively
Dichloromethane, 5mL methanol and 5mL high purity waters, in the flow velocity activation and rinse C18 solid-phase extraction columns with 1mL/min-5mL/min
C18 fillers；
3rd, the target water sample handled by step one is passed through by step 2 with 1ml/min-10ml/min speed
The C18 solid-phase extraction columns of reason, then vacuum drain the moisture in C18 solid-phase extraction columns；
4th, elute and elute Taste and odor compounds：
Use 5ml dichloromethane to be eluted with 1ml/min-6ml/min elution flow rates to C18 solid-phase extraction columns, collect odor
Material eluent, addition dehydrates the extract after agent, suck dry moisture, is put into rotary evaporator and is concentrated, after concentration
Liquid to be purged with nitrogen to volume be below 1mL, be transferred in Agilent special-purpose bottle, carried out with gas chromatography-mass spectrometry
Detect Taste and odor compounds；
5th, elute and elute Algae toxins：
The C18 solid-phase extraction columns first handled with the methanol solution elution of 5ml volume fractions 20% by step 4, then use
The methanol solution of 5ml volume fractions 80% is eluted to solid-phase extraction column, and elution flow rate is 1ml/min-6ml/min, is obtained
Microcystin eluent, Microcystin eluent rotary evaporator is concentrated, the liquid after concentration is blown with nitrogen
Volume is swept to for below 0.5mL, is transferred in Agilent special-purpose bottle, is carried out detection Algae toxins with high performance liquid chromatography, that is, complete
Typical four kinds of Taste and odor compounds and three kinds of Algae toxins in extracting and enriching gauge water simultaneously.
The present invention is with four kinds of Taste and odor compounds：Ground depth, 2- methyl isoborneols, β-cyclocitral, alpha, beta-lonone；Three kinds of algaes
Toxin：Microcapsule phycotoxin MC-LR, Microcystin MC-YR and Microcystin MC-RR are research object, have studied it in water
In simultaneously extracting and enriching and quantitative assay method.By target water sample suction filtration, regulation to acid pH, using extraction efficiency height, choosing
The good solid-phase extraction column of selecting property is extracted, the different elution of reasonable employment and eluting solvent, and different eluents is entered respectively
Row processing, by Taste and odor compounds eluent, adds after the extract for dehydrating and being filtered after agent, suck dry moisture, is put into rotary evaporation
Device is concentrated；It is below 1mL that liquid after concentration, which is purged with nitrogen to volume,；It is transferred in Agilent special-purpose bottle, uses gas
Phase chromatograph-mass spectrometer is detected.By Microcystin eluent without drying, rotary evaporator progress is directly placed into
Concentration；It is below 0.5mL that liquid after concentration, which is purged with nitrogen to volume, is transferred in Agilent special-purpose bottle；Use efficient liquid
Phase chromatogram is detected, that is, completes detection.
The invention provides rapidly and efficiently while extracting and enriching water environment in contained Taste and odor compounds and Microcystin
Method.The emulsification that similar liquid-liquid extraction will not be produced The present invention reduces the consumption of organic solvent, and in processing procedure shows
As the time used is short, efficiency high, and preci-sion and accuracy is high, has filled up in water environment while extracting and enriching and quantitative odor thing
The blank of matter and Algae toxins.
The emulsification that similar liquid-liquid extraction will not be produced The present invention reduces the consumption of organic solvent, and in processing procedure shows
As the time used is short, efficiency high, and preci-sion and accuracy is high, has filled up in water environment while extracting and enriching and quantitative odor thing
The blank of matter and Algae toxins.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment
Any combination.
Embodiment one：Present embodiment typical four kinds of Taste and odor compounds and three kinds in extracting and enriching gauge water simultaneously
The method of Algae toxins is followed the steps below：
First, it will be adjusted after the processing of target water sample suction filtration to acidity；
2nd, solid-phase extraction column is activated and cleaned：
Using C18 solid-phase extraction columns, sampling volume is 0.1L-5L, and 500mg stationary phases, C18 solid-phase extraction columns are used successively
5mL dichloromethane, 5mL methanol and 5mL high purity waters, flow velocity activation and rinse C18 solid-phase extraction columns with 1mL/min-5mL/min
In C18 fillers；
3rd, the target water sample handled by step one is passed through by step 2 with 1ml/min-10ml/min speed
The C18 solid-phase extraction columns of reason, then vacuum drain the moisture in C18 solid-phase extraction columns；
4th, elute and elute Taste and odor compounds：
Use 5ml dichloromethane to be eluted with 1ml/min-6ml/min elution flow rates to C18 solid-phase extraction columns, collect odor
Material eluent, addition dehydrates the extract after agent, suck dry moisture, is put into rotary evaporator and is concentrated, after concentration
Liquid to be purged with nitrogen to volume be below 1mL, be transferred in Agilent special-purpose bottle, carried out with gas chromatography-mass spectrometry
Detect Taste and odor compounds；
5th, elute and elute Algae toxins：
The C18 solid-phase extraction columns first handled with the methanol solution elution of 5ml volume fractions 20% by step 4, then use
The methanol solution of 5ml volume fractions 80% is eluted to solid-phase extraction column, and elution flow rate is 1ml/min-6ml/min, is obtained
Microcystin eluent, Microcystin eluent rotary evaporator is concentrated, the liquid after concentration is blown with nitrogen
Volume is swept to for below 0.5mL, is transferred in Agilent special-purpose bottle, is carried out detection Algae toxins with high performance liquid chromatography, that is, complete
Typical four kinds of Taste and odor compounds and three kinds of Algae toxins in extracting and enriching gauge water simultaneously.
Embodiment two：Present embodiment from unlike embodiment one described in step one by target water
It is 4-5 to be adjusted after the processing of sample suction filtration to pH value.It is other identical with embodiment one.
Embodiment three：Unlike one of present embodiment and embodiment one or two described in step 2
Sample introduction optimization volume is 1L.It is other identical with one of embodiment one or two.
Embodiment four：In step 2 unlike one of present embodiment and embodiment one to three with
2mL/min-4mL/min flow velocity activation and rinse C18 solid-phase extraction columns.Other phases one of with embodiment one to three
Together.
Embodiment five：In step 2 unlike one of present embodiment and embodiment one to four with
3mL/min flow velocity activation and rinse C18 solid-phase extraction columns.It is other identical with one of embodiment one to four.
Embodiment six：Will be through in step 3 unlike one of present embodiment and embodiment one to five
The target water sample for crossing step one processing passes through the C18 SPEs by step 2 processing with 3ml/min-8ml/min speed
Post.It is other identical with one of embodiment one to five.
Embodiment seven：Dichloro in step 4 unlike one of present embodiment and embodiment one to six
Methane is eluted with 1ml/min.It is other identical with one of embodiment one to six.
Embodiment eight：Used in step 4 unlike one of present embodiment and embodiment one to seven
Agilent GC7890N-MSD 6973N are detected, sample are separated using HP-5MS chromatographic columns, with gradient increased temperature program
HP-5MS chromatographic columns are heated up, initial temperature is 50 DEG C of holding 3min, with 5 DEG C/min-The programming rate of heating rises to 150
DEG C keep 2min, 300 DEG C carry out purification chromatographic columns, injector temperature be 250 DEG C, with not shunt mode sample introduction, interface temperature
280 DEG C, mass spectrum uses EI patterns, and ionizing energy is 70eV, and 230 DEG C of temperature carries out qualitative point using full scan pattern to sample
Analysis, m/z scopes are 50-500.It is other identical with one of embodiment one to seven.
Embodiment nine：Eluted in step 5 unlike one of present embodiment and embodiment one to eight
Flow velocity is 1ml/min.It is other identical with one of embodiment one to eight.
Embodiment ten：Step 5 unlike one of present embodiment and embodiment one to nine uses liquid
Chromatography Agilent 1260LC；Zorbax Eclipse XDB-C18 chromatographic columns, mobile phase is 0.05% trifluoroacetic acid
The aqueous solution and acetonitrile, according to 67:33 volume ratio composition, flow velocity is 1.0mL/min, 30 DEG C of detection temperature, sample size 50uL, inspection
Survey wavelength 238nm.It is other identical with one of embodiment one to nine.
Using following experimental verifications effect of the present invention：
Experiment one：
While the method for typical four kinds of Taste and odor compounds and three kinds of Algae toxins is according to following steps in extracting and enriching gauge water
Carry out：
First, it is 4 by regulation pH value after the processing of target water sample suction filtration；
2nd, solid-phase extraction column is activated and cleaned：
Using C18 solid-phase extraction columns, sampling volume is 1L, and 500mg stationary phases add 5mL bis- into C18 solid-phase extraction columns
Chloromethanes, 5mL methanol and 5mL high purity waters, the C18 fillers in flow velocity activation and rinse C18 solid-phase extraction columns with 2mL/min；
3rd, the target water sample handled by step one is consolidated with 5ml/min speed by the C18 handled by step 2
Phase extraction column, then vacuum drain the moisture in C18 solid-phase extraction columns；
4th, elute and elute Taste and odor compounds：
Use 5ml dichloromethane to be eluted with 1ml/min elution flow rates to C18 solid-phase extraction columns, collect Taste and odor compounds elution
Liquid, addition dehydrates the extract after agent, suck dry moisture, is put into rotary evaporator and is concentrated, and the liquid after concentration is used
It is below 1mL that nitrogen, which is purged to volume, is transferred in Agilent special-purpose bottle, is detected with gas chromatography-mass spectrometry；
Analysis detection is carried out to Taste and odor compounds extraction sample using Agilent GC7890N-MSD 6973N.With high-pure helium
Gas is carrier gas, and flow velocity is 1.0mL min-1；Sample is divided using HP-5MS (30m × 0.25mm × 0.25 μm) chromatographic column
From；Chromatographic column is heated up with gradient increased temperature program, initial temperature is 50 DEG C (keeping 3min), is warming up to 5 DEG C/min
150 DEG C (keeping 2min), purification chromatographic column is carried out at 300 DEG C；Injector temperature is 250 DEG C, with not shunt mode sample introduction；Interface
280 DEG C of temperature；Mass spectrum uses EI patterns, and ionizing energy is 70eV, 230 DEG C of temperature；Sample is determined using full scan pattern
Property analysis (m/z scopes be 50-500).
5th, elute and elute Algae toxins：
The C18 solid-phase extraction columns first handled with the methanol solution elution of 5ml volume fractions 20% by step 4, then use
The methanol solution of 5ml volume fractions 80% is eluted to solid-phase extraction column, and elution flow rate is 1ml/min, obtains microcystin
Plain eluent, Microcystin eluent rotary evaporator is concentrated, the liquid after concentration is purged with nitrogen to volume
For below 0.5mL, it is transferred in Agilent special-purpose bottle, is detected with high performance liquid chromatography；
Using liquid chromatograph Agilent 1260LC；Zorbax Eclipse XDB-C18 (4.6 × 150mm, 5um) color
Compose post；238nm Detection wavelengths；Mobile phase is that mass concentration is 0.05% trifluoroacetic acid aqueous solution with acetonitrile according to 67:33 body
Product is than composition；Flow velocity is 1.0mL/min；30 DEG C of detection temperature；Sample size 50uL.
Experiment two：
While the method for typical four kinds of Taste and odor compounds and three kinds of Algae toxins is according to following steps in extracting and enriching gauge water
Carry out：
First, it is 4 by regulation pH value after the processing of target water sample suction filtration；
2nd, solid-phase extraction column is activated and cleaned：
Using C18 solid-phase extraction columns, sampling volume is 0.1L-5L, and 500mg stationary phases, C18 solid-phase extraction columns are used successively
5mL dichloromethane, 5mL methanol and 5mL high purity waters, flow velocity activation and rinse C18 solid-phase extraction columns with 1mL/min-5mL/min
In C18 fillers；
3rd, the target water sample handled by step one is consolidated with 2ml/min speed by the C18 handled by step 2
Phase extraction column, then vacuum drain the moisture in C18 solid-phase extraction columns；
4th, elute and elute Taste and odor compounds：
Use 5ml dichloromethane to be eluted with 5ml/min elution flow rates to C18 solid-phase extraction columns, collect Taste and odor compounds elution
Liquid, addition dehydrates the extract after agent, suck dry moisture, is put into rotary evaporator and is concentrated, and the liquid after concentration is used
It is below 1mL that nitrogen, which is purged to volume, is transferred in Agilent special-purpose bottle, is detected with gas chromatography-mass spectrometry；
Analysis detection is carried out to Taste and odor compounds extraction sample using Agilent GC7890N-MSD 6973N.With high-pure helium
Gas is carrier gas, and flow velocity is 1.0mL min-1；Sample is divided using HP-5MS (30m × 0.25mm × 0.25 μm) chromatographic column
From；Chromatographic column is heated up with gradient increased temperature program, initial temperature is 50 DEG C (keeping 3min), is warming up to 5 DEG C/min
150 DEG C (keeping 2min), purification chromatographic column is carried out at 300 DEG C；Injector temperature is 250 DEG C, with not shunt mode sample introduction；Interface
280 DEG C of temperature；Mass spectrum uses EI patterns, and ionizing energy is 70eV, 230 DEG C of temperature；Sample is determined using full scan pattern
Property analysis (m/z scopes be 50-500).
5th, elute and elute Algae toxins：
The C18 solid-phase extraction columns first handled with the methanol solution elution of 5ml volume fractions 20% by step 4, then use
The methanol solution of 5ml volume fractions 80% is eluted to solid-phase extraction column, and elution flow rate is 2ml/min, obtains microcystin
Plain eluent, Microcystin eluent rotary evaporator is concentrated, the liquid after concentration is purged with nitrogen to volume
For below 0.5mL, it is transferred in Agilent special-purpose bottle, is detected with high performance liquid chromatography；
Using liquid chromatograph Agilent 1260LC；Zorbax Eclipse XDB-C18 (4.6 × 150mm, 5um) color
Compose post；238nm Detection wavelengths；Mobile phase is that mass concentration is 0.05% trifluoroacetic acid aqueous solution with acetonitrile according to 67:33 body
Product is than composition；Flow velocity is 1.0mL/min；30 DEG C of detection temperature；Sample size 50uL.
Experiment three：
While the method for typical four kinds of Taste and odor compounds and three kinds of Algae toxins is according to following steps in extracting and enriching gauge water
Carry out：
First, it is 4 by regulation pH value after the processing of target water sample suction filtration；
2nd, solid-phase extraction column is activated and cleaned：
Using C18 solid-phase extraction columns, sampling volume is 0.1L-5L, and 500mg stationary phases, C18 solid-phase extraction columns are used successively
5mL dichloromethane, 5mL methanol and 5mL high purity waters, flow velocity activation and rinse C18 solid-phase extraction columns with 1mL/min-5mL/min
In C18 fillers；
3rd, the target water sample handled by step one is consolidated with 8ml/min speed by the C18 handled by step 2
Phase extraction column, then vacuum drain the moisture in C18 solid-phase extraction columns；
4th, elute and elute Taste and odor compounds：
Use 5ml dichloromethane to be eluted with 4ml/min elution flow rates to C18 solid-phase extraction columns, collect Taste and odor compounds elution
Liquid, addition dehydrates the extract after agent, suck dry moisture, is put into rotary evaporator and is concentrated, and the liquid after concentration is used
It is below 1mL that nitrogen, which is purged to volume, is transferred in Agilent special-purpose bottle, is detected with gas chromatography-mass spectrometry；
Analysis detection is carried out to Taste and odor compounds extraction sample using Agilent GC7890N-MSD 6973N.With high-pure helium
Gas is carrier gas, and flow velocity is 1.0mL min-1；Sample is divided using HP-5MS (30m × 0.25mm × 0.25 μm) chromatographic column
From；Chromatographic column is heated up with gradient increased temperature program, initial temperature is 50 DEG C (keeping 3min), is warming up to 5 DEG C/min
150 DEG C (keeping 2min), purification chromatographic column is carried out at 300 DEG C；Injector temperature is 250 DEG C, with not shunt mode sample introduction；Interface
280 DEG C of temperature；Mass spectrum uses EI patterns, and ionizing energy is 70eV, 230 DEG C of temperature；Sample is determined using full scan pattern
Property analysis (m/z scopes be 50-500).
5th, elute and elute Algae toxins：
The C18 solid-phase extraction columns first handled with the methanol solution elution of 5ml volume fractions 20% by step 4, then use
The methanol solution of 5ml volume fractions 80% is eluted to solid-phase extraction column, and elution flow rate is 6ml/min, obtains microcystin
Plain eluent, Microcystin eluent rotary evaporator is concentrated, the liquid after concentration is purged with nitrogen to volume
For below 0.5mL, it is transferred in Agilent special-purpose bottle, is detected with high performance liquid chromatography；
Using liquid chromatograph Agilent 1260LC；Zorbax Eclipse XDB-C18 (4.6 × 150mm, 5um) color
Compose post；238nm Detection wavelengths；Mobile phase is that mass concentration is 0.05% trifluoroacetic acid aqueous solution with acetonitrile according to 67:33 body
Product is than composition；Flow velocity is 1.0mL/min；30 DEG C of detection temperature；Sample size 50uL.
Experiment one to three pairs of Taste and odor compounds of experiment and Algae toxins carry out extracting and enriching, the gas phase after optimizing respectively simultaneously
Chromatographic mass spectrometry and efficient liquid phase chromatographic analysis condition, set up the working curve of object, while having carried out recovery of standard addition and essence
Density experiment, its result is as shown in the table.
Table 1
Claims (10)
1. simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins method, it is characterised in that simultaneously
The method of typical four kinds of Taste and odor compounds and three kinds of Algae toxins is followed the steps below in extracting and enriching gauge water：
First, it will be adjusted after the processing of target water sample suction filtration to acidity；
2nd, solid-phase extraction column is activated and cleaned：
Using C18 solid-phase extraction columns, sampling volume is 0.1L-5L, and 500mg stationary phases, C18 solid-phase extraction columns use 5mL bis- successively
Chloromethanes, 5mL methanol and 5mL high purity waters, in the flow velocity activation and rinse C18 solid-phase extraction columns with 1mL/min-5mL/min
C18 fillers；
3rd, the target water sample handled by step one is passed through by step 2 processing with 1ml/min-10ml/min speed
C18 solid-phase extraction columns, then vacuum drain the moisture in C18 solid-phase extraction columns；
4th, elute and elute Taste and odor compounds：
Use 5ml dichloromethane to be eluted with 1ml/min-6ml/min elution flow rates to C18 solid-phase extraction columns, collect Taste and odor compounds
Eluent, addition dehydrates the extract after agent, suck dry moisture, is put into rotary evaporator and is concentrated, by the liquid after concentration
It is below 1mL that body, which is purged with nitrogen to volume, is transferred in Agilent special-purpose bottle, is detected with gas chromatography-mass spectrometry
Taste and odor compounds；
5th, elute and elute Algae toxins：
The C18 solid-phase extraction columns first handled with the methanol solution elution of 5ml volume fractions 20% by step 4, then use 5ml bodies
The methanol solution of fraction 80% is eluted to solid-phase extraction column, and elution flow rate is 1ml/min-6ml/min, obtains Microcystis aeruginosa
Toxin eluent liquid, Microcystin eluent rotary evaporator is concentrated, the liquid after concentration is purged with nitrogen to body
Product is below 0.5mL, is transferred in Agilent special-purpose bottle, detection Algae toxins are carried out with high performance liquid chromatography, that is, completes to extract simultaneously
Take typical four kinds of Taste and odor compounds and three kinds of Algae toxins in enrichment gauge water.
2. according to claim 1 simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins side
Method, it is characterised in that it is 4-5 to be adjusted after target water sample suction filtration is handled described in step one to pH value.
3. according to claim 1 simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins side
Method, it is characterised in that the optimization volume of sample introduction described in step 2 is 1L.
4. according to claim 1 simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins side
Method, it is characterised in that the flow velocity activation with 2mL/min-4mL/min and rinse C18 solid-phase extraction columns in step 2.
5. according to claim 1 simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins side
Method, it is characterised in that the flow velocity activation with 3mL/min and rinse C18 solid-phase extraction columns in step 2.
6. according to claim 1 simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins side
Method, it is characterised in that the target water sample handled by step one is passed through into warp with 3ml/min-8ml/min speed in step 3
Cross the C18 solid-phase extraction columns of step 2 processing.
7. according to claim 1 simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins side
Method, it is characterised in that dichloromethane is eluted with 1ml/min in step 4.
8. according to claim 1 simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins side
Method, it is characterised in that the detection of Taste and odor compounds in step 4：Detected using Agilent GC7890N-MSD 6973N, using HP-
5MS chromatographic columns are separated to sample, and HP-5MS chromatographic columns are heated up with gradient increased temperature program, and initial temperature is 50 DEG C
3min is kept, with 5 DEG C/min-The programming rate of heating rises to 150 DEG C of holding 2min, and purification chromatographic column, sample introduction are carried out at 300 DEG C
Mouth temperature is 250 DEG C, with not shunt mode sample introduction, 280 DEG C of interface temperature, and mass spectrum uses EI patterns, and ionizing energy is 70eV, temperature
230 DEG C of degree, qualitative analysis is carried out to sample using full scan pattern, and m/z scopes are 50-500.
9. according to claim 1 simultaneously in extracting and enriching gauge water typical four kinds of Taste and odor compounds and three kinds of Algae toxins side
Method, it is characterised in that elution flow rate is 1ml/min in step 5.
10. typical four kinds of Taste and odor compounds and three kinds of Algae toxins in extracting and enriching gauge water simultaneously according to claim 1
Method, it is characterised in that the detection of step 5 Algae toxins：Using liquid chromatograph Agilent 1260LC；Zorbax Eclipse
XDB-C18 chromatographic columns, mobile phase is 0.05% trifluoroacetic acid aqueous solution and acetonitrile, according to 67:33- volume ratio composition, flow velocity
For 1.0mL/min, 30 DEG C of detection temperature, sample size 50u L, Detection wavelength 238nm.
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| CN112730650A (en) * | 2020-12-15 | 2021-04-30 | 湖南微谱检测技术有限公司 | Method for enriching ultra-trace organic matters in large-volume water |
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| CN112730650A (en) * | 2020-12-15 | 2021-04-30 | 湖南微谱检测技术有限公司 | Method for enriching ultra-trace organic matters in large-volume water |
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