CN107037155B - 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 is related to a kind of method of typical four kinds of Taste and odor compounds and three kinds of algae toxins in extracting and enriching water simultaneously.The purpose of the present invention is to solve existing method poor reproducibility, consumption of organic solvent are larger, the technical issues of occurring emulsion in extraction process, extracting and enriching cannot be carried out simultaneously.This method is as follows: one, will be adjusted to acidity after the processing of target water sample suction filtration；Two, solid-phase extraction column is activated and is cleaned；Three, elute and elute Taste and odor compounds；Four, elute and elute algae toxin.Five, concentration is carried out to Taste and odor compounds and algae toxin respectively.The present invention reduces the dosages of organic solvent, and emulsion will not be generated in treatment process, and the time used is short, high-efficient, and preci-sion and accuracy is high, have filled up extracting and enriching and the quantitatively blank of Taste and odor compounds and algae toxin simultaneously in water environment.The invention belongs to the abstraction technique fields of pollutant.
Description
Technical field
The present invention relates to a kind of methods of typical four kinds of Taste and odor compounds and three kinds of algae toxins in extracting and enriching water simultaneously.
Background technique
As water eutrophication aggravates, planktonic organism especially algal blooms in natural water, algal grown generation
Thank to generation Taste and odor compounds, the dead rupture of algae can generate the pollutants such as Microcystin, deteriorate water quality.If as drink
With water water source, deals with improperly and will seriously affect drinking water quality.It is difficult to adapt to the water quality condition that becomes increasingly complex now and more
Stringent water standard, it is difficult to guarantee the safety of drinking water.And existing some method for extracting and enriching, there are poor reproducibilities, have
The problems such as solvent dosage is larger, occurs emulsion in extraction process, cannot carry out extracting and enriching simultaneously is established novel quick
The method of Taste and odor compounds and Microcystin contained in efficient Sync enrichment extraction water environment, for the environment matter for ensureing people
Amount is made efforts with safety and contribution is particularly important.
Summary of the invention
The purpose of the present invention is to solve existing method poor reproducibility, consumption of organic solvent are larger, go out in extraction process
The technical issues of showing emulsion, cannot carrying out extracting and enriching simultaneously provides typical in a kind of while extracting and enriching gauge water
Four kinds of Taste and odor compounds and three kinds of algae toxins method.
The method of typical four kinds of Taste and odor compounds and three kinds of algae toxins is according to the following steps in extracting and enriching gauge water simultaneously
It carries out:
One, acidity will be adjusted to after the processing of target water sample suction filtration；
Two, solid-phase extraction column is activated and is cleaned:
With C18 solid-phase extraction column, sampling volume 0.1L-5L, 500mg stationary phase, C18 solid-phase extraction column successively uses 5mL
Methylene chloride, 5mL methanol and 5mL high purity water, in the flow velocity activation of 1mL/min-5mL/min and rinse C18 solid-phase extraction column
C18 filler；
Three, will be passed through with the speed of 1ml/min-10ml/min by step 2 by the target water sample of step 1 processing
The C18 solid-phase extraction column of reason, then vacuum drain the moisture in C18 solid-phase extraction column；
Four, it elutes and elutes Taste and odor compounds:
It uses 5ml methylene chloride to elute with 1ml/min-6ml/min elution flow rate to C18 solid-phase extraction column, collects odor
Substance eluent, is added dehydration and drying agent, and the extract liquor after suck dry moisture is put into rotary evaporator and is concentrated, after concentration
Liquid to be purged with nitrogen to volume be 1mL hereinafter, being transferred in Agilent special-purpose bottle, carried out with gas chromatography-mass spectrometry
Detect Taste and odor compounds；
Five, it elutes and elutes algae toxin:
The first C18 solid-phase extraction column with the methanol solution elution of 5ml volume fraction 20% by step 4 processing, then use
The methanol solution of 5ml volume fraction 80% elutes solid-phase extraction column, and elution flow rate 1ml/min-6ml/min is obtained
Microcystin eluent rotary evaporator is concentrated, the liquid after concentration is blown with nitrogen by Microcystin eluent
Being swept to volume is 0.5mL hereinafter, being transferred in Agilent special-purpose bottle, carries out detection algae toxin with high performance liquid chromatography, that is, completes
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 isoborneol, β-cyclocitral, alpha, beta-lonone；Three seeds 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 measuring method.By target water sample suction filtration, it is adjusted to acid pH, choosing high using extraction efficiency
The good solid-phase extraction column of selecting property is extracted, the different elution of reasonable employment and eluting solvent, to different eluents respectively into
The extract liquor filtered after dehydration and drying agent is added in Taste and odor compounds eluent by row processing, after suck dry moisture, is put into rotary evaporation
Device is concentrated；It is 1mL or less 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, it is directly placed into rotary evaporator progress
Concentration；It is 0.5mL hereinafter, being transferred in Agilent special-purpose bottle that liquid after concentration, which is purged with nitrogen to volume,；With efficient liquid
Phase chromatography is detected, that is, completes detection.
The present invention provides rapidly and efficiently while extracting and enriching water environment contained in Taste and odor compounds and Microcystin
Method.The present invention reduces the dosages of organic solvent, and the emulsification that similar liquid-liquid extraction will not be generated in treatment process is existing
As the time used is short, and high-efficient, preci-sion and accuracy is high, has filled up extracting and enriching and quantitatively odor object simultaneously in water environment
The blank of matter and algae toxin.
The present invention reduces the dosages of organic solvent, and the emulsification that similar liquid-liquid extraction will not be generated in treatment process is existing
As the time used is short, and high-efficient, preci-sion and accuracy is high, has filled up extracting and enriching and quantitatively odor object simultaneously in water environment
The blank of matter and algae toxin.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: present embodiment typical four kinds of Taste and odor compounds and three kinds in extracting and enriching gauge water simultaneously
The method of algae toxin follows the steps below:
One, acidity will be adjusted to after the processing of target water sample suction filtration；
Two, solid-phase extraction column is activated and is cleaned:
Using C18 solid-phase extraction column, sampling volume 0.1L-5L, 500mg stationary phase, C18 solid-phase extraction column is successively used
5mL methylene chloride, 5mL methanol and 5mL high purity water, with the flow velocity activation of 1mL/min-5mL/min and rinse C18 solid-phase extraction column
In C18 filler；
Three, will be passed through with the speed of 1ml/min-10ml/min by step 2 by the target water sample of step 1 processing
The C18 solid-phase extraction column of reason, then vacuum drain the moisture in C18 solid-phase extraction column；
Four, it elutes and elutes Taste and odor compounds:
It uses 5ml methylene chloride to elute with 1ml/min-6ml/min elution flow rate to C18 solid-phase extraction column, collects odor
Substance eluent, is added dehydration and drying agent, and the extract liquor after suck dry moisture is put into rotary evaporator and is concentrated, after concentration
Liquid to be purged with nitrogen to volume be 1mL hereinafter, being transferred in Agilent special-purpose bottle, carried out with gas chromatography-mass spectrometry
Detect Taste and odor compounds；
Five, it elutes and elutes algae toxin:
The first C18 solid-phase extraction column with the methanol solution elution of 5ml volume fraction 20% by step 4 processing, then use
The methanol solution of 5ml volume fraction 80% elutes solid-phase extraction column, and elution flow rate 1ml/min-6ml/min is obtained
Microcystin eluent rotary evaporator is concentrated, the liquid after concentration is blown with nitrogen by Microcystin eluent
Being swept to volume is 0.5mL hereinafter, being transferred in Agilent special-purpose bottle, carries out detection algae toxin with high performance liquid chromatography, that is, completes
Typical four kinds of Taste and odor compounds and three kinds of algae toxins in extracting and enriching gauge water simultaneously.
Specific embodiment 2: the present embodiment is different from the first embodiment in that by target water described in step 1
It is 4-5 that pH value is adjusted to after the processing of sample suction filtration.It is other same as the specific embodiment one.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two described in step 2
It is 1L that sample introduction, which optimizes volume,.It is other identical as one of specific embodiment one or two.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three in step 2 with
The flow velocity activation of 2mL/min-4mL/min and rinse C18 solid-phase extraction column.Other phases one of with specific embodiment one to three
Together.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four in step 2 with
The flow velocity activation of 3mL/min and rinse C18 solid-phase extraction column.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: will be through in step 3 unlike one of present embodiment and specific embodiment one to five
The target water sample for crossing step 1 processing passes through the C18 Solid Phase Extraction by step 2 processing with the speed of 3ml/min-8ml/min
Column.It is other identical as one of specific embodiment one to five.
Specific embodiment 7: dichloro in step 4 unlike one of present embodiment and specific embodiment one to six
Methane is eluted with 1ml/min.It is other identical as one of specific embodiment one to six.
Specific embodiment 8: being used in step 4 unlike one of present embodiment and specific embodiment one to seven
Agilent GC7890N-MSD 6973N detection, separates sample using HP-5MS chromatographic column, with gradient increased temperature program
It heats up to HP-5MS chromatographic column, initial temperature is 50 DEG C of holding 3min, with 5 DEG C/min-The heating rate of heating rises to 150
DEG C 2min is kept, carries out purification chromatographic column at 300 DEG C, injector temperature is 250 DEG C, with not shunt mode sample introduction, interface temperature
280 DEG C, mass spectrum uses EI mode, and ionizing energy 70eV, carries out qualitative point to sample using full scan mode by 230 DEG C of temperature
Analysis, m/z range are 50-500.It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: being eluted in step 5 unlike one of present embodiment and specific embodiment one to eight
Flow velocity is 1ml/min.It is other identical as one of specific embodiment one to eight.
Specific embodiment 10: step 5 uses liquid unlike one of present embodiment and specific embodiment one to nine
Chromatography Agilent 1260LC；Zorbax Eclipse XDB-C18 chromatographic column, mobile phase are 0.05% trifluoroacetic acid
Aqueous solution and acetonitrile form, flow velocity 1.0mL/min according to the volume ratio of 67:33, detect 30 DEG C of temperature, sample volume 50uL, inspection
Survey wavelength 238nm.It is other identical as one of specific embodiment one to nine.
Using following experimental verifications effect of the present invention:
Experiment one:
The method of typical four kinds of Taste and odor compounds and three kinds of algae toxins is according to the following steps in extracting and enriching gauge water simultaneously
It carries out:
It one, is 4 by pH value is adjusted after the processing of target water sample suction filtration；
Two, solid-phase extraction column is activated and is cleaned:
Using C18 solid-phase extraction column, 5mL bis- is added into C18 solid-phase extraction column for sampling volume 1L, 500mg stationary phase
Chloromethanes, 5mL methanol and 5mL high purity water, with the C18 filler in the flow velocity activation of 2mL/min and rinse C18 solid-phase extraction column；
Three, the target water sample by step 1 processing is consolidated with the speed of 5ml/min by the C18 by step 2 processing
Phase extraction column, then vacuum drain the moisture in C18 solid-phase extraction column；
Four, it elutes and elutes Taste and odor compounds:
It uses 5ml methylene chloride to elute with 1ml/min elution flow rate to C18 solid-phase extraction column, collects Taste and odor compounds elution
Liquid, is added dehydration and drying agent, and the extract liquor after suck dry moisture is put into rotary evaporator and is concentrated, the liquid after concentration is used
It is 1mL hereinafter, being transferred in Agilent special-purpose bottle that nitrogen, which is purged to volume, 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；It heats up with gradient increased temperature program to chromatographic column, 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 use EI mode, ionizing energy 70eV, 230 DEG C of temperature；Sample is determined using full scan mode
Property analysis (m/z range be 50-500).
Five, it elutes and elutes algae toxin:
The first C18 solid-phase extraction column with the methanol solution elution of 5ml volume fraction 20% by step 4 processing, then use
The methanol solution of 5ml volume fraction 80% elutes solid-phase extraction column, and elution flow rate 1ml/min obtains microcystin
Microcystin eluent rotary evaporator is concentrated plain eluent, and the liquid after concentration is purged with nitrogen to volume
For 0.5mL hereinafter, being transferred in Agilent special-purpose bottle, detected with high performance liquid chromatography；
Using liquid chromatograph Agilent 1260LC；Zorbax Eclipse XDB-C18 (4.6 × 150mm, 5um) color
Compose column；238nm Detection wavelength；Mobile phase is that mass concentration is the body of 0.05% trifluoroacetic acid aqueous solution and acetonitrile according to 67:33
Product is than composition；Flow velocity is 1.0mL/min；30 DEG C of temperature of detection；Sample volume 50uL.
Experiment two:
The method of typical four kinds of Taste and odor compounds and three kinds of algae toxins is according to the following steps in extracting and enriching gauge water simultaneously
It carries out:
It one, is 4 by pH value is adjusted after the processing of target water sample suction filtration；
Two, solid-phase extraction column is activated and is cleaned:
Using C18 solid-phase extraction column, sampling volume 0.1L-5L, 500mg stationary phase, C18 solid-phase extraction column is successively used
5mL methylene chloride, 5mL methanol and 5mL high purity water, with the flow velocity activation of 1mL/min-5mL/min and rinse C18 solid-phase extraction column
In C18 filler；
Three, the target water sample by step 1 processing is consolidated with the speed of 2ml/min by the C18 by step 2 processing
Phase extraction column, then vacuum drain the moisture in C18 solid-phase extraction column；
Four, it elutes and elutes Taste and odor compounds:
It uses 5ml methylene chloride to elute with 5ml/min elution flow rate to C18 solid-phase extraction column, collects Taste and odor compounds elution
Liquid, is added dehydration and drying agent, and the extract liquor after suck dry moisture is put into rotary evaporator and is concentrated, the liquid after concentration is used
It is 1mL hereinafter, being transferred in Agilent special-purpose bottle that nitrogen, which is purged to volume, 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；It heats up with gradient increased temperature program to chromatographic column, 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 use EI mode, ionizing energy 70eV, 230 DEG C of temperature；Sample is determined using full scan mode
Property analysis (m/z range be 50-500).
Five, it elutes and elutes algae toxin:
The first C18 solid-phase extraction column with the methanol solution elution of 5ml volume fraction 20% by step 4 processing, then use
The methanol solution of 5ml volume fraction 80% elutes solid-phase extraction column, and elution flow rate 2ml/min obtains microcystin
Microcystin eluent rotary evaporator is concentrated plain eluent, and the liquid after concentration is purged with nitrogen to volume
For 0.5mL hereinafter, being transferred in Agilent special-purpose bottle, detected with high performance liquid chromatography；
Using liquid chromatograph Agilent 1260LC；Zorbax Eclipse XDB-C18 (4.6 × 150mm, 5um) color
Compose column；238nm Detection wavelength；Mobile phase is that mass concentration is the body of 0.05% trifluoroacetic acid aqueous solution and acetonitrile according to 67:33
Product is than composition；Flow velocity is 1.0mL/min；30 DEG C of temperature of detection；Sample volume 50uL.
Experiment three:
The method of typical four kinds of Taste and odor compounds and three kinds of algae toxins is according to the following steps in extracting and enriching gauge water simultaneously
It carries out:
It one, is 4 by pH value is adjusted after the processing of target water sample suction filtration；
Two, solid-phase extraction column is activated and is cleaned:
Using C18 solid-phase extraction column, sampling volume 0.1L-5L, 500mg stationary phase, C18 solid-phase extraction column is successively used
5mL methylene chloride, 5mL methanol and 5mL high purity water, with the flow velocity activation of 1mL/min-5mL/min and rinse C18 solid-phase extraction column
In C18 filler；
Three, the target water sample by step 1 processing is consolidated with the speed of 8ml/min by the C18 by step 2 processing
Phase extraction column, then vacuum drain the moisture in C18 solid-phase extraction column；
Four, it elutes and elutes Taste and odor compounds:
It uses 5ml methylene chloride to elute with 4ml/min elution flow rate to C18 solid-phase extraction column, collects Taste and odor compounds elution
Liquid, is added dehydration and drying agent, and the extract liquor after suck dry moisture is put into rotary evaporator and is concentrated, the liquid after concentration is used
It is 1mL hereinafter, being transferred in Agilent special-purpose bottle that nitrogen, which is purged to volume, 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；It heats up with gradient increased temperature program to chromatographic column, 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 use EI mode, ionizing energy 70eV, 230 DEG C of temperature；Sample is determined using full scan mode
Property analysis (m/z range be 50-500).
Five, it elutes and elutes algae toxin:
The first C18 solid-phase extraction column with the methanol solution elution of 5ml volume fraction 20% by step 4 processing, then use
The methanol solution of 5ml volume fraction 80% elutes solid-phase extraction column, and elution flow rate 6ml/min obtains microcystin
Microcystin eluent rotary evaporator is concentrated plain eluent, and the liquid after concentration is purged with nitrogen to volume
For 0.5mL hereinafter, being transferred in Agilent special-purpose bottle, detected with high performance liquid chromatography；
Using liquid chromatograph Agilent 1260LC；Zorbax Eclipse XDB-C18 (4.6 × 150mm, 5um) color
Compose column；238nm Detection wavelength；Mobile phase is that mass concentration is the body of 0.05% trifluoroacetic acid aqueous solution and acetonitrile according to 67:33
Product is than composition；Flow velocity is 1.0mL/min；30 DEG C of temperature of detection；Sample volume 50uL.
Experiment one to three pairs of Taste and odor compounds of experiment and algae toxin carry out extracting and enriching simultaneously, the gas phase after optimizing respectively
Chromatographic mass spectrometry and efficient liquid phase chromatographic analysis condition establish the working curve of object, while having carried out recovery of standard addition and essence
Density experiment, result are as shown in the table.
Table 1
Claims (9)
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 follows the steps below in extracting and enriching gauge water:
It one, is 4-5 by pH value is adjusted to after the processing of target water sample suction filtration；
Two, solid-phase extraction column is activated and is cleaned:
Using C18 solid-phase extraction column, sampling volume 0.1L-5L, 500mg stationary phase, C18 solid-phase extraction column successively uses 5mL bis-
Chloromethanes, 5mL methanol and 5mL high purity water, in the flow velocity activation of 1mL/min-5mL/min and rinse C18 solid-phase extraction column
C18 filler；
Three, the target water sample by step 1 processing is passed through with the speed of 1ml/min-10ml/min by step 2 processing
C18 solid-phase extraction column, then vacuum drain the moisture in C18 solid-phase extraction column；
Four, it elutes and elutes Taste and odor compounds:
It uses 5ml methylene chloride to elute with 1ml/min-6ml/min elution flow rate to C18 solid-phase extraction column, collects Taste and odor compounds
Eluent, is added dehydration and drying agent, and the extract liquor after suck dry moisture is put into rotary evaporator and is concentrated, by the liquid after concentration
It is 1mL hereinafter, being transferred in Agilent special-purpose bottle that body, which is purged with nitrogen to volume, is detected with gas chromatography-mass spectrometry
Taste and odor compounds；
Five, it elutes and elutes algae toxin:
The first C18 solid-phase extraction column with the elution of the methanol solution of 5ml volume fraction 20% by step 4 processing, then with 5ml body
The methanol solution of fraction 80% elutes solid-phase extraction column, and elution flow rate 1ml/min-6ml/min obtains Microcystis aeruginosa
Microcystin eluent rotary evaporator is concentrated toxin eluent liquid, and the liquid after concentration is purged with nitrogen to body
Product is 0.5mL hereinafter, being transferred in Agilent special-purpose bottle, carries out detection algae toxin with high performance liquid chromatography, that is, completes while extracting
Take typical four kinds of Taste and odor compounds and three kinds of algae toxins in enrichment gauge water；Wherein four kinds of Taste and odor compounds be ground depth,
2- methyl isoborneol, β-cyclocitral and alpha, beta-lonone；Three kinds of algae toxins are microcapsule phycotoxin MC-LR, Microcystin MC-
YR and Microcystin MC-RR.
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 1L that sample introduction described in step 2, which optimizes volume,.
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 with the flow velocity activation of 2mL/min-4mL/min and rinse C18 solid-phase extraction column in step 2.
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 with the flow velocity activation of 3mL/min and rinse C18 solid-phase extraction column 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 in step 3 will by step 1 processing target water sample with the speed of 3ml/min-8ml/min pass through through
Cross the C18 solid-phase extraction column of step 2 processing.
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 methylene chloride is eluted in step 4 with 1ml/min.
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 the detection of Taste and odor compounds in step 4: it is detected using Agilent GC7890N-MSD 6973N, using HP-
5MS chromatographic column separates sample, heats up with gradient increased temperature program to HP-5MS chromatographic column, and initial temperature is 50 DEG C
3min is kept, with 5 DEG C/min-The heating rate of heating rises to 150 DEG C of holding 2min, carries out purification chromatographic column, sample introduction at 300 DEG C
Mouth temperature is 250 DEG C, and with not shunt mode sample introduction, 280 DEG C of interface temperature, mass spectrum uses EI mode, ionizing energy 70eV, temperature
230 DEG C of degree carries out qualitative analysis to sample using full scan mode, and m/z range is 50-500.
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 elution flow rate is 1ml/min in step 5.
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 the detection of step 5 algae toxin: liquid chromatograph Agilent 1260LC is used；Zorbax Eclipse
XDB-C18 chromatographic column, mobile phase are 0.05% trifluoroacetic acid aqueous solution and acetonitrile, are formed according to the volume ratio of 67:33-, flow velocity
For 1.0mL/min, 30 DEG C of temperature are detected, sample volume 50uL, Detection wavelength 238nm.
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| CN102507801A (en) * | 2011-12-16 | 2012-06-20 | 同济大学 | Rapid analysis method of IPMP (2-isopropyl-3-methoxypyrazine) and IBMP (2-isobutyl-3-methoxypyrazine) odor compounds in water |
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