CN110146618A - A kind of method that rapidly extracting analyzes 10 kinds of polycyclic aromatic hydrocarbons in water - Google Patents
A kind of method that rapidly extracting analyzes 10 kinds of polycyclic aromatic hydrocarbons in water Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000002203 pretreatment Methods 0.000 claims abstract description 7
- 238000004458 analytical method Methods 0.000 claims abstract description 6
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 36
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthene Chemical compound C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 claims description 33
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 claims description 22
- 239000013558 reference substance Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 12
- CWRYPZZKDGJXCA-UHFFFAOYSA-N acenaphthene Chemical compound C1=CC(CC2)=C3C2=CC=CC3=C1 CWRYPZZKDGJXCA-UHFFFAOYSA-N 0.000 claims description 12
- HXGDTGSAIMULJN-UHFFFAOYSA-N acetnaphthylene Natural products C1=CC(C=C2)=C3C2=CC=CC3=C1 HXGDTGSAIMULJN-UHFFFAOYSA-N 0.000 claims description 12
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims description 12
- 238000010183 spectrum analysis Methods 0.000 claims description 8
- 125000004054 acenaphthylenyl group Chemical group C1(=CC2=CC=CC3=CC=CC1=C23)* 0.000 claims description 6
- 125000003983 fluorenyl group Chemical class C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000011550 stock solution Substances 0.000 claims description 6
- 239000003205 fragrance Substances 0.000 claims description 5
- 238000003556 assay Methods 0.000 claims description 4
- 125000005605 benzo group Chemical group 0.000 claims description 4
- 230000009514 concussion Effects 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000004704 ultra performance liquid chromatography Methods 0.000 claims description 4
- 238000003795 desorption Methods 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 238000000611 regression analysis Methods 0.000 claims description 3
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 3
- 238000003859 hyphenated technique Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- FMMWHPNWAFZXNH-UHFFFAOYSA-N ERM-AC051 Natural products C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000000944 Soxhlet extraction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 238000000899 pressurised-fluid extraction Methods 0.000 description 2
- 238000002470 solid-phase micro-extraction Methods 0.000 description 2
- TXVHTIQJNYSSKO-UHFFFAOYSA-N BeP Natural products C1=CC=C2C3=CC=CC=C3C3=CC=CC4=CC=C1C2=C34 TXVHTIQJNYSSKO-UHFFFAOYSA-N 0.000 description 1
- FTOVXSOBNPWTSH-UHFFFAOYSA-N benzo[b]fluoranthene Chemical compound C12=CC=CC=C1C1=CC3=CC=CC=C3C3=C1C2=CC=C3 FTOVXSOBNPWTSH-UHFFFAOYSA-N 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- VLCQZHSMCYCDJL-UHFFFAOYSA-N tribenuron methyl Chemical compound COC(=O)C1=CC=CC=C1S(=O)(=O)NC(=O)N(C)C1=NC(C)=NC(OC)=N1 VLCQZHSMCYCDJL-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Classifications
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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
-
- 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
-
- 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
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1826—Organic contamination in water
-
- 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
- G01N2030/8854—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 involving hydrocarbons
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention relates to parallel solid phase film chip sample pre-treatment microwell plate system and devices involved in method this method of 10 kinds of polycyclic aromatic hydrocarbons in a kind of rapidly extracting analysis water to be made of rocking equipment, 96 orifice plates and film Tab system, using ultra performance liquid chromatography-triple quadrupole bar mass spectrometric hyphenated technique, polycyclic aromatic hydrocarbon content is quantitative determined to environmental pollutants, detection, average each time for sample pretreatment 1 minute or so are completed in 10 minutes.This method favorable reproducibility, stability is good, is the fast and effective means of polycyclic aromatic hydrocarbon content in extraction and determination water.
Description
Technical field
The present invention relates to the methods of 10 kinds of polycyclic aromatic hydrocarbons in a kind of rapidly extracting analysis water, utilize parallel solid phase film sheet-like
Product pre-treatment microwell plate system rapidly extracting sample and a kind of ultra performance liquid chromatography-mass spectrometric hyphenated technique quickly analyze survey
Determine the method for polycyclic aromatic hydrocarbon content in water.
Background technique
Environmental contaminants polycyclic aromatic hydrocarbon PAHs is the compound containing 2 and 2 or more phenyl ring, and polarity is weaker, is soluble in
Nonpolar and moderately polar solvent.The extracting method of PAHs mainly have soxhlet extraction, ultrasonic extraction, microwave loss mechanisms,
Accelerated solvent extraction follows the example of, Solid-phase Microextraction etc..Soxhlet extraction is cumbersome, takes a long time, and solvent-oil ratio is bigger；It is micro-
Wave extraction method is less desirable to the extraction efficiency of low cycle compound；Accelerated solvent extraction is followed the example of to be needed to configure with Solid-phase Microextraction
Instrument, maintenance and higher operating costs；No matter which kind of extracting method is used, requires a large amount of sample, and process is many and diverse.
The Extraction solvent of PAHs be mainly methylene chloride, n-hexane, acetone different proportion mixed solvent.In liquid phase color
Need to be converted to methylene chloride, n-hexane, acetone equal solvent acetonitrile, methanol equal solvent before spectrum analysis, and solvent switch process
Be related to revolving, nitrogen is blown, and easily causes determinand loss, solvent switch is not easy sufficiently.
" liquid chromatogram-atmospheric pressure photoelectric ionization source mass spectrography measures in electronic and electrical equipment more than 16 kinds pertinent literature simultaneously
Cycloaromatics residual " Yin Juyi, Xie Donghua, Chen Jianguo etc., although and detecting polycyclic aromatic hydrocarbon, this opposite hair with LC-MS
Bright extracting method is cumbersome, takes a long time, and sample is not also identical, and present invention is generally directed to 10 kinds of polycyclic aromatic hydrocarbons in water sample
Detection method.
In contrast, the parallel solid phase film chip sample pre-treatment microwell plate system provided by the invention based on LC/MS/MS
Extracting method is easy to operate, cost is relatively low, and sample size is few, and batch samples is suitble to handle simultaneously.There is the testing time simultaneously
It is short, favorable reproducibility the advantages that.
Summary of the invention
Object of the present invention is to provide the method for 10 kinds of polycyclic aromatic hydrocarbons in a kind of rapidly extracting analysis water, involved in this method
Parallel solid phase film chip sample pre-treatment microwell plate system and device be by rocking equipment (1), 96 orifice plates (2) and film Tab system
(3) it forms, using ultra performance liquid chromatography-triple quadrupole bar mass spectrometric hyphenated technique, polycyclic aromatic hydrocarbon content is carried out to environmental pollutants
Detection, average each time for sample pretreatment 1 minute or so are completed in quantitative determination in 10 minutes.This method favorable reproducibility is stablized
Property is good, is the fast and effective means of polycyclic aromatic hydrocarbon content in extraction and determination water.
The method of 10 kinds of polycyclic aromatic hydrocarbons in a kind of rapidly extracting analysis water of the present invention, it is parallel involved in this method
Immobilon-p chip sample pre-treatment microwell plate system and device is by rocking equipment (1), 96 orifice plates (2) and film Tab system (3) group
At concrete operations follow these steps to carry out:
A, sample treatment: water sample being added in 96 orifice plates (2), 96 orifice plates (2) are placed in film Tab system (3),
It is shaken by rocking equipment (1), while being adsorbed 50 minutes by film Tab system (3), changed in new 96 orifice plates (2) each hole and be added
The acetonitrile of volume ratio 80:20: water concussion desorption 50 minutes, 96 orifice plates (2) are put into autosampler sample introduction to surpassing after the completion
High Performance Liquid Chromatography/Mass Spectrometry analysis is to be measured；
B, ultra performance liquid chromatography condition: chromatographic column: Hypersil GOLD, C18 100 × 2.1mm, 1.9 μm；Flowing
Phase: A- water, B- acetonitrile；Gradient: 0-2 minutes, A 60%；2-3 minutes, A 60%-20%；3.0-8.0 minute, A
20%；8.0-8.1 minutes, A 20%-60%；8.1-10.0 minutes, A60%, flow velocity: 0.35mL/min；Column temperature: 30 DEG C；Into
Sample amount: 5 μ L；
C, Mass Spectrometry Conditions: ion ource electric current :+4.0v；Ion source temperature: 400 DEG C；Sheath gas: 35arb；Assist gas: 5arb；
Ion transfer capillary temperature: 350 DEG C；Type ion source: atmospheric pressure chemical APCI ion source；
D, the preparation of reference substance solution: precision pipettes 100 μ L reference substances, 1mL is settled to acetonitrile dissolution, as reference substance
Solution stock solution；
E, Specification Curve of Increasing: precision pipettes reference substance solution stock solution, and with the water of diluent volume ratio 20:80: second
It is 2ng/mL, 4ng/mL, 20ng/mL, 40ng/mL, 200ng/mL, 400ng/mL that nitrile solution is diluted to concentration respectively, is marked
Quasi- solution；Ultra performance liquid chromatography-mass spectral analysis is carried out by chromatographic condition；Regression analysis is carried out to peak area with concentration, obtains it
Component Standard curve calculates regression equation；
F, assay: accurate pipette samples prepare liquid carries out ultra performance liquid chromatography-mass spectral analysis by chromatographic condition,
And bring peak area into standard curve, calculate content, testing result: naphthalene 6.0-207ng；Acenaphthene 2.4-30,7ng；Acenaphthylene 1.7-
48.0ng；Fluorenes 5.6-60.5ng；Luxuriant and rich with fragrance 11.1-64.2ng；Anthracene 1.06-66.8ng；Fluoranthene 5.9-52.5ng；Pyrene 3.7-70.4ng；
BaP b fluoranthene 1.7-16ng；Benzo a pyrene 18--118ng.
Detailed description of the invention
Fig. 1 is the spectrogram of standard specimen of the present invention, and wherein total ion current figure spectral peak is successively are as follows: naphthalene (4.15min)；Acenaphthylene
(4.30min)；Fluorenes (4.53min)；Acenaphthene (4.54min)；Luxuriant and rich with fragrance (4.63min)；Anthracene (4.72min)；Fluoranthene (4.94min)；Pyrene
(5.09min)；Benzo (b) fluoranthene (6.00min)；Benzo (a) pyrene (6.22min)；
Fig. 2 is parallel solid phase film chip sample pre-treatment microwell plate system and device schematic diagram of the present invention.
Specific embodiment
Embodiment
For present invention laboratory water sample, sample is extracted by preparation method provided by the invention after sample preparation, according to
Measuring method provided by the invention carries out the assay of polycyclic aromatic hydrocarbon:
Instrument and reagent:
Ultra Performance Liquid Chromatography instrument (Agilent 1290)；Mass spectrograph (Thermo TSQ QUANTUM ULTRA)；Very much
One of electronic balance (METTLER AM100)；Acetonitrile is chromatography pure reagent, polycyclic aromatic hydrocarbon reference substance (BePure)；
Instrument condition:
Ultra Performance Liquid Chromatography instrument condition:
Chromatographic column: Hypersil GOLD, C18 100 × 2.1mm, 1.9 μm；Mobile phase: A- ultrapure water, B- acetonitrile；Elution
Gradient:
Flow velocity: 0.35mL/min；Column temperature: 30 DEG C；Sample volume: 5 μ L；
Mass spectrograph condition: ion ource electric current :+4.0v；Ion source temperature: 400 DEG C；Sheath gas: 35arb；Assist gas: 5arb；
Ion transfer capillary temperature: 350 DEG C；Type ion source: atmospheric pressure chemical APCI ion source；
Sample treatment: precision draws 2mL water sample, is placed in 96 orifice plate, 2 hole, 96 orifice plates 2 are placed on film Tab system 3
In, it is shaken by rocking equipment 1, while being adsorbed 50 minutes by film Tab system 3, changes in the new each hole of 96 orifice plate 2 and 1mL is added
The acetonitrile of volume ratio 80:20: 96 orifice plates 2 are put into sample introduction in autosampler after the completion by water elution, concussion desorption 50 minutes
To ultra performance liquid chromatography-mass spectral analysis；
The preparation of reference substance solution: the preparation of reference substance solution: precision pipettes 100 μ L reference substances, dissolves constant volume with acetonitrile
To 1mL, as reference substance solution stock solution；
Specification Curve of Increasing: precision pipettes reference substance solution stock solution, and with the water of diluent volume ratio 20:80: acetonitrile
It is 2ng/mL, 4ng/mL, 20ng/mL, 40ng/mL, 200ng/mL, 400ng/mL that solution is diluted to concentration respectively, obtains standard
Solution；Ultra performance liquid chromatography-mass spectral analysis is carried out by chromatographic condition；Regression analysis is carried out to peak area with concentration, obtains its group
Minute mark directrix curve calculates regression equation；Naphthalene Y=2178.29+67.6777*X, R2=0.9975, n=6；Acenaphthene Y=4028.56+
100.466*X, R2=0.9993, n=6；Acenaphthylene Y=6233.36+616.158*X, R2=0.9989, n=7；Fluorenes Y=
3119.73+163.784*X R2=0.9993, n=6；Luxuriant and rich with fragrance Y=6227.49+286.401*X, R2=0.9982, n=8；Anthracene Y=
6399.69+593.228*X R2=0.9988, n=7；Fluoranthene Y=13232.8+501.493*X, R2=0.9987, n=7；Pyrene Y
=10948.7+861.248*X, R2=0.9991, n=7；BaP b fluoranthene Y=151.247+2556.68*X, R2=
0.9992, n=6；Benzo a pyrene Y=-23181+2382.35*X, R2=0.9987, n=6；
Assay: accurate pipette samples prepare liquid carries out ultra performance liquid chromatography-mass spectral analysis by chromatographic condition, and
It brings peak area into standard curve, calculates content；
Sample detection is as a result, naphthalene 6.0-207ng；Acenaphthene 2.4-30,7ng；Acenaphthylene 1.7-48.0ng；Fluorenes 5.6-60.5ng；It is luxuriant and rich with fragrance
11.1-64.2ng；Anthracene 1.06-66.8ng；Fluoranthene 5.9-52.5ng；Pyrene 3.7-70.4ng；BaP b fluoranthene 1.7-16ng；Benzene
And a pyrene 18--118ng；
Repetitive test: totally 7 parts of sample are taken, by the step, RSD result are as follows: naphthalene 4.19%；Acenaphthene 4.01%；Acenaphthylene
3.98%；Fluorenes 1.55%；Phenanthrene 6.19%；Anthracene 4.6%；Fluoranthene 4.82%；Pyrene 5.33%；BaP b fluoranthene 2.82%；Benzo a
Pyrene 1.87%.
Claims (1)
1. a kind of method of 10 kinds of polycyclic aromatic hydrocarbons in rapidly extracting analysis water, it is characterised in that parallel solid phase involved in this method
Film chip sample pre-treatment microwell plate system and device is made of rocking equipment (1), 96 orifice plates (2) and film Tab system (3), tool
Gymnastics follows these steps to carry out:
A, sample treatment: water sample is added in 96 orifice plates (2), 96 orifice plates (2) are placed in film Tab system (3), by shaking
Device (1) concussion is swung, while being adsorbed 50 minutes by film Tab system (3), changes in new 96 orifice plates (2) each hole and volume is added
Acetonitrile than 80:20: water concussion desorption 50 minutes, 96 orifice plates (2) are put into autosampler sample introduction to ultra high efficiency after the completion
LC-MS analysis is to be measured；
B, ultra performance liquid chromatography condition: chromatographic column: Hypersil GOLD, C18 100 × 2.1mm, 1.9 μm；Mobile phase:
A- water, B- acetonitrile；Gradient: 0-2 minutes, A 60%；2-3 minutes, A 60%-20%；3.0-8.0 minutes, A 20%；8.0-
8.1 minutes, A 20%-60%；8.1-10.0 minutes, A60%, flow velocity: 0.35mL/min；Column temperature: 30 DEG C；Sample volume: 5 μ L；
C, Mass Spectrometry Conditions: ion ource electric current :+4.0v；Ion source temperature: 400 DEG C；Sheath gas: 35arb；Assist gas: 5arb；Ion
Transfer capillary temperature: 350 DEG C；Type ion source: atmospheric pressure chemical APCI ion source；
D, the preparation of reference substance solution: precision pipettes 100 μ L reference substances, 1mL is settled to acetonitrile dissolution, as reference substance solution
Stock solution；
E, Specification Curve of Increasing: precision pipettes reference substance solution stock solution, and with the water of diluent volume ratio 20:80: acetonitrile is molten
It is 2ng/mL, 4ng/mL, 20ng/mL, 40ng/mL, 200ng/mL, 400ng/mL that liquid is diluted to concentration respectively, and it is molten to obtain standard
Liquid；Ultra performance liquid chromatography-mass spectral analysis is carried out by chromatographic condition；Regression analysis is carried out to peak area with concentration, obtains its component
Standard curve calculates regression equation；
F, assay: accurate pipette samples prepare liquid carries out ultra performance liquid chromatography-mass spectral analysis by chromatographic condition, and will
Peak area brings standard curve into, calculates content, testing result: naphthalene 6.0-207ng；Acenaphthene 2.4-30,7ng；Acenaphthylene 1.7-48.0ng；
Fluorenes 5.6-60.5ng；Luxuriant and rich with fragrance 11.1-64.2ng；Anthracene 1.06-66.8ng；Fluoranthene 5.9-52.5ng；Pyrene 3.7-70.4ng；BaP b
Fluoranthene 1.7-16ng；Benzo a pyrene 18--118ng.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910492469.4A CN110146618A (en) | 2019-06-06 | 2019-06-06 | A kind of method that rapidly extracting analyzes 10 kinds of polycyclic aromatic hydrocarbons in water |
| PCT/CN2020/084609 WO2020244311A1 (en) | 2019-06-06 | 2020-04-14 | Method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water |
| LU102485A LU102485B1 (en) | 2019-06-06 | 2020-04-14 | Method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910492469.4A CN110146618A (en) | 2019-06-06 | 2019-06-06 | A kind of method that rapidly extracting analyzes 10 kinds of polycyclic aromatic hydrocarbons in water |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110146618A true CN110146618A (en) | 2019-08-20 |
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|---|---|---|---|
| CN201910492469.4A Pending CN110146618A (en) | 2019-06-06 | 2019-06-06 | A kind of method that rapidly extracting analyzes 10 kinds of polycyclic aromatic hydrocarbons in water |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN110146618A (en) |
| LU (1) | LU102485B1 (en) |
| WO (1) | WO2020244311A1 (en) |
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| CN110579557A (en) * | 2019-09-19 | 2019-12-17 | 北京科技大学 | HPLC analysis detection method for simultaneously detecting 12 monocyclic aromatic hydrocarbons in water |
| WO2020244311A1 (en) * | 2019-06-06 | 2020-12-10 | 中国科学院新疆生态与地理研究所 | Method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water |
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| IT202100002717A1 (en) | 2021-02-08 | 2022-08-08 | Epi C S R L | METHOD FOR THE DETECTION AND MEASUREMENT OF SPECIFIC ANTIGENS |
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| WO2020244311A1 (en) * | 2019-06-06 | 2020-12-10 | 中国科学院新疆生态与地理研究所 | Method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water |
| CN110579557A (en) * | 2019-09-19 | 2019-12-17 | 北京科技大学 | HPLC analysis detection method for simultaneously detecting 12 monocyclic aromatic hydrocarbons in water |
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