CN106501391A - The immobilon-p extraction gas phase chromatographic tandem Mass Spectrometry detection method of organochlorine compound in a kind of water body - Google Patents
The immobilon-p extraction gas phase chromatographic tandem Mass Spectrometry detection method of organochlorine compound in a kind of water body Download PDFInfo
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- CN106501391A CN106501391A CN201610867631.2A CN201610867631A CN106501391A CN 106501391 A CN106501391 A CN 106501391A CN 201610867631 A CN201610867631 A CN 201610867631A CN 106501391 A CN106501391 A CN 106501391A
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Abstract
The invention discloses the immobilon-p of organochlorine compound extracts gas phase chromatographic tandem Mass Spectrometry detection method in a kind of water body, with C18Solid-phase extraction membrane realizes the enrichment of organochlorine compound in water body, detects that the method operating procedure is few, sensitivity is high, favorable reproducibility, the assay that can be used for organochlorine compound in water body using gas chromatogram tandem mass spectrum detection method.
Description
Technical field
The present invention relates to Water quality safety detection technology field, in more particularly to a kind of water body, organochlorine compound consolidates
Phase membrane extraction-gas chromatogram tandem mass spectrum detection method.
Background technology
Gamma Hexaochlorocyclohexane, clofenotane are the organochlorine pesticides of a class difficult degradation, many insects are had tag, stomach toxicity, stifling and
A certain degree of systemic action, about 2～20 years or so the half-life of organochlorine pesticide, can accumulate in vivo and pass through
Food chain is transmitted, and causes serious threat to ecological environment and health.Although many countries are prohibited already and limit use,
Due to Gamma Hexaochlorocyclohexane, clofenotane stable chemical nature, further investigation reveals that in the surrounding medium of domestic each department and have in human body residual
Stay, some are even higher by standard regulation manyfold.Such as Min River water body Gamma Hexaochlorocyclohexane, the contamination characteristics application form open fire body six of clofenotane
66 and clofenotane mass concentration scope respectively 1.031-1.804 and 0.767-1.156ng/L.Organochlorine pesticide in soil
Residual has directly harm to terrestrial life, also can be discharged into influence on water body aquatile by rainwash.Many chlorine connection in environment
Benzene (PCBs) mostlys come from the production of industrial goods.The commodity production of PCBs starts from nineteen twenty-nine.Although the production of PCBs and application
It has been prohibited in worldwide in 20 century 70s early stage, the production in whole world PCBs alreadys exceed 1,300,000 tons.
Start to produce from nineteen sixty-five, end (production of PCBs is prohibited) in 1974, China about produces 10000 tons of PCBs.Additionally,
The 1950's, China also constantly entered to suck the electric equipment of PCBs from other countries, and these also become between the eighties
The potential source of PCBs pollutions in Chinese environmental.In soils and sediments, according to existing PCB data, PCB in China s dense
Degree scope is 0.01～1840 μ g/kg.?《Water environment quality standard》In the total standard Limited Doses of 7 kinds of PCBs be 0.02 μ
G/L, the Limited Doses of clofenotane are 0.2 μ g/L.In scholar's research reservoir area of Three Gorges water body, the residual level of PCBs and its environment are handed over
Change, as a result show that the content range of PCBs in the water body of reservoir area is not detect～48.67ng/L.In eight big estuary water body of the Zhujiang River
The content range of PCBs is 0.19～7.04ng/L.Waste electric products, deposit are in suspension, atmospheric sedimentation and waste water treatment plant
Discharge is the significant contributor of water body PCBs pollutions.
As in environmental water sample, organochlorine compound concentration is extremely low, it usually needs could determine through enrichment.Traditional richness
Catchment middle organochlorine compound method be liquid-liquid extraction method, cumbersome time-consuming, need to consume substantial amounts of organic solvent,
And solid phase extraction because have simple to operate, consume that solvent is few and the high analysis for being widely used in pesticide of enrichment times in.
Searching is a kind of simpler, and in the water body of environmental protection, the pre-treating method of organochlorine compound becomes study hotspot.Solid phase membrane extraction is made
For one kind of Solid-Phase Extraction, the solid-phase extraction membrane used by it, large volume of water sample, and enrichment times can be processed faster
High.In addition, solid phase membrane extraction directly can process water sample at the scene, convenient and swift stable.The instrument detection of organochlorine compound
Technology has gas chromatogram, gas chromatography-mass spectrography etc..Gas chromatogram-electron capture detection is used as selectively highly sensitive
The detecting instrument of degree, has higher sensitivity and accuracy to organochlorine compound detection, but is easily disturbed by impurity, qualitative not
Enough accurate.In recent years, research worker has carried out the research to some Hekou Area organochlorine residues and distribution, but with regard to water body in
The research of trace organochlorine compound residual is few.
Content of the invention
It is an object of the invention to provide in a kind of water body organochlorine compound solid phase membrane extraction-gas chromatogram series connection matter
Spectrum detection method, fast and accurately can determine to trace organochlorine compound in water body, to realize trace organic chloride in water body
The quantitative and qualitative analyses of compound.
The technical solution adopted for the present invention to solve the technical problems is：
The solid phase membrane extraction of organochlorine compound-gas chromatogram tandem mass spectrum detection method in a kind of water body, including as follows
Step：
(1)C18The cleaning and activation of solid-phase extraction membrane：C18Solid-phase extraction membrane is in advance with 5mL normal hexane/dichloromethane mixing
Immersion steeps 3min, then successively with 10mL methanol, 10mL water activation C18Solid-phase extraction membrane, allows solvent all to flow through C18Solid phase extracts
Film is taken, in the process, it is to avoid solid-phase extraction membrane ingress of air；
(2) extraction of water sample：Water sample is filtered with 0.45 μm of glass fiber filter in advance and obtains pretreatment water sample, then will be located in advance
The 1000mL water samples of reason are added to equipped with the C after step (1) activation18In the glass filter of solid-phase extraction membrane, vacuum pump, water sample is opened
After passing through with the flow velocity of 10mL/min, continue evacuation to remove C18Residual moisture in solid-phase extraction membrane；
(3) eluting of organochlorine compound and concentration：Successively with 10mL normal hexane and 10mL dichloromethane eluent steps (2)
C after process18Solid-phase extraction membrane, eluent cross post eliminating water after 40 DEG C of water-bath rotary evaporated to dryness through anhydrous sodium sulfate, plus just
Hexane dissolves and is settled to 1.0mL and obtains liquid to be detected；
(4) gas chromatography tandem mass spectrometry detection：Liquid to be detected is using Agilent 7890B-7000C gas chromatogram series connection matter
Spectrometer detects that Component seperation is realized using DB-5 capillary gas chromatographic columns (30m × 0.25mm × 0.25 μm) in configuration EI sources,
Gas chromatography tandem mass spectrometry testing conditions according to setting are detected that MRM modes are scanned, quantified by external standard method.
Preferably, normal hexane/dichloromethane mixed liquor is normal hexane and dichloromethane according to 1 in step (1):1 body
The mixture of product ratio.
Preferably, gas chromatographic column heating schedule is in step (4)：80 DEG C of holding 2min, 25 DEG C/min are warming up to 150
DEG C, 3 DEG C/min is warming up to 200 DEG C, then is warming up to 280 DEG C of holding 10min with 8 DEG C/min.
Preferably, Mass Spectrometry Conditions are in step (4)：280 DEG C of chromatography-mass spectroscopy interface temperature, 300 DEG C of ion source temperature,
Electron bombardment ionization source (EI) energy 70eV, 150 DEG C of level Four bar temperature, collision gas flow 1.5mL/min are quenched throughput 2.25mL/
Min, solvent delay time 4.5min, MRM modes are scanned.
Preferably, in water body organochlorine compound include α-Gamma Hexaochlorocyclohexane, β-Gamma Hexaochlorocyclohexane, γ-Gamma Hexaochlorocyclohexane, δ-Gamma Hexaochlorocyclohexane,
p,p'-DDE、p,p'-DDD、o,p'-DDT、p,p'-DDT、PCB28、PCB52、PCB155、PCB101、PCB112、PCB118、
PCB153、PCB138、PCB180、PCB198.
The invention has the beneficial effects as follows：The present invention is with C18Solid-phase extraction membrane realizes the enrichment of organochlorine compound in water body,
Detected using gas chromatography tandem mass spectrometry detection method, the method operating procedure is few, sensitivity is high, favorable reproducibility, can be used for water
The assay of organochlorine compound in body.
Description of the drawings
Fig. 1 is the gas chromatogram tandem mass spectrum MRM scanning figures of 18 kinds of organochlorine compound standard solution；1. α-Gamma Hexaochlorocyclohexane,
2. β-Gamma Hexaochlorocyclohexane, 3. γ-Gamma Hexaochlorocyclohexane, 4. δ-Gamma Hexaochlorocyclohexane, 5.PCB28,6.PCB52,7.PCB155,8.PCB101,9.PCB112,
10.p, p'-DDE, 11.PCB118,12.p, p'-DDD, 13.o, p'-DDT, 14.PCB153,15.p, p'-DDT,
16.PCB138,17.PCB180,18.PCB198.
Specific embodiment
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, the raw material for being adopted and equipment etc. are commercially available or commonly used in the art.
Method in following embodiments, if no special instructions, is the conventional method of this area.
Gas chromatogram tandem mass spectrum MRM scannings can realize efficiently separating for 18 kinds of organochlorine compounds, as shown in Figure 1.
Table 2 is the recovery testu of different mark-on amounts in different water bodys (laboratory tap water and Zhoushan sea area sea water)
As a result.The content of organochlorine in table 3 certain reservoir water body.
Embodiment 1：The measure of 18 kinds of organochlorine compounds in laboratory tap water
(1)C18The cleaning and activation of solid-phase extraction membrane：C18Solid-phase extraction membrane uses 5mL normal hexane/dichloromethane (1 in advance：
1) 3min is soaked, successively with 10mL methanol, 10mL water activation C18Solid-phase extraction membrane, allows solvent all to flow through solid-phase extraction membrane,
During this, it is impossible to make solid-phase extraction membrane ingress of air；
(2) extraction of water sample：In advance with 0.45 μm of glass fiber filter filtration experiment room originally water sample, pretreatment
Originally water sample is added to equipped with C 1000mL laboratorys18In the glass filter of solid-phase extraction membrane, vacuum pump is opened, water sample is with 10mL/
After the flow velocity of min passes through, continue evacuation to remove the residual moisture in solid-phase extraction membrane；
(3) eluting of organochlorine compound and concentration：Successively with 10mL normal hexane and 10mL dichloromethane eluent C18Solid phase
Spe membrane, eluent cross post eliminating water after 40 DEG C of water-bath rotary evaporated to dryness through anhydrous sodium sulfate, are settled to normal hexane
1.0mL, to be analyzed；
(4) gas chromatography tandem mass spectrometry detection：Using Agilent 7890B-7000C gas chromatogram tandem mass spectrometer, configure
EI sources, realize Component seperation using DB-5 capillary gas chromatographic columns (30m × 0.25mm × 0.25 μm).Gas chromatographic column heats up
Program is：80 DEG C of holding 2min, 25 DEG C/min are warming up to 150 DEG C, and 3 DEG C/min is warming up to 200 DEG C, then is warming up to 8 DEG C/min
280 DEG C of holding 10min.Gas chromatography tandem mass spectrometry testing conditions according to setting are detected (table 1), and MRM modes are swept
Retouch, quantified by external standard method.
The MRM scanning mass spectrometry parameters of 1 organochlorine compound of table
(5) Specification Curve of Increasing (external standard method)：Take appropriate organochlorine compound standard reserving solution respectively, matched somebody with somebody with normal hexane
Put the organochlorine compound mixing that concentration is 0.02 μ g/L, 0.05 μ g/L, 0.10 μ g/L, 0.50 μ g/L, 1.0 μ g/L, 2.0 μ g/L
Standard solution.Requirement according to above-mentioned (1), (2), (3), (4) step is operated, according to the organochlorine compound concentration for adding
Corresponding relation Criterion curve with product ion peak area.
Using the external standard method, measure 18 kinds of organochlorine class content of material in laboratory tap water and be and do not detect, mark-on reality
The response rate for testing each organochlorine compound of room tap water is 83%-104% (being shown in Table 2), meets analysis method and the response rate is wanted
Ask.
The recovery of standard addition of 2 different substrates water body of table and Precision Experiment result
Embodiment 2：The measure of 18 kinds of organochlorine compounds in Zhoushan sea area sea water
Method measures 18 kinds of organochlorine class content of material in Zhoushan sea area sea water and is and do not detect with embodiment 1, mark-on boat
In the sea water of mountain and sea domain, the response rate of each organochlorine compound is 85%-115% (being shown in Table 2), meets analysis method to the response rate
Require.
The measure of 18 kinds of organochlorine compounds in embodiment 3 certain reservoir water
(1)C18The cleaning and activation of solid-phase extraction membrane：C18Solid-phase extraction membrane uses 5mL normal hexane/dichloromethane (1 in advance：
1) 3min is soaked, successively with 10mL methanol, 10mL water activation C18Solid-phase extraction membrane, allows solvent all to flow through solid-phase extraction membrane,
During this, it is impossible to make solid-phase extraction membrane ingress of air；
(2) extraction of water sample：Certain reservoir water sample, the 1000mL of pretreatment are filtered in advance with 0.45 μm of glass fiber filter
Reservoir water sample is added to equipped with C18In the glass filter of solid-phase extraction membrane, vacuum pump is opened, water sample is passed through with the flow velocity of 10mL/min
Afterwards, continue evacuation to remove the residual moisture in solid-phase extraction membrane；
(3) eluting of organochlorine compound and concentration：Successively with 10mL normal hexane and 10mL dichloromethane eluent C18Solid phase
Spe membrane, eluent cross post eliminating water after 40 DEG C of water-bath rotary evaporated to dryness through anhydrous sodium sulfate, are settled to normal hexane
1.0mL, to be analyzed；
(4) gas chromatography tandem mass spectrometry detection：Using Agilent 7890B-7000C gas chromatogram tandem mass spectrometer, configure
EI sources, realize Component seperation using DB-5 capillary gas chromatographic columns (30m × 0.25mm × 0.25 μm).Gas chromatographic column heats up
Program is：80 DEG C of holding 2min, 25 DEG C/min are warming up to 150 DEG C, and 3 DEG C/min is warming up to 200 DEG C, then is warming up to 8 DEG C/min
280 DEG C of holding 10min.Gas chromatography tandem mass spectrometry testing conditions according to setting are detected (table 1), and MRM modes are swept
Retouch, quantified by external standard method；
(5) Specification Curve of Increasing (external standard method)：Take appropriate organochlorine compound standard reserving solution respectively, matched somebody with somebody with normal hexane
Put the organochlorine compound mixing that concentration is 0.02 μ g/L, 0.05 μ g/L, 0.10 μ g/L, 0.50 μ g/L, 1.0 μ g/L, 2.0 μ g/L
Standard solution.Requirement according to above-mentioned (1), (2), (3), (4) step is operated, according to the organochlorine compound concentration for adding
Corresponding relation Criterion curve with product ion peak area.
Using quantified by external standard method, 18 kinds of organochlorine content of material in certain reservoir water body are measured as shown in table 3.
The content (ng/L) of organochlorine in table 3 certain reservoir water body
Note：ND is represented and is not detected.
Embodiment described above is one kind preferably scheme of the present invention, not the present invention is made any pro forma
Limit, also have other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (5)
1. in a kind of water body organochlorine compound solid phase membrane extraction-gas chromatogram tandem mass spectrum detection method, it is characterised in that
Comprise the steps：
(1)C18The cleaning and activation of solid-phase extraction membrane：C18Solid-phase extraction membrane is in advance with 5mL normal hexane/dichloromethane mixing immersion
Bubble 3min, then successively with 10mL methanol, 10mL water activation C18Solid-phase extraction membrane, allows solvent all to flow through C18Solid-phase extraction membrane,
In the process, it is to avoid solid-phase extraction membrane ingress of air；
(2) extraction of water sample：Water sample is filtered with 0.45 μm of glass fiber filter in advance and obtains pretreatment water sample, then by pretreatment
1000mL water samples are added to equipped with the C after step (1) activation18In the glass filter of solid-phase extraction membrane, open vacuum pump, water sample with
After the flow velocity of 10mL/min passes through, continue evacuation to remove C18Residual moisture in solid-phase extraction membrane；
(3) eluting of organochlorine compound and concentration：Processed with 10mL normal hexane and 10mL dichloromethane eluent steps (2) successively
C afterwards18Solid-phase extraction membrane, eluent cross post eliminating water after 40 DEG C of water-bath rotary evaporated to dryness through anhydrous sodium sulfate, plus normal hexane
Dissolve and be settled to 1.0mL and obtain liquid to be detected；
(4) gas chromatography tandem mass spectrometry detection：Liquid to be detected adopts Agilent 7890B-7000C gas chromatogram tandem mass spectrometer
Detection, configuration EI sources, realizes Component seperation using DB-5 capillary gas chromatographic columns, according to the gas chromatogram-series connection for setting
Mass Spectrometer Method condition detected, quantified by external standard method.
2. in a kind of water body according to claim 1 organochlorine compound solid phase membrane extraction-gas chromatogram tandem mass spectrum
Detection method, it is characterised in that normal hexane/dichloromethane mixed liquor is normal hexane and dichloromethane according to 1 in step (1):1
The mixture of volume ratio.
3. in a kind of water body according to claim 1 and 2 organochlorine compound solid phase membrane extraction-gas chromatogram series connection matter
Spectrum detection method, it is characterised in that gas chromatographic column heating schedule is in step (4)：80 DEG C of holding 2min, 25 DEG C/min heat up
To 150 DEG C, 3 DEG C/min is warming up to 200 DEG C, then is warming up to 280 DEG C of holding 10min with 8 DEG C/min.
4. in a kind of water body according to claim 1 and 2 organochlorine compound solid phase membrane extraction-gas chromatogram series connection matter
Spectrum detection method, it is characterised in that Mass Spectrometry Conditions are in step (4)：280 DEG C of chromatography-mass spectroscopy interface temperature, ion source temperature
300 DEG C, electron bombardment ionization source (EI) energy 70eV, 150 DEG C of level Four bar temperature, collision gas flow 1.5mL/min are quenched throughput
2.25mL/min, solvent delay time 4.5min, MRM modes are scanned.
5. in a kind of water body according to claim 1 and 2 organochlorine compound solid phase membrane extraction-gas chromatogram series connection matter
Spectrum detection method, it is characterised in that organochlorine compound includes α-Gamma Hexaochlorocyclohexane, β-Gamma Hexaochlorocyclohexane, γ-Gamma Hexaochlorocyclohexane, δ-six in water body
Six or six, p, p'-DDE, p, p'-DDD, o, p'-DDT, p, p'-DDT, PCB28, PCB52, PCB155, PCB101, PCB112,
PCB118、PCB153、PCB138、PCB180、PCB198.
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| CN107132305A (en) * | 2017-07-18 | 2017-09-05 | 泉州出入境检验检疫局综合技术服务中心 | The detection method of organochlorine class compound in leather |
| CN107643347A (en) * | 2017-09-14 | 2018-01-30 | 浙江省海洋水产研究所 | The immobilon-p extraction gaschromatographic mass spectrometry detection method of phthalate compound in a kind of water body |
| CN108680687A (en) * | 2018-04-19 | 2018-10-19 | 浙江省海洋水产研究所 | The detection method of Polychlorinated biphenyls in a kind of marine product |
| CN108931588A (en) * | 2018-04-27 | 2018-12-04 | 中国地质大学（武汉） | A kind of method that qualitative, quantitative measures organochlorine in Oilfield Chemicals |
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| CN113376305A (en) * | 2021-07-13 | 2021-09-10 | 浙江省海洋水产研究所 | Solid-phase membrane extraction gas chromatography-mass spectrometry detection method for carbazole and polyhalogen carbazole in water body |
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|---|---|---|---|---|
| CN107132305A (en) * | 2017-07-18 | 2017-09-05 | 泉州出入境检验检疫局综合技术服务中心 | The detection method of organochlorine class compound in leather |
| CN107643347A (en) * | 2017-09-14 | 2018-01-30 | 浙江省海洋水产研究所 | The immobilon-p extraction gaschromatographic mass spectrometry detection method of phthalate compound in a kind of water body |
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| CN108931588A (en) * | 2018-04-27 | 2018-12-04 | 中国地质大学（武汉） | A kind of method that qualitative, quantitative measures organochlorine in Oilfield Chemicals |
| CN110146618A (en) * | 2019-06-06 | 2019-08-20 | 中国科学院新疆生态与地理研究所 | A kind of method that rapidly extracting analyzes 10 kinds of polycyclic aromatic hydrocarbons in water |
| CN113376305A (en) * | 2021-07-13 | 2021-09-10 | 浙江省海洋水产研究所 | Solid-phase membrane extraction gas chromatography-mass spectrometry detection method for carbazole and polyhalogen carbazole in water body |
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