CN106226418A - Polycyclic aromatic hydrocarbon detection method - Google Patents
Polycyclic aromatic hydrocarbon detection method Download PDFInfo
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- CN106226418A CN106226418A CN201610551686.2A CN201610551686A CN106226418A CN 106226418 A CN106226418 A CN 106226418A CN 201610551686 A CN201610551686 A CN 201610551686A CN 106226418 A CN106226418 A CN 106226418A
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
Abstract
The present invention provides a kind of quick, low cost, simple and effective polycyclic aromatic hydrocarbon detection method.This polycyclic aromatic hydrocarbon detection method includes step: 1] extract, 2] acidifying remove impurity, 3] acidification, 4] gaschromatographic mass spectrometry detection.The present invention uses 5～10 times amount and the close weak organic phase solvent of polycyclic aromatic hydrocarbon polarity to extract, and reduces the polar component interference to detection in sample.The sulphuric acid using finite concentration (50%～80%) and a certain amount of (0.5ml～1.0ml) carries out acidification to sample, the pre-treatment making sample is simple, easily operation, low cost, and impurity-eliminating effect is obvious, acidification improves the polycyclic aromatic hydrocarbon ionizing efficiency when Mass Spectrometer Method simultaneously, is effectively improved the sensitivity that 4 kinds of polycyclic aromatic hydrocarbons are detected by mass spectrum.
Description
Technical field
The present invention relates to a kind of polycyclic aromatic hydrocarbon detection method, locate before being specifically related to the sample of 4 kinds of polycyclic aromatic hydrocarbon content detections
Reason method and gas chromatography combined with mass spectrometry technology.
Technical background
Polycyclic aromatic hydrocarbon (Polycyclic Aromatic Hhydrocarbons, PAHs) be a class by two or two with
Upper phenyl ring composition Hydrocarbon, its steady chemical structure, it is difficult to degraded, the polycyclic aromatic hydrocarbon in environment be mainly derived from coal,
The imperfect combustion of the carbonaceous organic material such as oil and timber, owing to it has half volatile, it is possible to migrates with atmosphere pollution, holds
Free settling is at plant surface, and enters in plant extract along with producing, and it is carcinogenic to be that a class has, teratogenesis and cause gene mutation
Persistence organic pollutant.
Having now been found that more than 200 kind of PAHs, have carcinogenesis mostly is heavy PAHs.European Union's regulation in 2015, from
On April 1st, 2016 rises, and the product of all outlet ports European Union will carry out the detection of 4 kinds of polycyclic aromatic hydrocarbons, and these four polycyclic aromatic hydrocarbon is respectively
For benzo [a] anthracene, bend, benzo [b] fluoranthene and benzo [a] pyrene, and specify that the total amount of these 4 kinds of polycyclic aromatic hydrocarbons not can exceed that 50ug/
Kg, benzopyrene individual event not can exceed that 10ug/kg.
At present for the detection of polycyclic aromatic hydrocarbon and the main method of sample pre-treatments have saponification method, the SPE pillar method of purification,
GCP gel chromatography, enzyme linked immunosorbent assay etc., these sample-pretreating method cycles are long, and cost is high, operation complexity；And adopt
When detecting with gas chromatography combined with mass spectrometry, due to polycyclic arene compound not easily ionizable, cause responding during its Mass Spectrometer Method non-
The lowest, do not reach the testing requirement of limitation.In order to solve the problems referred to above, technical staff have developed following multiple method and carries out many
The detection of PAH:
Application No. 200810237007.X, a kind of method detecting PAHs in Plastic Products, this invention is by plastics
After goods are pulverized, after using the mixed solvent of acetone and dichloromethane to extract, extracting solution is crossed florisil and purifies SPE pillar,
Detect with gas chromatogram-fid detector.
Application No. 201110022991.X, a kind of polycyclic aromatic hydrocarbon detection method, this invention has synthesized a kind of core-shell type
Fe3O4@Ag magnetic nanoparticle, utilizes amyl hydrosulfide to modify nano grain surface.Magnetic nanoparticle after modifying is used
In the enrichment of PAHs, and be observed the raman characteristic peak of PAHs by Portable Raman spectrometer, use ENWAVE portable
Raman spectrometer carries out signals collecting, and the SERS spectrogram obtaining polycyclic aromatic hydrocarbon carries out detection analysis.
Application No. 201310331973.9, polycyclic aromatic hydrocarbon and the detection method of phthalic acid ester in plant extract,
After sample is used water and organic phase solvent to sample extraction by this invention, directly carry out gas chromatogram tandem mass spectrometry and examine
Survey.
Application No. 201410002007.7, a kind of detects the method for polycyclic aromatic hydrocarbon in fried food, and this invention is by sample
Add normal hexane extraction after pulverizing and obtain oil sample, then obtain organic facies after oil sample is added N,N-Dimethylformamide and water extraction, will
Organic facies, after solid phase extraction column carries out enriching and purifying, detects with gaschromatographic mass spectrometry.
Application No. 201410658017.6, the detection preprocess method of polycyclic aromatic hydrocarbon, this invention in a kind of oily sludge
Take oily sludge, add kieselguhr, grind, sieve, extract with extract after mixing, collect extract and concentrate, obtaining
Extraction concentrated solution；By extract after column chromatography eluting, collect eluent, concentrate, and nitrogen purging concentrated solution obtains many cyclophanes
Hydrocarbon samples.
Application No. 201410832327.5, the detection method of polycyclic aromatic hydrocarbon in a kind of edible oil, oil sample is used by this invention
After the mixed solvent of acetone and acetonitrile extracts, centrifugal, take supernatant, supernatant adds alkali liquor and carries out saponification, after centrifugal for saponification liquor,
Taking supernatant to cross decontaminating column and carry out eluting, the mixed solution that will add acetonitrile and acetone after eluent concentrate drying dissolves constant volume, uses
GC-MS detects.
Wang Xiaodong et al. uses solvent extraction, and the method crossing Sep Pak cartridge, by gas chromatography tandem mass spectrometry method to many
PAH detects.
Xu Wenjun et al. uses solvent extraction, and the method crossing gel chromatographic columns, with GC-MS in edible oil
Polycyclic aromatic hydrocarbon detect.
But the problem that said method all exists cycle length, operation is inconvenient and testing cost is high, and the serious shadow of these problems
Having rung the detection of polycyclic aromatic hydrocarbon, quality safety and outlet for product bring huge hidden danger.Set up quickly for this, easy,
The detection technique of low cost is particularly important.
Sulfuric acid purification method is used for sample pre-treatments remove impurity, easy due to it, and quickly, low cost, impurity-eliminating effect is thoroughly etc. excellent
Point, is currently mainly used in the detection of pesticide residues, but owing to industry is cognitive and himself character causes not yet there is people by sulfur
Acid purification method detects for polycyclic aromatic hydrocarbon.
Summary of the invention
For the deficiency in above detection technique, it is an object of the invention to provide a kind of quickly, low cost, simple and effective
Polycyclic aromatic hydrocarbon detection method.
The concrete technical solution of the present invention is as follows:
This polycyclic aromatic hydrocarbon detection method comprises the following steps:
1] extract
Take solid sample pulverize or take comminution solid sample, add the low pole of 5～10 times of sample quality volumes
Solvent extraction, extracting solution adds the weak polar solvent of 5 times of sample quality volumes and dissolves after being concentrated to dryness；
Or taking liquid oily sample, the weak polar solvent being directly added into 5～10 times of sample quality volumes extracts；
Described weak polar solvent is normal hexane, hexamethylene or petroleum ether；
2] acidifying remove impurity
Preparing to step 1 and adding the concentration of gained liquor capacity in 0.5～1 times of step 1 in the solution of gained is 50%
～the sulfuric acid solution of 80%, shake well, stand, make layering；After upper organic phase is crossed microporous filter membrane, treat Mass Spectrometer Method；
3] acidification
Weigh the reference substance of concentration known and dissolve with organic solvent, adding 0.1～0.2 times of reference substance solution volume
Concentration is the sulfuric acid solution of 50%～80%, shake well, stands, makes layering, after upper organic phase is crossed microporous filter membrane, treat matter
Spectrum detection；
4] gaschromatographic mass spectrometry detection
The material of step 2 with step 3 gained is detected with gaschromatographic mass spectrometry simultaneously, and carries out quantitatively by external standard method
Analyze, obtain testing result.
The weak polar solvent extraction adding 5～10 times of sample quality volumes in above-mentioned steps 1 specifically uses ultrasonic carrying
Access method, extracts one to three time altogether.
In above-mentioned steps 4, the testing conditions of gaschromatographic mass spectrometry detection is: injector temperature 280 DEG C, sample size 2.0 μ L,
Input mode: Splitless injecting samples；Chromatographic column: HP-5MS (30m × 0.25mm × 0.25 μm)；Carrier gas: helium (purity >=
99.999%), flow velocity 1.5mL/min, transmission line temperature 280；Temperature programming: initial temperature 60 DEG C, keep 2min, with 20 DEG C/
Min is raised to 200 DEG C, then is raised to 300 DEG C with 5 DEG C/min, keeps 5min；Ionization energy 70eV；Ion source temperature 230 DEG C；Scanning side
Formula SIM pattern.
The invention have the advantages that
Use 5～10 times amount and the close weak organic phase solvent (normal hexane, hexamethylene or petroleum ether) of polycyclic aromatic hydrocarbon polarity
Extract, reduce the polar component interference to detection in sample.
Sample is carried out at acidifying by the sulphuric acid using finite concentration (50%～80%) and a certain amount of (0.5ml～1.0ml)
Reason so that the pre-treatment of sample is simple, easily operates, low cost, and impurity-eliminating effect is obvious, acidification improves multi-ring simultaneously
The aromatic hydrocarbons ionizing efficiency when Mass Spectrometer Method, is effectively improved the sensitivity that 4 kinds of polycyclic aromatic hydrocarbons are detected by mass spectrum.
Standard substance are also adopted by finite concentration and a certain amount of sulphuric acid carries out acidification, make standard substance and sample at mass spectrum
There is during detection identical ionizing efficiency, thus ensure that the impact of cyclophane more than 4 kinds is examined at mass spectrum by sample acidifying dedoping step
Concordance during survey.
Detailed description of the invention
The technological thought of the present invention is:
One, pretreatment of raw material；For the character of polycyclic aromatic hydrocarbon, use weakly polar organic solvent to extract, greatly reduce pole
The dissolution of property composition, reduces the interference of impurity component.
Two, after extracting solution being concentrated into prescribed volume, it is directly added into finite concentration and a certain amount of sulphuric acid purifies.Sulfur
Acid can be with most of material generation sulfonating reactions so that it is character changes thus reaches the effect of remove impurity.It is the most simple to operate,
Low cost, impurity and purification are effective, and the effect of sulphuric acid makes 4 kinds of polycyclic aromatic hydrocarbons ionisation effect when Mass Spectrometer Method substantially increase
By force, make the response value of detection improve a lot on mass spectrum, add the sensitivity of Mass Spectrometer Method.
Three, after being dissolved with the organic solvent of molten sample by the standard substance of 4 kinds of polycyclic aromatic hydrocarbons, take suitable volume, add certain
Concentration and a certain amount of sulphuric acid carry out acidification, make reference substance and sample have identical ionisation effect when Mass Spectrometer Method.
Four, the sample after acidification and standard substance are detected with gaschromatographic mass spectrometry simultaneously.
Above-mentioned whole detection process sulphuric acid impurity and purification are thorough, simple to operate, low cost, and when Mass Spectrometer Method, right
Standard substance carry out acidification simultaneously, make the ionisation effect of 4 kinds of polycyclic aromatic hydrocarbons be remarkably reinforced, and are effectively improved mass spectrum to 4 kinds
The sensitivity of polycyclic aromatic hydrocarbon detection.
Specifically, above-mentioned steps includes:
The concrete scheme of the present invention is as follows:
1] extract
After crushed, employing 5～10 times amount weak polar solvents (petroleum ether, hexamethylene or normal hexane) is ultrasonic to be carried solid sample
Take 2 times, each 30min, filter, united extraction liquid, be concentrated to dryness.Residue adds 5ml n-hexane dissolution.Liquid oils sample is direct
Use normal hexane ultrasonic dissolution.
2] the acidifying remove impurity of sample
Add in normal hexane liquid 0.5～1.0ml 50%～80% sulfuric acid solution, shake well, stand, make point
Layer.After upper organic phase is crossed microporous filter membrane, treat Mass Spectrometer Method.The when of processing polycyclic aromatic hydrocarbon with sulphuric acid acidization, sulphuric acid
Concentration has critically important impact to reaction, and when the concentration of sulphuric acid is less than 50% when, sample solution does not reaches and well removes
Miscellaneous effect, when the concentration of sulphuric acid is higher than 80% when, the response rate of polycyclic aromatic hydrocarbon can reduce.Therefore the selection of sulfuric acid concentration is right
When polyaromatic hydrocarbon samples detects extremely important.
3] acidification of reference substance
Weigh a certain amount of reference substance organic solvent (petroleum ether, hexamethylene or normal hexane) dissolve, add 0.5～
The 50% of 1.0ml～the sulfuric acid solution of 80%, shake well, stand, make layering.After upper organic phase is crossed microporous filter membrane, treat
Mass Spectrometer Method.
4] gaschromatographic mass spectrometry detection
The material of step 2 with step 3 gained is detected with gaschromatographic mass spectrometry simultaneously, and carries out quantitatively by external standard method
Analyze, obtain testing result.Wherein gaschromatographic mass spectrometry testing conditions is: chromatographic column: HP-5MS (30m × 0.25mm × 0.25 μ
m)；Carrier gas: helium (purity >=99.999%), flow velocity 1.5mL/min, transmission line temperature 280；Injector temperature 280 DEG C, sample introduction
Measure 2.0 μ L, input mode: Splitless injecting samples.Temperature programming: initial temperature 60 DEG C, keeps 2min, is raised to 200 with 20 DEG C/min
DEG C, then it is raised to 300 DEG C with 5 DEG C/min, keep 5min；Ionization energy 70eV；Ion source temperature 230 DEG C；Scan mode SIM pattern.
It is further described below in conjunction with embodiment:
Embodiment one
As a example by solid sample, and the standard substance adding 4 kinds of polycyclic aromatic hydrocarbons carry out recovery of standard addition research.Weigh about 5g
Solid sample, add the normal hexane supersound extraction twice of 5 times amount, each 30min, extracting solution merged and is concentrated into 5ml, add
The sulfuric acid solution of 0.6ml 80%, shake well 1 minute, stand, take supernatant to be detected after filtering with microporous membrane.Weigh suitable
The reference substance solution of amount, after adding n-hexane dissolution constant volume, takes 5ml in scale test tube, adds the sulfuric acid solution of 0.6ml 80%,
Shake well 1 minute, stands, takes supernatant to be detected after filtering with microporous membrane.The while of by sample solution and reference substance solution
Detect with gaschromatographic mass spectrometry, carry out quantitative analysis by external standard method.The response rate of actually measured 4 kinds of polycyclic aromatic hydrocarbons is respectively
Benzo [a] anthracene 92%, bends 95%, benzo [b] fluoranthene 90% and benzo [a] pyrene 85%.
Embodiment two
As a example by liquid oily sample, and the standard substance adding 4 kinds of polycyclic aromatic hydrocarbons carry out recovery of standard addition research.Weigh
The oily liquids sample of about 0.2g, after adding the hexamethylene ultrasonic dissolution of 5 times amount, adds the sulfuric acid solution of 0.8ml60%, fully
Shake 1 minute, stand, take supernatant to be detected after filtering with microporous membrane.Weigh appropriate reference substance solution, add hexamethylene molten
Solve after constant volume, take 5ml in scale test tube, add the sulfuric acid solution of 0.8ml 60%, shake well 1 minute, stand, take supernatant
Liquid is to be detected after filtering with microporous membrane.Sample solution and reference substance solution are detected with gaschromatographic mass spectrometry simultaneously, uses
External standard method carries out quantitative analysis.The response rate of actually measured 4 kinds of polycyclic aromatic hydrocarbons is respectively benzo [a] anthracene 90%, bends 93%, benzo
[b] fluoranthene 87% and benzo [a] pyrene 84%.
Embodiment three
As a example by solid sample, and the standard substance adding 4 kinds of polycyclic aromatic hydrocarbons carry out recovery of standard addition research.Weigh about 5g
Solid sample, add the petroleum ether supersound extraction twice of 6 times amount, each 30min, extracting solution merged and is concentrated into 5ml, add
The sulfuric acid solution of 0.9ml 50%, shake well 1 minute, stand, take supernatant to be detected after filtering with microporous membrane.Weigh suitable
The reference substance solution of amount, after adding petroleum ether dissolution constant volume, takes 5ml in scale test tube, adds the sulfuric acid solution of 0.8ml 50%,
Shake well 1 minute, stands, takes supernatant to be detected after filtering with microporous membrane.The while of by sample solution and reference substance solution
Detect with gaschromatographic mass spectrometry, carry out quantitative analysis by external standard method.The response rate of actually measured 4 kinds of polycyclic aromatic hydrocarbons is respectively
Benzo [a] anthracene 83%, bends 87%, benzo [b] fluoranthene 90% and benzo [a] pyrene 93%.
Embodiment four
As a example by liquid oily sample, and the standard substance adding 4 kinds of polycyclic aromatic hydrocarbons carry out recovery of standard addition research.Weigh
The oily liquids sample of about 0.2g, after adding the normal hexane ultrasonic dissolution of 8 times amount, adds the sulfuric acid solution of 0.6ml80%, fully
Shake 1 minute, stand, take supernatant to be detected after filtering with microporous membrane.Weigh appropriate reference substance solution, n-hexane dissolution
After constant volume, take 5ml in scale test tube, add the sulfuric acid solution of 0.6ml80%, shake well 1 minute, stand, take supernatant
After filtering with microporous membrane to be detected.Sample solution and reference substance solution are detected with gaschromatographic mass spectrometry simultaneously, with outward
Mark method carries out quantitative analysis.The response rate of actually measured 4 kinds of polycyclic aromatic hydrocarbons is respectively benzo [a] anthracene 85%, bends 90%, benzo
[b] fluoranthene 91% and benzo [a] pyrene 94%.
Embodiment five
As a example by solid sample, and the standard substance adding 4 kinds of polycyclic aromatic hydrocarbons carry out recovery of standard addition research.Weigh about 3g
Solid sample, add 60min of organic solvent petroleum ether supersound extraction of 8 times amount, by extracting solution merge be concentrated into 5ml,
Add the sulfuric acid solution of 0.8ml 70%, shake well 1 minute, stand, take supernatant to be detected after filtering with microporous membrane.Weigh
Appropriate reference substance solution, after adding petroleum ether dissolution constant volume, takes 5ml in scale test tube, and the sulphuric acid adding 0.8ml 70% is molten
Liquid, shake well 1 minute, stand, take supernatant to be detected after filtering with microporous membrane.By same to sample solution and reference substance solution
Time detect with gaschromatographic mass spectrometry, carry out quantitative analysis by external standard method.The response rate of actually measured 4 kinds of polycyclic aromatic hydrocarbons is respectively
For benzo [a] anthracene 93%, bend 97%, benzo [b] fluoranthene 88% and benzo [a] pyrene 87%.
Embodiment six
As a example by liquid oily sample, and the standard substance adding 4 kinds of polycyclic aromatic hydrocarbons carry out recovery of standard addition research.Weigh 2g
The oily liquids sample of left and right, after adding the organic solvent-normal hexane ultrasonic dissolution of 7 times amount, adds the sulfuric acid solution of 1ml 50%,
Shake well 1 minute, stands, takes supernatant to be detected after filtering with microporous membrane.Weigh appropriate reference substance solution, add organic
Solvent hexane dissolves after constant volume, takes 5ml in scale test tube, adds the sulfuric acid solution of 1ml 50%, shake well 1 minute,
Stand, take supernatant to be detected after filtering with microporous membrane.Sample solution and reference substance solution are used gaschromatographic mass spectrometry simultaneously
Detect, carry out quantitative analysis by external standard method.The response rate of actually measured 4 kinds of polycyclic aromatic hydrocarbons is respectively benzo [a] anthracene 90%,
Bend 93%, benzo [b] fluoranthene 87% and benzo [a] pyrene 84%.
Embodiment seven
As a example by solid sample, and the standard substance adding 4 kinds of polycyclic aromatic hydrocarbons carry out recovery of standard addition research.Weigh 33g left
Right solid sample, adds the organic solvent hexamethylene supersound extraction twice of 10 times amount, each 35min, is merged by extracting solution dense
It is reduced to 5ml, adds the sulfuric acid solution of 0.5ml 80%, shake well 1 minute, stand, take supernatant and treat after filtering with microporous membrane
Detection.Weigh appropriate reference substance solution, add organic solvent hexamethylene and dissolve after constant volume, take 5ml in scale test tube, add
The sulfuric acid solution of 0.5ml80%, shake well 1 minute, stand, take supernatant to be detected after filtering with microporous membrane.By sample
Solution and reference substance solution detect with gaschromatographic mass spectrometry simultaneously, carry out quantitative analysis by external standard method.Actually measured more than 4 kinds
The response rate of PAH is respectively benzo [a] anthracene 89%, bends 91%, benzo [b] fluoranthene 91% and benzo [a] pyrene 90%.
Embodiment eight
As a example by liquid oily sample, and the standard substance adding 4 kinds of polycyclic aromatic hydrocarbons carry out recovery of standard addition research.Weigh
The oily liquids sample of about 0.8g, after adding the organic solvent-normal hexane ultrasonic dissolution of 10 times amount, adds the sulphuric acid of 1ml 77%
Solution, shake well 1 minute, stand, take supernatant to be detected after filtering with microporous membrane.Weigh appropriate reference substance solution,
Add organic solvent-normal hexane to dissolve after constant volume, take 5ml in scale test tube, add the sulfuric acid solution of 1ml 77%, shake well 1
Minute, stand, take supernatant to be detected after filtering with microporous membrane.Sample solution and reference substance solution are used gas chromatogram simultaneously
Mass spectrum detects, and carries out quantitative analysis by external standard method.The response rate of actually measured 4 kinds of polycyclic aromatic hydrocarbons is respectively benzo [a] anthracene
93%, bend 94%, benzo [b] fluoranthene 92% and benzo [a] pyrene 82%.
Claims (4)
1. a polycyclic aromatic hydrocarbon detection method, it is characterised in that comprise the following steps:
1] extract
Take solid sample pulverize or take comminution solid sample, add the weak polar solvent of 5～10 times of sample quality volumes
Extracting, extracting solution adds the weak polar solvent of 5 times of sample quality volumes and dissolves after being concentrated to dryness；
Or taking liquid oily sample, the weak polar solvent being directly added into 5～10 times of sample quality volumes extracts；
2] acidifying remove impurity
Prepare to step 1 solution of gained adds the concentration of gained liquor capacity in 0.5～1 times of step 1 be 50%～
The sulfuric acid solution of 80%, shake well, stand, make layering；After upper organic phase is crossed microporous filter membrane, treat Mass Spectrometer Method；
3] acidification
Weighing the reference substance of concentration known and dissolve with organic solvent, the concentration adding 0.1～0.2 times of reference substance volume is
The sulfuric acid solution of 50%～80%, shake well, stand, make layering, after upper organic phase is crossed microporous filter membrane, treat that mass spectrum is examined
Survey；
4] gaschromatographic mass spectrometry detection
The material of step 2 with step 3 gained is detected with gaschromatographic mass spectrometry simultaneously, and quantitatively divides by external standard method
Analysis, obtains testing result.
Polycyclic aromatic hydrocarbon detection method the most according to claim 1, it is characterised in that: described weak polar solvent is normal hexane,
Hexamethylene or petroleum ether.
Polycyclic aromatic hydrocarbon detection method the most according to claim 1, it is characterised in that: described step 1 adds low pole molten
Agent is extracted and is specifically used ultrasonic extracting method, extracts one to three time altogether.
4. according to the arbitrary described polycyclic aromatic hydrocarbon detection method of claims 1 to 3, it is characterised in that: gas phase color in described step 4
The testing conditions of spectrum Mass Spectrometer Method is: injector temperature 280 DEG C, sample size 2.0 μ L, input mode: Splitless injecting samples；Chromatograph
Post: HP-5MS (30m × 0.25mm × 0.25 μm)；Carrier gas: helium (purity >=99.999%), flow velocity 1.5mL/min, transmission line
Temperature 280；Temperature programming: initial temperature 60 DEG C, keeps 2min, is raised to 200 DEG C with 20 DEG C/min, then is raised to 300 with 5 DEG C/min
DEG C, keep 5min；Ionization energy 70eV；Ion source temperature 230 DEG C；Scan mode SIM pattern.
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| CN111562334A (en) * | 2020-06-09 | 2020-08-21 | 劲牌有限公司 | Method for detecting polycyclic aromatic hydrocarbon residue in plant traditional Chinese medicinal materials and extracts |
| CN112147257A (en) * | 2017-03-24 | 2020-12-29 | 上海安谱实验科技股份有限公司 | Method for extracting polycyclic aromatic hydrocarbon from PET (polyethylene terephthalate) product |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112147257A (en) * | 2017-03-24 | 2020-12-29 | 上海安谱实验科技股份有限公司 | Method for extracting polycyclic aromatic hydrocarbon from PET (polyethylene terephthalate) product |
| CN108896674A (en) * | 2018-07-04 | 2018-11-27 | 肇庆市创业帮信息技术有限公司 | The detection method of polycyclic aromatic hydrocarbon in a kind of meat products |
| CN111562334A (en) * | 2020-06-09 | 2020-08-21 | 劲牌有限公司 | Method for detecting polycyclic aromatic hydrocarbon residue in plant traditional Chinese medicinal materials and extracts |
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