CN108414652A - The detection method of anthracene and its oxide anthraquinone, anthrone content in multi-interfacial feature - Google Patents
The detection method of anthracene and its oxide anthraquinone, anthrone content in multi-interfacial feature Download PDFInfo
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Abstract
The present invention relates to the detection methods of anthracene in multi-interfacial feature and its oxide anthraquinone, anthrone content.This method includes：（1）Sample pre-treatments；（2）Instrument detects；The assay method of the present invention measures air, soil and the anthracene in water, anthraquinone, anthrone content using GC MS/MS, and method is easy to operate, and detection limit, the rate of recovery and precision etc. are satisfied by environmental monitoring requirement.
Description
Technical field
The present invention relates to polycyclic aromatic hydrocarbon compounds detection technique fields, and in particular to anthracene and its oxygen in a kind of multi-interfacial feature
The detection method of compound anthraquinone, anthrone content.
Background technology
Polycyclic aromatic hydrocarbon（PAHs）Compound is a kind of persistence organic pollutant of generally existing in environment, have it is carcinogenic,
Teratogenesis, mutagenesis.In process of crop growth, it can be enriched with the PAHs in the multimediums such as air, soil and water, to
Cause Food Quality Safety, threat is brought to human health.Anthracene（Anthracene ANT,CAS No 120-12-7,
C14H10）, it is widely used in the industry such as dyestuff, paper pulp, mainly by the fossil fuels such as oil, coal, solid waste such as timber, tobacco
It is generated in equal partial combustion process, is that one of 16 kinds of PAHs priority pollutants are confirmed by Environmental Protection Agency；The main oxidation of AN
Product is anthraquinone（Anthraquinone AQ, CAS No 84-65-1, C14H8O2）And anthrone（Anthrone AT, CAS No
90-44-8, C14H10O）, wherein AQ is reduced compared to ANT toxicity, but is also arranged by international cancer research institution of the World Health Organization
Enter 2B class carcinogenic substances.Currently, not had been reported that about the detection method of ANT and its oxidation product AQ and AT in the environment.
Invention content
In view of the problems of the existing technology, it is an object of the invention to design provide in a kind of multi-interfacial feature anthracene and its
Oxide anthraquinone, anthrone content detection method technical solution, this method can be that source, conversion and the biology of AN be repaiied in environment
Multiple wait provides technical support.
The detection method of anthracene and its oxide anthraquinone, anthrone content in the multi-interfacial feature, it is characterised in that including
Following steps：
1）Sample pre-treatments
Air：It is 4 to take air sample dichloromethane and acetone volume ratio：1 mixed solution ultrasonic extraction 3 times merges all
Supernatant after concentrating constant volume, waits for that GC-MS/MS is analyzed without purification；
Soil：It is 1 to take pedotheque dichloromethane and acetone volume ratio：1 mixed solution vortex oscillation-ultrasonic extraction, from
Supernatant is taken after the heart, without purification, after concentrating constant volume, waits for that GC-MS/MS is analyzed；
Water：Sample of fetching water distributes extraction merging filtrate with dichloromethane solution liquid, and GC-MS/MS is waited for after concentrating constant volume without purification
Analysis；
2）Instrument detects
Standard working solution and the sample solution sample introduction under the GC-MS/MS Parameter Conditions of following setting；
Mass spectrometry parameters：
Instrument condition parameter：
Chromatographic column：Agilent J&W GC VF-5ms；Ionization mode：EI；Electron energy：70 eV；Ion source temperature：210
℃；Interface temperature：280 ℃；Injector temperature：250 ℃；Program column temperature：80 DEG C of initial temperature, is warming up to 15 DEG C/min
240 DEG C, then 280 DEG C are warming up to 25 DEG C/min, retain 5 min.Carrier gas：Helium 99.999%, 1.0 mL/min of flow velocity；It touches
Hit gas:Argon gas 99.999%, 2.0 mTorr；Sample size：1 μL；Input mode does not shunt；
Mensuration mode：Selective reaction monitoring pattern, with respect to the maximum allowable offset of abundance of ions when qualitative confirmation：Relative ion is rich
Spend ＞ 50%, relative deviation ± 20% of permission；Relative ion abundance ＞ 20%~50%, relative deviation ± 25% of permission；
Relative ion abundance ＞ 10%~20%, relative deviation ± 30% of permission；Relative ion abundance≤10%, permission it is opposite
Deviation ± 50%；
3）Blank test
In addition to being not added with sample, press above-mentioned steps 1), step 2) operating procedure carry out；
4）Interpretation of result and calculating
Using mass concentration as abscissa X, peak area ratio is ordinate Y, draws 5 standard working curves, is worked with standard
Curve quantifies sample, and the response of drug should be in the range of linearity that instrument detects in sample solution；In above-mentioned chromatography
Under the conditions of, it whether there is corresponding measured object in judgement sample, need to meet following condition：The mass spectrum color occurred in sample solution
Spectral peak retention time is consistent with standard items working solution, and tolerance is less than ± 0.5%, and the drug corresponding to the chromatographic peak is in mass spectrum
The relative abundance of qualitative ion is consistent with the comparable relative abundance of mixed-matrix standard working solution of concentration, and relative abundance deviation is not
More than above-mentioned regulation, then can determine containing the drug；
Chromatographic software is used in combination or calculates the content of anthraquinone in sample as follows, result of calculation needs to deduct blank：
In formula：X i The residual quantity of i component drugs, mg/kg in sample；
As：The peak area of i component drugs in sample；
Asi：The peak area of i component drugs in standard specimen；
Csi：The content ng/ μ L of i component drugs in standard specimen；
Cf：Improvement factor；
V 1 ：Standard specimen sample size, μ L；
V 2 ：Extracting solution total volume, mL；
V 3 ：Divide and takes extracting liquid volume, mL；
V 4 ：Sample constant volume, mL；
V 5 ：Sample injection volume, μ L；
m：The quality of sample, g.
The detection method of anthracene and its oxide anthraquinone, anthrone content in the multi-interfacial feature, it is characterised in that air
Sample pre-treatments are specially：Glass fibre membrane is taken, is 4 with 15mL dichloromethane and acetone volume ratio：1 mixed solution ultrasound
Immersion 30min, is extracted 3 times by above-mentioned solution, merges whole supernatants, 35 DEG C of rotary evaporations of water-bath are done to close, with a concentration of 0.04
Mg/L anthraquinone-d8 n-hexanes and acetone volume ratio are 39:1 mixed solution is settled to 1mL, crosses 0.22 μm of filter membrane, waits for GC-
MS/MS is analyzed.
The detection method of anthracene and its oxide anthraquinone, anthrone content in the multi-interfacial feature, it is characterised in that soil
Sample pre-treatments are specially：It takes 2 g pedotheques in 50 mL polytetrafluoroethylene (PTFE) centrifuge tubes, 20 mL dichloromethane is added：Acetone
Volume ratio is 1：1 mixed solution, 1 min ultrasonic wave extractions of vortex oscillation, 30 min, 1 g anhydrous magnesium sulfates of addition shake up cold
But, 30 s of vortex oscillation, 6000 r/min centrifuge 5 min, take 10 mL supernatants in 35 DEG C of rotary evaporations of heart bottle to close
It is dry, it is 39 with anthraquinone-d8 n-hexanes and acetone volume ratio:1 mixed solution is settled to 1mL, 0.22 μm of filter membrane is crossed, into GC-
MS/MS is analyzed.
The detection method of anthracene and its oxide anthraquinone, anthrone content in the multi-interfacial feature, it is characterised in that water sample
Product pre-treatment is specially：It takes 100mL water samples in 250 mL separatory funnels, 25 mL dichloromethane is added, shake up and carry out liquid liquid extraction
It takes 2 times, merges lower liquid, 35 DEG C of rotary evaporations of water-bath are done to close, with a concentration of 0.04 mg/L anthraquinone-d8 n-hexanes and third
Ketone volume ratio is 39:1 mixed solution is settled to 1mL, crosses 0.22 μm of filter membrane, waits for that GC-MS/MS is analyzed.
The present invention develops GC-MS/MS in multi-environment medium while measuring anthracene and its metabolite anthraquinone and anthrone for the first time,
Technological gap is filled up.In addition the present invention provides the optimal items of anthracene, anthraquinone and anthrone in GC-MS/MS method determination of the environment samples
Part.
Description of the drawings
Fig. 1 structural formula of compound（From left to right it is followed successively by A anthracenes, B anthraquinones, C anthrones, D anthraquinones-D8）；
Fig. 2 air samples（From left to right it is followed successively by blank, matrix mark-on -20ppb）Mass spectrogram；
Fig. 3 pedotheques（From left to right it is followed successively by blank, matrix mark-on -100ppb）Mass spectrogram；
Fig. 4 water samples（From left to right it is followed successively by blank, matrix mark-on -10ppb）Mass spectrogram；
A is anthracene in Fig. 2-4, B is anthraquinone, C is anthrone, D is anthraquinone-D8.
Specific implementation mode
It further illustrates the present invention with reference to embodiments.
Embodiment
1, reagent and material
1.1 n-hexanes, acetone, dichloromethane are chromatographic grade；Anthracene, anthraquinone, anthrone, anthraquinone-D8 standard substances
(Anthracene CAS:120-12-7, Anthraquinone CAS:84-65-1, Anthrone CAS:90-44-8,
Anthraquinone-D8 CAS:10439-39-1) ：Purity is more than or equal to 99%.
1.2 Standard Stock solutions：It accurately weighs through appropriate standard substance (1.1), is configured to 0.4mg/mL's with acetone
Single mark storing solution, in being protected from light storage, the term of validity 6 months in 0 DEG C~4 DEG C refrigerators.
The preparation of 1.3 standard working solutions：Above-mentioned standard stock solution (1.2) is diluted to acetone as needed
The standard working solution of debita spissitudo, in being protected from light storage, the term of validity 6 months in 0 DEG C~4 DEG C refrigerators.
1.4 miillpore filter：0.22 μm, organic facies pattern.
2, instrument and equipment
GC-MS/MS (EI ion sources)；Assay balance (precision 0.000 1g and 0.01g)；Turbine mixer；Homogenizer；
Oscillator；Height centrifuge；Rotary Evaporators；Pulverizer.Supersonic wave cleaning machine；Low-temperature cooling fluid circulating pump.
3, determination step
3.1 sample pre-treatments
Air：Clip half glass fibre membrane, with 15mL dichloromethane：Acetone（4：1）Ultrasound impregnates 30min, by above-mentioned solution
Extraction 3 times merges whole supernatants, and 35 DEG C of rotary evaporations of water-bath are done to close, with a concentration of 0.04 mg/L anthraquinones-d8 n-hexanes：Third
Ketone（39:1）It is settled to 1mL, crosses 0.22 μm of filter membrane（Without purification）, wait for that GC-MS/MS is analyzed.
Soil：20 mL dichloromethane are added in 50 mL polytetrafluoroethylene (PTFE) centrifuge tubes in 2 g samples：Acetone（1：1）, it is vortexed
1 min ultrasonic wave extractions, 30 min is vibrated, 1 g anhydrous magnesium sulfates are added and shake up cooling.Vortex oscillation 30 s, 6000 r/min
5 min are centrifuged, take 10 mL supernatants to be done to close in 35 DEG C of rotary evaporations of heart bottle, with anthraquinone-d8 n-hexanes：Acetone（39:1）
It is settled to 1mL, crosses 0.22 μm of filter membrane（Without purification）, analyzed into GC-MS/MS.
Water：It takes 100mL water samples in 250 mL separatory funnels, 25 mL dichloromethane is added, shake up and carry out liquid-liquid extraction 2
It is secondary.Merge lower liquid, 35 DEG C of rotary evaporations of water-bath are done to close, with a concentration of 0.04 mg/L anthraquinones-d8 n-hexanes：Acetone
（39:1）It is settled to 1mL, crosses 0.22 μm of filter membrane（Without purification）, wait for that GC-MS/MS is analyzed.
3.2 instruments detect
Since different model instrument is there are some chromatographic condition differences, condition presented below has proved to be applicable, specifically
Parameter is shown in Table 1, and mass spectrometry parameters are shown in Table 2.
1 GC-MS/MS Parameter Conditions of table
2 mass spectrometry parameters of table
* quota ion is indicated
4, blank test
In addition to being not added with sample, presses aforesaid operations step and carry out.
5, interpretation of result and calculating
Using mass concentration as abscissa X, peak area ratio is ordinate Y, 5 standard working curves is drawn, with standard work
Make curve to quantify sample, the response of drug should be in the range of linearity that instrument detects in sample solution；In above-mentioned color
Under spectral condition, it whether there is corresponding measured object in judgement sample, need to meet following condition：The mass spectrum occurred in sample solution
Chromatographic peak retention time is consistent with standard items working solution, and tolerance is less than ± 0.5%, and the drug corresponding to the chromatographic peak is in matter
The relative abundance for composing qualitative ion is consistent with the comparable relative abundance of mixed-matrix standard working solution of concentration, relative abundance deviation
No more than above-mentioned regulation, then can determine containing the drug.
The content of anthraquinone in sample is calculated with chromatographic software or as follows, and result of calculation needs to deduct blank：
In formula：X i The residual quantity of i component drugs, mg/kg in sample；
As：The peak area of i component drugs in sample；
Asi：The peak area of i component drugs in standard specimen；
Csi：The content ng/ μ L of i component drugs in standard specimen；
Cf：Improvement factor；
V 1 ：Standard specimen sample size, μ L；
V 2 ：Extracting solution total volume, mL；
V 3 ：Divide and takes extracting liquid volume, mL；
V 4 ：Sample constant volume, mL；
V 5 ：Sample injection volume, μ L；
m：The quality of sample, g.
6, minimum detection limit
The lower limit of measurement of this method is 0.2 μ g/kg.
7, the rate of recovery
This method recovery test sets three addition concentration, experiment condition determined by the method by the present embodiment, to each
Add concentration and carry out 3 experiments, the rate of recovery and precision the results are shown in Table 3, air sample, pedotheque and water sample mass spectrogram
As in Figure 2-4.
3 sample of table adds concentration and rate of recovery range
。
Claims (4)
1. the detection method of anthracene and its oxide anthraquinone, anthrone content in multi-interfacial feature, it is characterised in that include the following steps：
1）Sample pre-treatments
Air：It is 4 to take air sample dichloromethane and acetone volume ratio：1 mixed solution ultrasonic extraction 3 times merges all
Supernatant after concentrating constant volume, waits for that GC-MS/MS is analyzed without purification；
Soil：It is 1 to take pedotheque dichloromethane and acetone volume ratio：1 mixed solution vortex oscillation-ultrasonic extraction, from
Supernatant is taken after the heart, without purification, after concentrating constant volume, waits for that GC-MS/MS is analyzed；
Water：Sample of fetching water distributes extraction merging filtrate with dichloromethane solution liquid, and GC-MS/MS is waited for after concentrating constant volume without purification
Analysis；
2）Instrument detects
Standard working solution and the sample solution sample introduction under the GC-MS/MS Parameter Conditions of following setting；
Mass spectrometry parameters：
Instrument condition parameter：
Chromatographic column：Agilent J&W GC VF-5ms；Ionization mode：EI；Electron energy：70 eV；Ion source temperature：210
℃；Interface temperature：280 ℃；Injector temperature：250 ℃；Program column temperature：80 DEG C of initial temperature, is warming up to 15 DEG C/min
240 DEG C, then 280 DEG C are warming up to 25 DEG C/min, retain 5 min；Carrier gas：Helium 99.999%, 1.0 mL/min of flow velocity；It touches
Hit gas:Argon gas 99.999%, 2.0 mTorr；Sample size：1 μL；Input mode does not shunt；
Mensuration mode：
Selective reaction monitoring pattern, with respect to the maximum allowable offset of abundance of ions when qualitative confirmation：Relative ion abundance ＞ 50%,
Relative deviation ± 20% of permission；Relative ion abundance ＞ 20%~50%, relative deviation ± 25% of permission；It is opposite from
Sub- abundance ＞ 10%~20%, relative deviation ± 30% of permission；Relative ion abundance≤10%, the relative deviation of permission ±
50%；
3）Blank test
In addition to being not added with sample, press above-mentioned steps 1), step 2) operating procedure carry out；
4）Interpretation of result and calculating
Using mass concentration as abscissa X, peak area ratio is ordinate Y, 5 standard working curves is drawn, with standard work
Make curve to quantify sample, the response of drug should be in the range of linearity that instrument detects in sample solution；In above-mentioned color
Under spectral condition, it whether there is corresponding measured object in judgement sample, need to meet following condition：The mass spectrum occurred in sample solution
Chromatographic peak retention time is consistent with standard items working solution, and tolerance is less than ± 0.5%, and the drug corresponding to the chromatographic peak is in matter
The relative abundance for composing qualitative ion is consistent with the comparable relative abundance of mixed-matrix standard working solution of concentration, relative abundance deviation
No more than above-mentioned regulation, then can determine containing the drug；
Chromatographic software is used in combination or calculates the content of anthraquinone in sample as follows, result of calculation needs to deduct blank：
In formula：X i The residual quantity of i component drugs, mg/kg in sample；
As：The peak area of i component drugs in sample；
Asi：The peak area of i component drugs in standard specimen；
Csi：The content ng/ μ L of i component drugs in standard specimen；
Cf：Improvement factor；
V 1 ：Standard specimen sample size, μ L；
V 2 ：Extracting solution total volume, mL；
V 3 ：Divide and takes extracting liquid volume, mL；
V 4 ：Sample constant volume, mL；
V 5 ：Sample injection volume, μ L；
m：The quality of sample, g.
2. the detection method of anthracene and its oxide anthraquinone, anthrone content in multi-interfacial feature according to claim 1, special
Sign is that air sample pre-treatment is specially：Glass fibre membrane is taken, is 4 with 15mL dichloromethane and acetone volume ratio：1 it is mixed
It closes solution ultrasound and impregnates 30min, by above-mentioned solution extraction 3 times, merge whole supernatants, 35 DEG C of rotary evaporations of water-bath to close dry, use
A concentration of 0.04 mg/L anthraquinone-d8 n-hexanes and acetone volume ratio are 39:1 mixed solution is settled to 1mL, crosses 0.22 μm
Filter membrane waits for that GC-MS/MS is analyzed.
3. the detection method of anthracene and its oxide anthraquinone, anthrone content in multi-interfacial feature according to claim 1, special
Sign is that pedotheque pre-treatment is specially：It takes 2 g pedotheques in 50 mL polytetrafluoroethylene (PTFE) centrifuge tubes, 20 mL dichloros is added
Methane：Acetone volume ratio is 1：1 g anhydrous slufuric acids are added in 1 mixed solution, 1 min ultrasonic wave extractions of vortex oscillation, 30 min
Magnesium shakes up cooling, and vortex oscillation 30 s, 6000 r/min centrifuge 5 min, and 10 mL supernatants is taken to be steamed in the 35 DEG C of rotations of heart bottle
It is sent to and closely does, be 39 with anthraquinone-d8 n-hexanes and acetone volume ratio:1 mixed solution is settled to 1mL, crosses 0.22 μm of filter membrane,
It is analyzed into GC-MS/MS.
4. the detection method of anthracene and its oxide anthraquinone, anthrone content in multi-interfacial feature according to claim 1, special
Sign is that water sample pre-treatment is specially：It takes 100mL water samples in 250 mL separatory funnels, 25 mL dichloromethane is added, shake up
Liquid-liquid extraction 2 times is carried out, merges lower liquid, 35 DEG C of rotary evaporations of water-bath are done to close, with a concentration of 0.04 mg/L anthraquinones-d8
N-hexane and acetone volume ratio are 39:1 mixed solution is settled to 1mL, crosses 0.22 μm of filter membrane, waits for that GC-MS/MS is analyzed.
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Cited By (2)
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| CN111272909A (en) * | 2020-04-23 | 2020-06-12 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone and anthrone substances in soil and sediment |
| CN111272908A (en) * | 2020-04-23 | 2020-06-12 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone and anthrone substances in water |
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| YEHUA HAN等: ""Supercritical fluid extraction with carbon nanotubes as a solidcollection trap for the analysis of polycyclic aromatic hydrocarbonsand their derivatives"", 《JOURNAL OF CHROMATOGRAPHY A》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111272909A (en) * | 2020-04-23 | 2020-06-12 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone and anthrone substances in soil and sediment |
| CN111272908A (en) * | 2020-04-23 | 2020-06-12 | 上海国齐检测技术有限公司 | Method for detecting anthraquinone and anthrone substances in water |
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