CN108872415A - The analyzing detecting method of monohydroxy polycyclic aromatic hydrocarbon in a kind of urine - Google Patents
The analyzing detecting method of monohydroxy polycyclic aromatic hydrocarbon in a kind of urine Download PDFInfo
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- CN108872415A CN108872415A CN201810414324.8A CN201810414324A CN108872415A CN 108872415 A CN108872415 A CN 108872415A CN 201810414324 A CN201810414324 A CN 201810414324A CN 108872415 A CN108872415 A CN 108872415A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
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- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
- G01N30/724—Nebulising, aerosol formation or ionisation
- G01N30/7266—Nebulising, aerosol formation or ionisation by electric field, e.g. electrospray
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- G—PHYSICS
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- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid 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
- G01N2030/062—Preparation extracting sample from raw material
Abstract
It is to establish Solid Phase Extraction-liquid chromatography-tandem mass spectrometry while measuring luxuriant and rich with fragrance 1- hydroxyl naphthalene, 2 hydroxy naphthalene, 2- hydroxyphenyl fluorene, 1- hydroxyl, 2- hydroxyl phenanthrene, 3- hydroxyl phenanthrene, 4- hydroxyl phenanthrene, 9- hydroxyl phenanthrene, 1- hydroxyl pyrene and 6- hydroxyl the invention discloses a kind of analyzing detecting method of monohydroxy polycyclic aromatic hydrocarbon in urineMethod, by 2mL urine through enzyme hydrolysis, after CNWBOND HC-C18 solid phase extraction column enrichment purification, it is eluted with 10mL methanol, nitrogen is blown to close dry under soft nitrogen, with methanol constant volume to 1mL, with chromatographic column isolating target compound, detected under electric spray ion source negative ion mode.The advantage of the invention is that：The detection research of the polycyclic aromatic hydrocarbon exposure suitable for the urine of biological sample, can measure 10 kinds of monohydroxy polycyclic aromatic hydrocarbons in human urine simultaneously, have the advantages that pre-treatment is simple, detection limit is low, stability is good, accuracy is good.
Description
Technical field
The present invention relates to polycyclic aromatic hydrocarbon detection technique field, in particular to the analysis of monohydroxy polycyclic aromatic hydrocarbon in a kind of urine
Detection method.
Background technique
Polycyclic aromatic hydrocarbon is that (PAHs) refers to arene in molecule containing two or more phenyl ring, common to have
Naphthalene, fluorenes, phenanthrene, pyrene etc..Polycyclic aromatic hydrocarbon in environment be mainly derived from the organic matters such as coal, petroleum, timber pyrolysis and not exclusively
Burning.Existing result of study shows that PAHs has detection in the surrounding mediums such as empty gas and water, soil, in the biological sample,
As being also found in blood, urine and hair.
The measurement process of OH-PAHs includes that sample pre-treatments and instrument detect two parts in urine.Wherein before sample
Reason process has an impact to detection limit, stability and the accuracy etc. of detection method, the extraction skill of the OH-PAHs reported at present
Art mainly has the methods of Solid Phase Extraction, solid phase microextraction, liquid-liquid extraction, but the most mature with solid phase extraction techniques at present, effect
Stablize, is most common abstraction technique.
The instrument detection method of OH-PAHs mainly includes high performance liquid chromatography (HPLC) method, liquid phase (gas phase) chromatography-at present
Mass spectrometry (LC/GC-MS) method, Synchronous fluorimetric method, capillary electrophoresis, enzyme-linked immunization (ELISA) and electrochemistry
Method etc..Although HPLC has the characteristics that sensitive, accurate, detection limit is low, treatment process is excessively complicated, is not easily applicable to a large amount of
The detection of sample；The sample of synchronous fluorimetry does not need to pre-process, although easy to operate, interference is too big；Capillary electricity
Swimming method has many advantages, such as good separating effect, analysis speed is fast and reproducibility is preferable, but its application range is relatively narrow；
ELISA method specificity is stronger, and sensitivity is also higher, but interference is too big, is easy to appear cross reaction；GC-MS method is to same point
The measurement of isomers has advantage, but sample needs derivatization treatment, and pretreatment process is excessively complicated.
Summary of the invention
The present invention in view of the drawbacks of the prior art, provides a kind of analysis detection side of monohydroxy polycyclic aromatic hydrocarbon in urine
Method can effectively solve the above-mentioned problems of the prior art.In order to realize the above goal of the invention, the technical side that the present invention takes
Case is as follows：
The analyzing detecting method of monohydroxy polycyclic aromatic hydrocarbon, includes the following steps in a kind of urine：
Step 1, the singly mark solution of 10 kinds of monohydroxy polycyclic aromatic hydrocarbon standard items is prepared, then appropriate 10 kinds of singly mark solutions is taken to be made into
Mixed standard solution containing various monohydroxy polycyclic aromatic hydrocarbons and the mixing inner mark solution containing 2 kinds of deuterated Hydroxyl Polycyclic Aromatics.
The standard curve of 10 kinds of monohydroxy polycyclic aromatic hydrocarbons is established by liquid chromatography-tandem mass spectrometry method.
Step 2, urine sample is thawed at room temperature, 2mL urine sample is accurately pipetted after urine defrosting, 10mL tool plug is added
In centrifuge tube, and 3mL acetic acid-sodium acetate buffer solution is added in centrifuge tube, accurately pipette 10 μ L β-grape respectively later
Glycuronide/aryl sulphatase and mixing internal standard solution are added in centrifuge tube, are uniformly mixed with turbula shaker, by centrifuge tube corking
37 DEG C of water-bath 12h of thermostatic control oscillator vibration are put into after good, is taken out after water-bath 12h and prepared SPE pillar.
Step 3, SPE pillar is attached on 12 hole solid-phase extraction devices, taking 5mL methanol to be added in SPE pillar fills it
Divide activation, adding 5mL ultrapure water makes its balance, and keeps sample with 1mL/ not entirely through preceding addition sample in ultrapure water
The rate of min passes through.
Step 4, after sample passes through SPE pillar completely, 4mL ultrapure water is added and elutes extraction column, passes through extraction to leacheate
After taking column, 1min is kept under vacuum conditions, is sufficiently removed the moisture in SPE pillar, then elute pillar with the methanol of 10mL, is received
Collection eluent nitrogen into test tube, which is blown to, closely to be done, and with methanol constant volume to 1mL, after mixing with turbula shaker, crosses 0.2 μm of aperture
The syringe needle filter of organic filter membrane is filtered into brown sample bottle, to sample introduction.
Step 5, after obtaining a result, the standard serial solution for being 10 μ g/mL according to the inner mark solution concentration in above-mentioned steps 1
Describe and finds 10 kinds of monohydroxy polycyclic aromatic hydrocarbon contents in sample on the standard curve of system.
Further, 10 kinds of monohydroxy polycyclic aromatic hydrocarbon standard items are in the step 1：1- hydroxyl naphthalene, 2 hydroxy naphthalene, 2- hydroxyl
Base fluorenes, 1- hydroxyl phenanthrene, 2- hydroxyl phenanthrene, 3- hydroxyl phenanthrene, 4- hydroxyl phenanthrene, 9- hydroxyl phenanthrene, 1- hydroxyl pyrene and 6- hydroxyl。
The concentration that singly mark solution object and mixed standard solution further, are prepared in the step 1 is respectively 0.20,
0.40,0.60,0.80,1.00,2.00,5.00,10.00,20.00 and 50.00 μ g/mL.
Further, the singly mark solution need to be saved under the conditions of temperature is 4 DEG C, and period of storage is 1 year.
Compared with prior art the advantage of the invention is that (1) has pretreatment process fast and convenient, detection method is stablized
Property it is good, detection limit is low, accuracy is good；(2) there is good separating effect to the isomer of monohydroxy polycyclic aromatic hydrocarbon；
(3) measurement of 10 kinds of monohydroxy polycyclic aromatic hydrocarbon contents in human urine can be measured simultaneously.
Detailed description of the invention
Fig. 1 is the chromatogram of OH-PAHs monomer in OH-PAHs of embodiment of the present invention mixed standard solution.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, right hereinafter, referring to the drawings and the embodiments,
The present invention is described in further details.
The analyzing detecting method of monohydroxy polycyclic aromatic hydrocarbon, includes the following steps in a kind of urine：
(1) chemical reagent is prepared
1- hydroxyl naphthalene, 2 hydroxy naphthalene, 2- hydroxyphenyl fluorene, 1- hydroxyl are luxuriant and rich with fragrance, 2- hydroxyl is luxuriant and rich with fragrance, 3- hydroxyl is luxuriant and rich with fragrance, 4- hydroxyl is luxuriant and rich with fragrance, 9- hydroxyl
Luxuriant and rich with fragrance, 1- hydroxyl pyrene, 6- hydroxyl, 1- hydroxyl naphthalene-d7,1- hydroxyl pyrene-d9, acetic acid-sodium acetate buffer solution (pH=5,5mol/L).
(2) standard curve is established
10 kinds of monohydroxy polycyclic aromatic hydrocarbon standard solution：Using methanol as solvent, compound concentration is the 1- hydroxyl of 100mg/L respectively
Naphthalene, 2 hydroxy naphthalene, 2- hydroxyphenyl fluorene, 1- hydroxyl are luxuriant and rich with fragrance, 2- hydroxyl is luxuriant and rich with fragrance, 3- hydroxyl is luxuriant and rich with fragrance, 4- hydroxyl is luxuriant and rich with fragrance, 9- hydroxyl is luxuriant and rich with fragrance, 1- hydroxyl pyrene, 6-
HydroxylTotally 10 kinds of Hydroxyl Polycyclic Aromatic standard items singly mark solutions；Distinguishing compound concentration by solvent of methanol in the same way is
The singly mark solution of the 1- hydroxyl naphthalene-d7 of 100mg/L, the deuterated Hydroxyl Polycyclic Aromatic of 1- hydroxyl pyrene-d9；Using methanol as solvent, by table 1
Preparing target concentration is that 0.20,0.40,0.60,0.80,1.00,2.00,5.00,10.00,20.00,50.00 μ g/mL are (interior
Mark concentration is the standard serial solution of 10 μ g/mL), establishes 10 kinds of Hydroxyl Polycyclic Aromatics by liquid chromatography-tandem mass spectrometry method
Standard curve.With 1- hydroxyl naphthalene, 2 hydroxy naphthalene, 2- hydroxyphenyl fluorene, 1- hydroxyl is luxuriant and rich with fragrance, 2- hydroxyl is luxuriant and rich with fragrance, 3- hydroxyl is luxuriant and rich with fragrance, 4- hydroxyl is luxuriant and rich with fragrance,
Peak area (the A of 9- hydroxyl phenanthrene quota ioni) with the peak area (A of 1- hydroxyl naphthalene-d7is) ratio be ordinate, with 1- hydroxyl
Naphthalene, 2 hydroxy naphthalene, 2- hydroxyphenyl fluorene, 1- hydroxyl phenanthrene, 2- hydroxyl phenanthrene, 3- hydroxyl phenanthrene, 4- hydroxyl phenanthrene, 9- hydroxyl phenanthrene and 1- hydroxyl naphthalene-
D7 concentration ratio is that abscissa carries out linear regression, obtains 1- hydroxyl naphthalene, 2 hydroxy naphthalene, 2- hydroxyphenyl fluorene, 1- hydroxyl phenanthrene, 2- hydroxyl
Phenanthrene, 3- hydroxyl are luxuriant and rich with fragrance, 4- hydroxyl is luxuriant and rich with fragrance, linear equation and related coefficient of 9- hydroxyl phenanthrene；With 1- hydroxyl pyrene, 6- hydroxylQuota ion
Peak area (Ai) with the peak area (A of 1- hydroxyl pyrene-d9is) ratio be ordinate, with 1- hydroxyl pyrene, 6- hydroxylWith 1- hydroxyl
Base pyrene-d9 concentration ratio is that abscissa carries out linear regression, obtains 1- hydroxyl pyrene, 6- hydroxylLinear equation and related coefficient,
See Table 2 for details.
The preparation of 1 10 kinds of OH-PAHs hybrid standard liquids of table
Using methanol as solvent, preparation obtains 10 kinds of different concentration gradients of Hydroxyl Polycyclic Aromatic (totally 10 test points), draws
Standard curve processed simultaneously calculates its range of linearity, as linear coefficient (R2)>When 0.999, show linearly preferably, can thus be quantified
It calculates.
2 Hydroxyl Polycyclic Aromatic linear equation of table and related coefficient
(3) sample treatment
Urine is thawed at room temperature, 2mL urine sample is accurately pipetted after urine dissolution and is added in 10mL tool plug centrifuge tube, and
3mL acetic acid-sodium acetate buffer solution is added in centrifuge tube, accurately pipettes 10 μ L beta-glucosidase acid/aryl respectively later
Sulfuric acid lipase and mixing internal standard solution be added centrifuge tube in, with turbula shaker be uniformly mixed, by centrifuge tube corking it is good after be put into perseverance
37 DEG C of water-bath 12h of tepidarium oscillator take out after water-bath 12h and prepared SPE pillar.CNWBOND HC-C18 pillar is attached to
On 12 hole solid-phase extraction devices, taking 5mL methanol to be added in CNWBOND HC-C18 solid phase extraction column activates it sufficiently, then
5mL ultrapure water, which is added, makes its balance, and keeps sample with the rate of 1mL/min not entirely through preceding addition sample in ultrapure water
Pass through.After sample passes through SPE pillar completely, 4ml ultrapure water is added and elutes extraction column, after leacheate is by extraction column,
1min is kept under vacuum condition, the moisture in SPE pillar is sufficiently removed, then elute pillar with the methanol of 10mL, collects eluent
Into test tube, nitrogen is blown to close dry, after mixing with turbula shaker crosses 0.2 μm of organic filter membrane in aperture with methanol constant volume to 1mL
Syringe needle filter filter into brown sample bottle, cryo-conservation, wait sample introduction.
(4) LC-MS testing conditions
Liquid phase chromatogram condition：The present invention uses reverse chromatograms column ZORBAX SB-C18 (250mm × 4.6mm, 5 μm) chromatography
Column separates target compound, as shown in Figure 1, mobile phase is pure methanol and ultrapure water；Gradient elution：Gradient：0-
13min, 60% methanol；14-20min, 78% methanol；21-29min, 85% methanol；30-38min, 100% methanol；39-
45min, 60% methanol；The elution program of flow velocity 0.6mL/min, 10 μ L of sampling volume；Column temperature：30℃.
Mass Spectrometry Conditions：Electrospray ionisation source negative ion mode (ESI-)；Multiple-reaction monitoring pattern (MRM) scanning；Collision gas
(CAD)：10psi；Gas curtain gas (CUR)：25psi；Atomization gas (GS1)：40psi；It heats gas (GS2)：45psi；Spray voltage：-
4500V；Desolvation temperature (TEM)：450℃.Sweep time：300ms.More reactive ion detection pattern (MRM) detections；Entrance
Voltage (EP)：- 10V, exit potential (CXP)：- 15V, each the retention time of the compound, MRM ion pair, broken voltage, impact energy
Amount is shown in Table 3.
The MRM parameter of 3 10 kinds of OH-PAHs of table
Respective standard product are separately added into urine sample by following spiked levels, after sample pre-treatments extracting and enriching,
Calculate the recovery of standard addition of respective objects object.
(5) influence of the different leacheates to the mark-on compound rate of recovery
Since the background of urine is more complicated, in order to utmostly remove the impurity in C18 extraction pillar, targeted is reduced
The loss of object is closed, so increasing rinsing step after urine is enriched with by C18 solid phase extraction column.In relatively 4mL ultrapure water
After the elution effect of 30% methanol, discovery is eluted using 30% methanol will cause object heavy losses, and ultrapure water
Cleaning effect is preferable.
(6) measurement of matrix recovery of standard addition and accuracy
The veracity and precision of target compound is measured using matrix plus calibration method, takes 12 parts of urines in an experiment
Parallel sample, is divided into 3 groups, every group of hybrid standard liquid for taking 3 parallel samples to be separately added into 3 concentration, makes its concentration be respectively
5.00,3 Duplicate Samples, 1 blank control is arranged in 10.00,40.00 μ g/mL, each concentration.According to above-mentioned detection method into
Row measurement, calculates the rate of recovery and relative standard deviation (RSD).As shown in table 4, the rate of recovery of this method is 61.80-
148.80%, relative standard deviation (RSD, n=9) is 0.79-14.85%, it was demonstrated that this method has preferable repeatability and standard
True property.
4 Hydroxyl Polycyclic Aromatic matrix recovery of standard addition (n=9) of table
(7) actual sample detection (example)
10 parts of practical urine samples are taken, 2mL urine sample is accurately pipetted after thawing at room temperature and is added in 10mL tool plug centrifuge tube, and
3mL sodium acetate buffer is added in centrifuge tube, accurately pipettes 10 μ L beta-glucosidase acid/aryl sulphatase respectively later
With mixing internal standard solution be added centrifuge tube in, with turbula shaker be uniformly mixed, by centrifuge tube corking it is good after be put into water bath with thermostatic control shake
37 DEG C of water-bath 12h of device are swung, is taken out after water-bath 12h and prepared SPE pillar.CNWBOND HC-C18 pillar is attached to 12 holes to consolidate
On phase extraction equipment, taking 5mL methanol to be added in CNWBOND HC-C18 solid phase extraction column activates it sufficiently, adds 5mL
Ultrapure water makes its balance, and keeps sample to pass through with the rate of 1mL/min not entirely through preceding addition sample in ultrapure water.To
After the complete SPE pillar excessively of sample, extraction column is eluted 4mL ultrapure water is added, after leacheate is by extraction column, in vacuum condition
Lower holding 1min sufficiently removes the moisture in SPE pillar, then elutes pillar with the methanol of 10mL, collects eluent into test tube
Nitrogen, which is blown to, closely to be done, and after mixing with turbula shaker crosses the syringe needle filter of 0.2 μm of organic filter membrane in aperture with methanol constant volume to 1mL
Device is filtered into brown sample bottle, sample detection, it is found that 10 kinds of monohydroxy polycyclic aromatic hydrocarbons have detection in practical urine sample, dense
Spending range is respectively 1- hydroxyl naphthalene (0.607-6.834 μ g/L), 2 hydroxy naphthalene (0.863-17.086 μ g/L), 2- hydroxyphenyl fluorene
(0.454-2.914 μ g/L), 1+9- hydroxyl phenanthrene (0.169-0.888 μ g/L), 2- hydroxyl phenanthrene (0.116-0.656 μ g/L), 3- hydroxyl
Ji Fei (0.112-1.176 μ g/L), 4- hydroxyl phenanthrene (0.087-0.117 μ g/L), 1- hydroxyl pyrene (0.102-0.931 μ g/L), 6-
Hydroxyl(0.132-2.983 μ g/L), see Table 5 for details.
The contents level (μ g/L) of OH-PAHs in certain the city dweller's urine of table 5
Those of ordinary skill in the art will understand that the embodiments described herein, which is to help reader, understands this hair
Bright implementation method, it should be understood that protection scope of the present invention is not limited to such specific embodiments and embodiments.Ability
The those of ordinary skill in domain disclosed the technical disclosures can make its various for not departing from essence of the invention according to the present invention
Its various specific variations and combinations, these variations and combinations are still within the scope of the present invention.
Claims (4)
1. the analyzing detecting method of monohydroxy polycyclic aromatic hydrocarbon in a kind of urine, which is characterized in that include the following steps：
Step 1, prepare the singly mark solution of 10 kinds of monohydroxy polycyclic aromatic hydrocarbon standard items, then take appropriate 10 kinds of singly mark solutions be made into containing
The mixed standard solution of various monohydroxy polycyclic aromatic hydrocarbons and mixing inner mark solution containing 2 kinds of deuterated Hydroxyl Polycyclic Aromatics；Pass through
Liquid chromatography-tandem mass spectrometry method establishes the standard curve of 10 kinds of monohydroxy polycyclic aromatic hydrocarbons；
Step 2, urine sample is thawed at room temperature, after urine defrosting after accurately pipette 2.00mL urine sample be added 10mL tool plug from
In heart pipe, and 3mL acetic acid-sodium acetate buffer solution is added in centrifuge tube, accurately pipette 10 μ L β-glucose respectively later
Thuja acid/aryl sulphatase and mixing internal standard solution are added in centrifuge tube, are uniformly mixed with turbula shaker, and centrifuge tube corking is good
After be put into 37 DEG C of water-bath 12h of thermostatic control oscillator vibration, after water-bath 12h take out prepared Solid Phase Extraction (SPE) pillar；
Step 3, SPE pillar is attached on 12 hole solid-phase extraction devices, taking 5mL methanol to be added in SPE pillar keeps it sufficiently living
Change, adding 5mL ultrapure water makes its balance, and keeps sample with 1mL/min's not entirely through preceding addition sample in ultrapure water
Rate passes through；
Step 4, after sample passes through SPE pillar completely, 4mL ultrapure water is added and elutes extraction column, passes through extraction column to leacheate
Afterwards, 1min is kept under vacuum conditions, sufficiently removes the moisture in SPE pillar, then elute pillar with the methanol of 10mL, collection is washed
De- liquid is into test tube, and then nitrogen is blown to close dry, with methanol constant volume to 1mL, after mixing with turbula shaker, crosses 0.2 μm of hole
The syringe needle filter of the organic filter membrane of diameter is filtered into brown sample bottle, to sample introduction；
Step 5, it after obtaining a result, is drawn according to the inner mark solution concentration in above-mentioned steps 1 by the standard serial solution of 10 μ g/mL
It is horizontal that 10 kinds of monohydroxy polycyclic aromatic hydrocarbon contents in sample are found on the standard curve of system.
2. according to the method described in claim 1, it is characterized in that：10 kinds of monohydroxy polycyclic aromatic hydrocarbon standard items in the step 1
For 1- hydroxyl naphthalene, 2 hydroxy naphthalene, 2- hydroxyphenyl fluorene, 1- hydroxyl is luxuriant and rich with fragrance, 2- hydroxyl is luxuriant and rich with fragrance, 3- hydroxyl is luxuriant and rich with fragrance, 4- hydroxyl is luxuriant and rich with fragrance, 9- hydroxyl is luxuriant and rich with fragrance, 1-
Hydroxyl pyrene and 6- hydroxyl
3. according to the method described in claim 2, it is characterized in that：Singly mark solution is prepared in the step 1 and hybrid standard is molten
The concentration of liquid is respectively 0.20,0.40,0.60,0.80,1.00,2.00,5.00,10.00,20.00 and 50.00 μ g/mL.
4. according to the method described in claim 1, it is characterized in that：The singly mark solution need to carry out under the conditions of temperature is 4 DEG C
It saves, period of storage is 1 year.
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| CN110441427A (en) * | 2019-08-19 | 2019-11-12 | 生态环境部华南环境科学研究所 | Based on the method for not being metabolized polycyclic aromatic hydrocarbon in cryogenic freezing abstraction technique detection urine |
| CN110441427B (en) * | 2019-08-19 | 2022-02-08 | 生态环境部华南环境科学研究所 | Method for detecting unmetabolized polycyclic aromatic hydrocarbons in urine based on low-temperature freezing extraction technology |
| CN111057055A (en) * | 2019-12-10 | 2020-04-24 | 曲阜师范大学 | Multichannel mass spectrum derivatization reagent for detecting hydroxyl polycyclic aromatic hydrocarbon, and preparation method and application thereof |
| CN111057055B (en) * | 2019-12-10 | 2022-03-25 | 曲阜师范大学 | Multichannel mass spectrum derivatization reagent for detecting hydroxyl polycyclic aromatic hydrocarbon, and preparation method and application thereof |
| CN111337590A (en) * | 2020-03-20 | 2020-06-26 | 中国辐射防护研究院 | Method for simultaneously measuring 8 polycyclic aromatic hydrocarbon hydroxyl metabolites in urine |
| CN111983053A (en) * | 2020-07-23 | 2020-11-24 | 广东工业大学 | Solid phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for online determination of hydroxyl polycyclic aromatic hydrocarbons in urine |
| CN111983053B (en) * | 2020-07-23 | 2022-08-02 | 广东工业大学 | Solid phase extraction-liquid chromatography triple quadrupole mass spectrometry isotope dilution method for online determination of hydroxyl polycyclic aromatic hydrocarbons in urine |
| CN114563502A (en) * | 2022-03-08 | 2022-05-31 | 广东工业大学 | Method for synchronously and quantitatively determining concentrations of various aromatic compounds and metabolites in urine |
| CN116754348A (en) * | 2023-06-06 | 2023-09-15 | 华北理工大学 | ZIF-8-90 material-based effervescent tablet, preparation method and application thereof |
| CN116754348B (en) * | 2023-06-06 | 2024-03-08 | 华北理工大学 | ZIF-8-90 material-based effervescent tablet, preparation method and application thereof |
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