CN110161165A - It is a kind of while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair - Google Patents
It is a kind of while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair Download PDFInfo
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- CN110161165A CN110161165A CN201910412315.XA CN201910412315A CN110161165A CN 110161165 A CN110161165 A CN 110161165A CN 201910412315 A CN201910412315 A CN 201910412315A CN 110161165 A CN110161165 A CN 110161165A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
The analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair is detected simultaneously the invention discloses a kind of, this method is to clean Hair grooming acetone to obtain exogenous extract liquor, hair after cleaning is cleared up under the conditions of 40~80 DEG C, obtains endogenous extract liquor；Gel permeation chromatography column purification will be used respectively after the concentration of exogenous and endogenous extract liquor, is eluted with eluent, collect leacheate；It is separated and is purified after leacheate is concentrated, first is eluted with the hexane solution of the polar solvent containing 2~5% and collected component 1, it is eluted followed in turn by the hexane solution containing 30~60% polar solvents and collects component 2, elution liquid nitrogen blows constant volume, by data processing and quantitative calculating, the contents level of object in hair is obtained.The present invention detects while realization to external sources a variety of in human hair and endogenous polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content, provides effective Method means for the Human body package health risk assessment of polycyclic aromatic hydrocarbon.
Description
Technical field
The invention belongs to organic pollutant analysis technical fields, detect simultaneously more particularly, to one kind polycyclic in hair
The analysis method of aromatic hydrocarbons (PAHs) and its Metabolism of hydroxyl content (OH-PAHs).
Background technique
Polycyclic aromatic hydrocarbon (Polycyclic Aromatic Hydrocarbons, PAHs) is that two and multiple aromatic ring fusions exist
A kind of compound being formed together, it is prevalent in natural environment.PAHs mostlys come from the incomplete of hydrocarbon
Burning, hitherto it is found that PAHs homologue up to more than 200, it is most of that there is persistence and strong carcinogenic, teratogenesis, mutagenesis
Property, there is biggish threat to ecological environment and human health.Wherein there are 16 kinds of PAHs to be classified as priority acccess control by Environmental Protection Agency
7 kinds of PAHs are also included in priority monitoring list by pollutant, China.
PAHs The book of Changes crosses atmosphere breathing, skin exposure and diet approach and enters human body, and in the effect of human hepatocyte's enzyme
Under, it is discharged after forming a series of hydroxy metabolite products through urine.Therefore, generally pass through the content of OH-PAHs metabolin in urine
To assess the exposure level of human body PAHs.But the OH-PAHs due to PAHs in the intracorporal half-life short of people (< 2 days), urine
Concentration can only reflect the exposure of the short-term PAHs of human body.In comparison, hair is as a kind of emerging lossless biological monitoring
Sample, have the characteristics that it is low in cost, be easy to acquire, facilitate storage and transport, and can reflect that pollutant is short-term in human body
With long-term exposure.Therefore powerful of the hair as a kind of lossless biological monitoring of human body, has been widely applied to
The exposure monitoring of human body heavy metal lead, cadmium, mercury and organic pollution.
Currently, having the analysis method of PAHs in document report hair, also there is a small amount of research to the OH-PAHs in hair
Level of pollution is analyzed, and has also been researched and analysed mouse and has been fed 52 kinds of OH-PAHs metabolins after poison in hair, these are existing
The analysis method of OH-PAHs is all based on the gas chromatography mass spectrometry of derivatization, and method flow is long and time-consuming and laborious.Another party
Face can not carry out simultaneously them using under same instrument condition because of the difference in PAHs and OH-PAHs physicochemical property
It tests and analyzes.That is there is presently no suitable methods PAHs in human hair and OH-PAHs can be carried out while be detected.
In addition, the PAHs in hair may be from the infiltration of the dust and particulate matter adsorbed on hair, it is also possible to from PAHs in people
Intracorporal tissue metabolism's distribution, and OH-PAHs is then mainly derived from metabolite in the intracorporal migration of people, therefore, by simultaneously
Detecting PAHs and OH-PAHs accurately can carry out clear definition to the sources discrimination of PAHs and exposed features.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, it is an object of that present invention to provide a kind of detectors simultaneously
The analysis method of polycyclic aromatic hydrocarbon (PAHs) and its Metabolism of hydroxyl content (OH-PAHs) level in hair.
The purpose of the present invention is realized by following technical proposals:
It is a kind of while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair, including following specific step
It is rapid:
S1. it takes hair sample that acetone soln ultrasonic cleaning is added, obtains exogenous extract liquor；Hair after cleaning passes through alkali
Property digestion solution cleared up under 40~80 DEG C of water bath conditions, gained digestion solution n-hexane and t-butyl methyl ether mixed solution extraction
It takes, is centrifugated and collects supernatant, obtain endogenous extract liquor；
S2. gel permeation chromatography column purification will be used respectively after the concentration of exogenous and endogenous extract liquor, with eluent just oneself
Alkane and methylene chloride mixed solution are eluted, and leacheate is collected；
S3. will be transferred to silica gel solid phase extraction column after the leacheate concentration after collection and separated and purified, with containing 2~
The hexane solution of 5% polar solvent elutes and collects component 1, is then washed with the hexane solution containing 30~60% polar solvents
It takes off and collects component 2；
S4. nitrogen blows constant volume to eluent respectively: internal standard compound is added in component 1, constant volume is in isooctane, with gas-chromatography-series connection
Mass spectrum quantifies the PAHs in component 1；By 2 constant volume of component in methanol, using liquid chromatography-tandem mass spectrometry isotopic dilution
Method analyzes OH-PAHs, by data processing and quantitative calculating, obtains the contents level of object in hair.
Preferably, the quality of hair sample described in step S1 and the volume ratio of acetone soln be (0.2~1) g:(5~
20)mL。
Preferably, alkalinity digestion solution described in step S1 is sodium hydroxide solution or potassium hydroxide solution.
It is further preferable that the concentration of the alkalinity digestion solution is 0.5~1.5mol/L.
Preferably, the time of resolution described in step S1 is 2~12h.
Preferably, the revolving speed of centrifugation described in step S1 is 1500~3500rpm.
Preferably, the volume ratio of n-hexane described in step S2 and methylene chloride is (3~7): (4~6), the eluent
Elution speed be 2~5mL/min.
Preferably, the quality of the amount of filler in silica gel solid phase extraction column described in step S3 and volumetric ratio be (60~
1000) mg:(3~6) mL；The polar solvent is one or more of methylene chloride, acetone or ethyl acetate, the elution
Elution speed is 1~2mL/min.
Preferably, the test condition of gas chromatography tandem mass spectrometry described in step S4 are as follows: GC conditions are not shunt
1~2 μ L of sample introduction, injector temperature are 250~280 DEG C, and transmission line temperature is 300 DEG C, high-purity helium 1~1.5mL/min of flow velocity,
Temperature program is 80 DEG C of reservation 1min, 10 DEG C/min to 200 DEG C, 2 DEG C/min to 260 DEG C, 10 DEG C/min to 300 DEG C, is retained
10min, it is 5% phenyl-methyl polysiloxanes capillary column that chromatographic column, which is specification, the size of the capillary column be 30m ×
0.25mm × 0.25 μm, the temperature in electron impact ionization source are 230 DEG C.
Preferably, the test condition of liquid chromatography-tandem mass spectrometry isotope-dilution analysis described in step S4 are as follows: liquid phase used
Chromatogram flow phase is to add the ultrapure water and methanol of 0.1% acetic acid, and flow velocity is 0.2~0.4mL/min, 30~40 DEG C of column temperature, terraced
Degree elution program starts as 50% methanol, and 90% methanol is risen in 15min, retains 5min；It is less than or equal to 2.7 μm using partial size
C18 reverse-phase chromatography post separation OH-PAHs, ion source is ESI negative mode, and nitrogen temperature is 300~350 DEG C in ion source, stream
Speed is 4~6L/min, and sheath temperature degree is 300~350 DEG C, and flow velocity is 10~12L/min, and capillary voltage is 3000~4000V.
Compared with prior art, the invention has the following advantages:
1. the primary analysis of prototype PAHs and its metabolin can be carried out this invention simplifies sample pre-treatments step, contract
The time required to short sample analysis.The OH-PAHs in hair is analyzed by liquid chromatography-tandem mass spectrometry, without cumbersome
And time-consuming derivatization treatment.It is quantified by Internal standard, reduces possible matrix interference, improved quantitative
Accuracy.
2. multi-component separation strategy of the present invention may be implemented in hair PAHs and the OH-PAHs same time-division
Analysis, avoiding PAHs and OH-PAHs, respectively individually processing causes the error of result between batch, while significantly improving sample
Analysis efficiency.
3. the present invention takes nondestructive sample pre-treatments means, method compatibility is strong.It is tested carrying out method applicability
After card, the sample of retention is used equally for the analysis of the similar arene compounds of structure and its hydroxy metabolite product.
4. detection method of the invention may be implemented to external sources a variety of in human hair and endogenous polycyclic aromatic hydrocarbon and its hydroxyl
It is detected while metabolin, provides effective Method means for the Human body package health risk assessment of polycyclic aromatic hydrocarbon.
Detailed description of the invention
Fig. 1 is the total ion of liquid chromatography-tandem mass spectrometry of OH-PAHs and its corresponding Isotopic Internal Standard object in embodiment 1
Flow graph.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Embodiment 1
The present embodiment hair sample picks up from certain electronic waste dismantling area's occupational exposure dismantling worker and neighbouring non-professional exposure
Resident.All samples are tightly wrapped up with aluminium foil, and hermetic bag sealing is placed in -20 DEG C of preservations.
1. taking 1g hair sample, 20mL acetone is added and is cleaned by ultrasonic 1 minute, obtains exogenous extract liquor；Head after cleaning
Hair dries, and shreds to about 1mm, is placed in 50mLTeflon centrifuge tube, and PAHs rate of recovery indicant Nap-d is added8、Ace-
d10、Phe-d10、Chr-d12、Pery-d12And OH-PAHs Isotopic Internal Standard 2-OH-Nap-d7、2-OH-Flu-d9、1-OH-
Pyr-d9、13C12Then 5mL 1M NaOH is added in -3-OH-Phe in the hair dried, it is small that 12 are cleared up in 40 DEG C of water-baths
When, obtain alkaline digestion solution；Afterwards with n-hexane/t-butyl methyl ether mixed solution extraction, endogenous extract liquor is obtained；
2. using gel permeation chromatography column purification respectively after extract liquor concentration, eluted with n-hexane/methylene chloride mixed solution,
Collect 65-165mL leacheate；
Silica gel solid phase extraction column (CNW BOND Si silica gel is transferred to 3. the leacheate after collection is concentrated into after 1mL
SPE pillar 1g/6mL) double purification and the separation of middle polarity are carried out, it is eluted with the n-hexane containing 5% ethyl acetate and collects 10mL
PAHs (component 1) is then eluted with the n-hexane containing 50% ethyl acetate and is collected 8mL OH-PAHs (component 2)；
4. nitrogen blows constant volume to eluent respectively.Internal standard compound is added in component 1, and constant volume is in 50 μ L isooctane, with gas-chromatography-series connection
Mass spectrum (GC-MS/MS) quantifies the PAHs in component 1；2 constant volume of component is in 200 μ L methanol, using liquid chromatography-tandem
Mass spectrum (LC-MS/MS) isotope-dilution analysis analyzes OH-PAHs.By data processing and quantitative calculating, obtain in hair
The contents level of object.
The model Shimadzu GC-MS TQ8040 series of gas chromatography tandem mass spectrometry (GC-MS/MS), gas-chromatography
Condition is 1 μ L of Splitless injecting samples, and injector temperature is 280 DEG C, and transmission line temperature is 300 DEG C, high-purity helium flow velocity 1mL/min,
Temperature program is 80 DEG C of reservation 1min, 10 DEG C/min to 200 DEG C, 2 DEG C/min to 260 DEG C, 10 DEG C/min to 300 DEG C, is retained
10min, chromatographic column are DB-5MS (30m × 0.25mm × 0.25 μm).Electron bombardment (EI) ionization source, ion source temperature 230
DEG C, other mass spectrometry parameters, such as ion pair, impact energy and retention time, with shown in table 1.
The model Agilent 1260-6470 series of liquid chromatography-tandem mass spectrometry (LC-MS/MS), liquid chromatogram used
Mobile phase is to add the ultrapure water and methanol of 0.1% acetic acid, and flow velocity 0.4mL/min, 40 DEG C of column temperature, gradient elution program starts
For 50% methanol, 90% methanol is risen in 15min, retains 5min；Using Poroshell 120EC-C18 (4.6mm × 100mm,
2.7 μm) reverse-phase chromatography post separation OH-PAHs, ion source is AJS ESI negative mode, and nitrogen temperature is 300 DEG C in ion source, stream
Speed be 5L/min, sheath temperature degree be 300 DEG C, flow velocity 12L/min, capillary voltage 3500V, other mass spectrometry parameters, such as from
Son is to, impact energy and retention time, with shown in table 2.
Fig. 1 is the liquid chromatography-tandem mass spectrometry appearance time of OH-PAHs and its corresponding Isotopic Internal Standard object.From Fig. 1
It is found that other OH-PAHs objects have obtained baseline separation other than 1/9-OH-Phe and 2/3-OH-Phe.
Embodiment 2
The method of the foundation can be applied to occupational exposure population and non-exposed resident hair is exogenous and endogenous
PAHs and OH-PAHs is detected.In addition to individual external source OH-PAHs, the recall rate of PAHs and OH-PAHs is in external source in hair
100%.The average total concentration of non-exposed 16 kinds of PAHs of resident's hair external source is 116ng/g hair dry weight, and endogenous concentration is
164ng/g；The average total concentration of 16 kinds of PAHs of Exposure hair external source is 111ng/g, endogenous concentration 292ng/g；Wherein
Phe, Fluo, Pyr and Chr are main component.This 4 kinds of PAHs in the distribution of interior external source be it is discrepant, endogenous is Phe
27.5% > Pyr, 20% > Fluo, 19.5% > Chr 8.5%, external source be 21.5% > Fluo of Pyr, 20.5% > Phe 15% >
Chr 11.5%.
On the other hand, average total concentration of the OH-PAHs in non-exposed resident's hair external source is 10ng/g, and endogenous concentration is
171ng/g；The average total concentration of Exposure hair external source OH-PAHs is 9ng/g, endogenous concentration 178ng/g.Endogenous OH-
PAHs accounts for the 71% and 81% of worker and resident's hair OH-PAHs total concentration using OH-Nap as main component respectively.Inside and outside hair
The huge concentration difference of OH-PAHs shows the unique of validity that PAHs Metabolism of hydroxyl content accumulates in hair and source in source
Property.On the other hand accumulation of the metabolin in hair is disclosed, therefore, this method proves that hair can be used as assessment human body
The ideal sample of PAHs exposure for a long time.
The gas chromatography tandem mass spectrometry parameter that PAHs is analyzed in 1 hair of table
The liquid chromatography-tandem mass spectrometry parameter that OH-PAHs is analyzed in 2 hair of table
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of detect the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair simultaneously, which is characterized in that including
Following specific steps:
S1. it takes hair sample that acetone soln ultrasonic cleaning is added, obtains exogenous extract liquor；Hair after cleaning disappears through parlkaline
Solution liquid is cleared up under 40~80 DEG C of water bath conditions, gained digestion solution n-hexane and the extraction of t-butyl methyl ether mixed solution,
It is centrifugated and is collected supernatant, obtains endogenous extract liquor；
S2. gel permeation chromatography column purification will be used respectively after the concentration of exogenous and endogenous extract liquor, with eluent n-hexane and
Methylene chloride mixed solution is eluted, and leacheate is collected；
S3. will be transferred to silica gel solid phase extraction column after the leacheate concentration after collection and separated and purified, first with containing 2~
The hexane solution of 5% polar solvent elutes and collects component 1, molten followed in turn by the n-hexane containing 30~60% polar solvents
Liquid elutes and collects component 2.
S4. nitrogen blows constant volume to eluent respectively: internal standard compound is added in component 1, constant volume uses gas chromatography tandem mass spectrometry in isooctane
PAHs in component 1 is quantified；By 2 constant volume of component in methanol, using liquid chromatography-tandem mass spectrometry isotope-dilution analysis pair
OH-PAHs is analyzed, and by data processing and quantitative calculating, obtains the contents level of object in hair.
2. it is according to claim 1 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, the quality of hair sample described in step S1 and the volume ratio of acetone soln are (0.2~1) g:(5~20) mL.
3. it is according to claim 1 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, alkalinity digestion solution described in step S1 is sodium hydroxide solution or potassium hydroxide solution.
4. it is according to claim 3 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, the concentration of the alkalinity digestion solution is 0.5~1.5mol/L.
5. it is according to claim 1 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, the time of resolution described in step S1 is 2~12h.
6. it is according to claim 1 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, the revolving speed of centrifugation described in step S1 is 1500~3500rpm.
7. it is according to claim 1 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, the volume ratio of n-hexane described in step S2 and methylene chloride is (3~7): (4~6), the leaching of the eluent
Washing speed is 2~5mL/min.
8. it is according to claim 1 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, the quality and volumetric ratio of the amount of filler in silica gel solid phase extraction column described in step S3 are (60~1000)
Mg:(3~6) mL；The polar solvent is one or more of methylene chloride, acetone or ethyl acetate, the elution of the elution
Speed is 1~2mL/min.
9. it is according to claim 1 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, the test condition of gas chromatography tandem mass spectrometry described in step S4 are as follows: GC conditions are Splitless injecting samples
1~2 μ L, injector temperature are 250~280 DEG C, and transmission line temperature is 300 DEG C, high-purity helium 1~1.5mL/min of flow velocity, heating
Program is 80 DEG C of reservation 1min, 10 DEG C/min to 200 DEG C, 2 DEG C/min to 260 DEG C, 10 DEG C/min to 300 DEG C, retains 10min,
It is 5% phenyl-methyl polysiloxanes capillary column that chromatographic column, which is specification, the size of the capillary column be 30m × 0.25mm ×
0.25 μm, the temperature in electron impact ionization source is 230 DEG C.
10. it is according to claim 1 while detecting the analysis method of polycyclic aromatic hydrocarbon and its Metabolism of hydroxyl content level in hair,
It is characterized in that, the test condition of liquid chromatography-tandem mass spectrometry isotope-dilution analysis described in step S4 are as follows: liquid chromatogram used
Mobile phase is to add the ultrapure water and methanol of 0.1% acetic acid, and flow velocity is 0.2~0.4mL/min, and 30~40 DEG C of column temperature, gradient is washed
De- program starts as 50% methanol, and 90% methanol is risen in 15min, retains 5min；Using partial size less than or equal to 2.7 μm
C18 reverse-phase chromatography post separation OH-PAHs, ion source are ESI negative mode, and nitrogen temperature is 300~350 DEG C in ion source, flow velocity
For 4~6L/min, sheath temperature degree is 300~350 DEG C, and flow velocity is 10~12L/min, and capillary voltage is 3000~4000V.
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| 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 |
| 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 |
| CN113960220A (en) * | 2021-12-15 | 2022-01-21 | 生态环境部华南环境科学研究所 | Synchronous detection method and application of polycyclic aromatic hydrocarbon and derivatives thereof in blood |
| CN113960220B (en) * | 2021-12-15 | 2022-03-04 | 生态环境部华南环境科学研究所 | Synchronous detection method and application of polycyclic aromatic hydrocarbon and derivatives thereof in blood |
| CN115032296A (en) * | 2022-05-25 | 2022-09-09 | 广东工业大学 | Method for measuring polycyclic aromatic hydrocarbon derivatives in surface water suspended matters |
| CN114965797B (en) * | 2022-06-22 | 2023-08-08 | 广东工业大学 | Rapid detection method for 24 polycyclic aromatic hydrocarbons in complex cooked food matrix |
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