CN110161165B - Analysis method for simultaneously detecting levels of polycyclic aromatic hydrocarbon and hydroxyl metabolites thereof in hair - Google Patents
Analysis method for simultaneously detecting levels of polycyclic aromatic hydrocarbon and hydroxyl metabolites thereof in hair Download PDFInfo
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Abstract
The invention discloses an analysis method for simultaneously detecting the levels of polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in hair, which comprises the steps of cleaning the hair with acetone to obtain exogenous extract liquor, and digesting the cleaned hair at 40-80 ℃ to obtain endogenous extract liquor; concentrating the exogenous and endogenous extractive solutions, purifying with gel permeation chromatography column, eluting with eluent, and collecting eluate; concentrating the leacheate, separating and purifying, eluting with a normal hexane solution containing 2-5% of a polar solvent, collecting the component 1, eluting with a normal hexane solution containing 30-60% of a polar solvent, collecting the component 2, blowing the elution liquid nitrogen to a constant volume, and performing data processing and quantitative calculation to obtain the content level of the target substance in the hair. The invention realizes the simultaneous detection of various exogenous and endogenous polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in human hair, and provides an effective method for human exposure health risk assessment of polycyclic aromatic hydrocarbons.
Description
Technical Field
The invention belongs to the technical field of organic pollutant analysis, and particularly relates to an analysis method for simultaneously detecting Polycyclic Aromatic Hydrocarbons (PAHs) and hydroxyl metabolites (OH-PAHs) thereof in hair.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) are compounds formed by fusing two or more Aromatic rings together, and are ubiquitous in the natural environment. PAHs mainly come from incomplete combustion of hydrocarbon, and the PAHs homologues as many as more than 200 species have been found so far, most of which have persistence and strong carcinogenicity, teratogenicity and mutagenicity and have great threat to the ecological environment and human health. Among them, 16 PAHs are listed as the priority control pollutants by the United states environmental protection agency, and 7 PAHs are also listed as the priority monitoring list in China.
PAHs easily enter human body through atmospheric respiration, skin exposure and dietary approaches, and form a series of hydroxyl metabolites under the action of human liver cell enzymes, and then are discharged through urine. Thus, the exposure level of human PAHs is generally assessed by the content of OH-PAHs metabolites in urine. However, due to the short half-life of PAHs in humans (<2 days), the concentration of OH-PAHs in urine reflects only short-term exposure of PAHs in humans. In comparison, the hair is used as a novel nondestructive biological monitoring material, has the characteristics of low cost, easiness in collection, convenience in storage and transportation and the like, and can reflect short-term and long-term exposure conditions of pollutants in a human body. Therefore, the hair is used as a powerful tool for nondestructive biological monitoring of human bodies, and has been widely applied to exposure monitoring of heavy metal lead, cadmium, mercury and organic matter pollution of human bodies.
At present, the existing literature reports analysis methods of PAHs in hair, few studies also analyze the pollution level of OH-PAHs in hair, and 52 OH-PAHs metabolites in hair after mice are fed with poison, and the existing analysis methods of OH-PAHs are all based on derivatization gas chromatography-mass spectrometry, and have long process flow and time and labor consumption. On the other hand, due to the difference in physicochemical properties between PAHs and OH-PAHs, they cannot be detected and analyzed simultaneously by the same instrument. That is, there is no suitable method for simultaneously detecting PAHs and OH-PAHs in human hair. In addition, the PAHs in the hair can come from the penetration of dust and particles adsorbed on the hair and the tissue metabolic distribution of the PAHs in the human body, and the OH-PAHs mainly come from the migration of metabolites in the human body, so that the source discrimination and the exposure characteristic of the PAHs can be accurately and clearly defined by simultaneously detecting the PAHs and the OH-PAHs.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide an analysis method for simultaneously detecting the levels of Polycyclic Aromatic Hydrocarbons (PAHs) and hydroxyl metabolites (OH-PAHs) thereof in hair.
The purpose of the invention is realized by the following technical scheme:
an analysis method for simultaneously detecting the levels of polycyclic aromatic hydrocarbon and hydroxyl metabolites thereof in hair comprises the following specific steps:
s1, adding an acetone solution into a hair sample, and ultrasonically cleaning to obtain an exogenous extraction liquid; digesting the cleaned hair by an alkaline digestion solution in a water bath at 40-80 ℃, extracting the digestion solution by using a mixed solution of n-hexane and tert-butyl methyl ether, centrifugally separating, and collecting a supernatant to obtain an endogenous extraction liquid;
s2, concentrating the exogenous and endogenous extraction liquids, purifying the concentrated exogenous and endogenous extraction liquids by using gel permeation chromatography columns respectively, eluting the concentrated exogenous and endogenous extraction liquids by using a mixed solution of eluent n-hexane and dichloromethane, and collecting eluent;
s3, concentrating the collected leacheate, transferring the concentrated leacheate to a silica gel solid phase extraction column for separation and purification, eluting with an n-hexane solution containing 2-5% of a polar solvent, collecting the component 1, and then eluting with an n-hexane solution containing 30-60% of a polar solvent and collecting the component 2;
s4, respectively carrying out nitrogen blowing on the eluent to fix the volume: adding the component 1 into an internal standard substance, fixing the volume in isooctane, and quantifying PAHs in the component 1 by using gas chromatography-tandem mass spectrometry; and (3) fixing the volume of the component 2 in methanol, analyzing OH-PAHs by adopting a liquid chromatography-tandem mass spectrometry isotope dilution method, and obtaining the content level of the target object in the hair through data processing and quantitative calculation.
Preferably, the volume ratio of the mass of the hair sample to the acetone solution in step S1 is (0.2-1) g: (5-20) mL.
Preferably, the alkaline digestion solution in step S1 is a sodium hydroxide solution or a potassium hydroxide solution.
More preferably, the concentration of the alkaline digestion solution is 0.5-1.5 mol/L.
Preferably, the digestion time in the step S1 is 2-12 h.
Preferably, the rotation speed of the centrifugation in the step S1 is 1500-3500 rpm.
Preferably, the volume ratio of the n-hexane to the dichloromethane in the step S2 is (3-7): (4-6), wherein the leaching speed of the eluent is 2-5 mL/min.
Preferably, the mass-to-volume ratio of the amount of the filler in the silica gel solid phase extraction cartridge in step S3 is (60-1000) mg: (3-6) mL; the polar solvent is more than one of dichloromethane, acetone or ethyl acetate, and the elution speed of elution is 1-2 mL/min.
Preferably, the test conditions of the gas chromatography-tandem mass spectrometry in the step S4 are: the gas chromatography conditions comprise that the flow of a non-shunting sample is 1-2 mu L, the temperature of a sample inlet is 250-280 ℃, the temperature of a transmission line is 300 ℃, the flow rate of high-purity helium gas is 1-1.5 mL/min, the temperature rise program is that the temperature is kept for 1min at 80 ℃, 10 ℃/min to 200 ℃, 2 ℃/min to 260 ℃, 10 ℃/min to 300 ℃, the temperature is kept for 10min, a chromatographic column is a 5% phenyl-methyl polysiloxane capillary column, the size of the capillary column is 30m multiplied by 0.25mm multiplied by 0.25 mu m, and the temperature of an electron bombardment ionization source is 230 ℃.
Preferably, the test conditions of the liquid chromatography-tandem mass spectrometry isotope dilution method in step S4 are as follows: the liquid chromatography mobile phase is ultrapure water added with 0.1% acetic acid and methanol, the flow rate is 0.2-0.4 mL/min, the column temperature is 30-40 ℃, the gradient elution procedure is started to be 50% methanol, the methanol is increased to 90% within 15min, and the methanol is kept for 5 min; and (2) separating OH-PAHs by using a C18 reversed phase chromatographic column with the particle size of less than or equal to 2.7 microns, wherein an ion source is in an ESI negative mode, the temperature of nitrogen in the ion source is 300-350 ℃, the flow rate is 4-6L/min, the temperature of sheath gas is 300-350 ℃, the flow rate is 10-12L/min, and the capillary voltage is 3000-4000V.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention simplifies the sample pretreatment steps, can carry out one-time analysis on the prototype PAHs and the metabolites thereof, and shortens the time required by sample analysis. OH-PAHs in the hair are analyzed by liquid chromatography-tandem mass spectrometry without cumbersome and time-consuming derivatization treatment. The method has the advantages that the quantification is carried out by an isotope internal standard method, the possible matrix interference is reduced, and the quantification accuracy is improved.
2. The multi-component separation strategy adopted by the invention can realize the simultaneous analysis of PAHs and OH-PAHs in hair, avoid the error of results between batches caused by the independent treatment of PAHs and OH-PAHs, and simultaneously remarkably improve the analysis efficiency of samples.
3. The invention adopts a non-destructive sample pretreatment means, and the method has strong compatibility. After the method suitability is verified, the remaining samples can be used for analyzing aromatic compounds with similar structures and hydroxyl metabolites thereof.
4. The detection method can realize the simultaneous detection of various exogenous and endogenous polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in human hair, and provides an effective method for the human exposure health risk assessment of the polycyclic aromatic hydrocarbons.
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FIG. 1 is a total ion flow diagram of liquid chromatography-tandem mass spectrometry of OH-PAHs and their corresponding isotopic internal standards in example 1.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention.
Example 1
The hair sample of the embodiment is collected from professional exposure dismantling workers in an electronic waste dismantling area and nearby non-professional exposure residents. All samples were tightly wrapped with aluminum foil, sealed in a sealed bag and stored at-20 ℃.
1. Taking 1g of hair sample, adding 20mL of acetone, and ultrasonically cleaning for 1 minute to obtain exogenous extraction liquid; air drying the cleaned hair, cutting to about 1mm, placing in a 50ml Leflo centrifuge tube, adding PAHs recovery indicator Nap-d8、Ace-d10、Phe-d10、Chr-d12、Pery-d12And 2-OH-Nap-d as an isotope internal standard of OH-PAHs7、2-OH-Flu-d9、1-OH-Pyr-d9、13C123-OH-Phe, then adding 5mL of 1M NaOH into the air-dried hair, and digesting in a water bath kettle at 40 ℃ for 12 hours to obtain an alkaline digestion solution; then extracting with a mixed solution of n-hexane/tert-butyl methyl ether to obtain endogenous extract liquor;
2. concentrating the extract, purifying with gel permeation chromatography column, eluting with n-hexane/dichloromethane mixed solution, and collecting 65-165mL eluate;
3. concentrating the collected eluate to 1mL, transferring to a silica gel solid phase extraction column (CNW BOND Si silica gel SPE column 1g/6mL) for secondary purification and medium polarity separation, eluting with n-hexane containing 5% ethyl acetate, collecting 10mL PAHs (component 1), eluting with n-hexane containing 50% ethyl acetate, and collecting 8mL OH-PAHs (component 2);
4. the eluent is respectively blown with nitrogen to fix the volume. Adding an internal standard substance into the component 1, fixing the volume in 50 mu L of isooctane, and quantifying PAHs in the component 1 by using gas chromatography-tandem mass spectrometry (GC-MS/MS); component 2 was dissolved in 200. mu.L of methanol and analyzed for OH-PAHs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) isotope dilution. And obtaining the content level of the target object in the hair through data processing and quantitative calculation.
The gas chromatography-tandem mass spectrometry (GC-MS/MS) model is Shimadzu GC-MS TQ8040 series, the gas chromatography conditions are that the sample injection is carried out in a non-flow mode by 1 mu L, the sample injection port temperature is 280 ℃, the transmission line temperature is 300 ℃, the high-purity helium flow rate is 1mL/min, the temperature rise program is that the temperature is kept for 1min at 80 ℃, the temperature is kept for 10min to 200 ℃, the temperature is kept for 2 ℃/min to 260 ℃, the temperature is kept for 10min to 300 ℃, and the chromatographic column is DB-5MS (30m multiplied by 0.25mm multiplied by 0.25 mu m). Electron Impact (EI) ionization source with ion source temperature of 230 ℃, other mass spectral parameters such as ion pair, collision energy and retention time, as shown in table 1.
The model of liquid chromatography-tandem mass spectrometry (LC-MS/MS) is Agilent 1260-6470 series, the mobile phase of the liquid chromatography is ultrapure water added with 0.1% acetic acid and methanol, the flow rate is 0.4mL/min, the column temperature is 40 ℃, the gradient elution program starts to be 50% methanol, the methanol rises to 90% within 15min, and the methanol is kept for 5 min; OH-PAHs were separated using a Poroshell 120EC-C18(4.6 mm. times.100 mm, 2.7 μm) reverse phase chromatography column with the ion source in AJS ESI negative mode, nitrogen temperature in the ion source at 300 deg.C, flow rate at 5L/min, sheath gas temperature at 300 deg.C, flow rate at 12L/min, capillary voltage at 3500V, and other mass spectral parameters such as ion pair, collision energy and retention time, as shown in Table 2.
FIG. 1 shows the liquid chromatography-tandem mass spectrometry peak discharge times of OH-PAHs and their corresponding isotopic internal standard. As can be seen from FIG. 1, in addition to 1/9-OH-Phe and 2/3-OH-Phe, baseline separation of the OH-PAHs targets was obtained.
Example 2
The established method can be applied to the detection of exogenous and endogenous PAHs and OH-PAHs in the hair of occupational exposure workers and unexposed residents. Except for individual exogenous OH-PAHs, the detection rates of the PAHs and the OH-PAHs in the exogenous hair are both 100 percent. The average total concentration of the 16 exogenous PAHs in the non-exposed resident hair is 116ng/g dry hair weight, and the endogenous concentration is 164 ng/g; the average total concentration of the 16 exogenous PAHs in the hair of the exposure worker is 111ng/g, and the endogenous concentration is 292 ng/g; wherein Phe, Fluo, Pyr and Chr are main components. The 4 PAHs are distributed differently between internal and external sources, wherein the internal source is Phe 27.5% > Pyr 20% > Fluo 19.5% > Chr 8.5%, and the external source is Pyr 21.5% > Fluo 20.5% > Phe 15% > Chr 11.5%.
On the other hand, the average total concentration of OH-PAHs in the hair of non-exposed residents is 10ng/g, and the endogenous concentration is 171 ng/g; the average total concentration of exogenous OH-PAHs in the hair of the exposure worker is 9ng/g, and the endogenous concentration is 178 ng/g. The endogenous OH-PAHs take OH-Nap as a main component, and respectively account for 71 percent and 81 percent of the total concentration of the OH-PAHs of workers and residents. The large concentration differences of OH-PAHs in the hair at the external sources indicate the effectiveness and uniqueness of the sources of accumulation of the PAHs hydroxyl metabolites in the hair. On the other hand, the accumulation of metabolites in the hair is revealed, so that the method proves that the hair can be used as an ideal test material for evaluating the long-term exposure of the PAHs in the human body.
TABLE 1 GC-MS parameters for PAHs analysis in the hair
TABLE 2 liquid chromatography-tandem Mass Spectrometry parameters for OH-PAHs analysis in Hair
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. An analysis method for simultaneously detecting the levels of polycyclic aromatic hydrocarbon and hydroxyl metabolites thereof in hair is characterized by comprising the following specific steps:
s1, adding an acetone solution into the hair sample, and ultrasonically cleaning to obtain an exogenous extraction liquid; digesting the cleaned hair by an alkaline digestion solution in a water bath at 40-80 ℃, extracting the digestion solution by using a mixed solution of n-hexane and tert-butyl methyl ether, centrifugally separating, and collecting a supernatant to obtain an endogenous extraction liquid;
s2, concentrating the exogenous and endogenous extraction liquids, purifying the concentrated exogenous and endogenous extraction liquids by using gel permeation chromatography columns respectively, eluting the concentrated exogenous and endogenous extraction liquids by using a mixed solution of eluent n-hexane and dichloromethane, and collecting eluent;
s3, concentrating the collected eluent, transferring the concentrated eluent to a silica gel solid phase extraction column for separation and purification, eluting with an n-hexane solution containing 2-5% of a polar solvent, collecting the component 1, and eluting with an n-hexane solution containing 30-60% of a polar solvent, and collecting the component 2;
s4, respectively carrying out nitrogen blowing on the eluent to fix the volume: adding the component 1 into an internal standard substance, fixing the volume in isooctane, and quantifying PAHs in the component 1 by using gas chromatography-tandem mass spectrometry; fixing the volume of the component 2 in methanol, analyzing OH-PAHs by adopting a liquid chromatography-tandem mass spectrometry isotope dilution method, and obtaining the content level of a target object in hair through data processing and quantitative calculation;
in the step S2, the volume ratio of the n-hexane to the dichloromethane is (3-7): (4-6);
in step S3, the polar solvent is one or more of dichloromethane, acetone or ethyl acetate.
2. The method for simultaneously detecting the levels of polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in hair according to claim 1, wherein the ratio of the mass of the hair sample to the volume of the acetone solution in step S1 is (0.2-1) g: (5-20) mL.
3. The analytical method for simultaneously detecting the levels of polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in hair according to claim 1, wherein the alkaline digestion solution in step S1 is a sodium hydroxide solution or a potassium hydroxide solution.
4. The analytical method for simultaneously detecting the levels of polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in hair according to claim 3, wherein the concentration of the alkaline digestion solution is 0.5-1.5 mol/L.
5. The analysis method for simultaneously detecting the levels of the polycyclic aromatic hydrocarbon and the hydroxyl metabolites thereof in the hair according to claim 1, wherein the digestion time in the step S1 is 2-12 h.
6. The method for simultaneously detecting the levels of polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in hair according to claim 1, wherein the rotation speed of the centrifugation in step S1 is 1500-3500 rpm.
7. The analysis method for simultaneously detecting the levels of the polycyclic aromatic hydrocarbon and the hydroxyl metabolites thereof in the hair according to claim 1, wherein in the step S2, the elution speed of the eluent is 2-5 mL/min.
8. The method for simultaneously detecting the levels of polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in hair according to claim 1, wherein the mass to volume ratio of the amount of the filler in the silica gel solid phase extraction cartridge in step S3 is (60-1000) mg: (3-6) mL; and the elution speed of elution is 1-2 mL/min.
9. The analytical method for simultaneously detecting the levels of polycyclic aromatic hydrocarbons and hydroxyl metabolites thereof in hair according to claim 1, wherein the gas chromatography-tandem mass spectrometry test conditions in step S4 are as follows: the gas chromatography conditions include that split-flow sample introduction is carried out for 1-2 muL, the temperature of a sample inlet is 250-280 ℃, the temperature of a transmission line is 300 ℃, the flow rate of high-purity helium gas is 1-1.5 mL/min, the temperature rise program is that 1min is reserved at 80 ℃, 10 ℃/min to 200 ℃, 2 ℃/min to 260 ℃, 10 ℃/min to 300 ℃, 10min is reserved, a chromatographic column is a 5% phenyl-methyl polysiloxane capillary column, the size of the capillary column is 30m multiplied by 0.25mm multiplied by 0.25 mu m, and the temperature of an electron bombardment ionization source is 230 ℃.
10. The analytical method for simultaneously detecting the levels of polycyclic aromatic hydrocarbons and hydroxy metabolites thereof in hair according to claim 1, wherein the conditions of the liquid chromatography-tandem mass spectrometry isotope dilution method in step S4 are as follows: the liquid chromatography mobile phase is ultrapure water added with 0.1% acetic acid and methanol, the flow rate is 0.2-0.4 mL/min, the column temperature is 30-40 ℃, the gradient elution procedure is started to be 50% methanol, the methanol is increased to 90% within 15min, and the methanol is kept for 5 min; and (2) separating OH-PAHs by using a C18 reversed phase chromatographic column with the particle size of less than or equal to 2.7 microns, wherein an ion source is in an ESI negative mode, the temperature of nitrogen in the ion source is 300-350 ℃, the flow rate is 4-6L/min, the temperature of sheath gas is 300-350 ℃, the flow rate is 10-12L/min, and the capillary voltage is 3000-4000V.
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| 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 |
| 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 |
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