CN111307996B - Method for detecting black carbon in animal biological sample - Google Patents
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- CN111307996B CN111307996B CN202010298346.XA CN202010298346A CN111307996B CN 111307996 B CN111307996 B CN 111307996B CN 202010298346 A CN202010298346 A CN 202010298346A CN 111307996 B CN111307996 B CN 111307996B
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Abstract
A method for detecting black carbon in an animal biological sample relates to the field of atmospheric particle poison research. Collecting an animal biological sample, carrying out nitrolysis on black carbon particles in the sample to obtain benzene polycarboxylic acid in a small molecular state, detecting the concentration of the benzene polycarboxylic acid by using a gas chromatography-mass spectrometry combined platform, and finally converting the concentration of the benzene polycarboxylic acid into the concentration of black carbon. The molecular state of the benzene polycarboxylic acid in the aqueous solution is maintained under a strong acidic condition, the adsorption of target molecules is realized based on an action mechanism mainly based on pi-pi adsorption between the molecular benzene polycarboxylic acid and a stationary phase, and meanwhile, the strong acidic operating condition is favorable for the chelation removal and elution of metal ions and other interferents. The solid phase extraction technology is utilized to greatly simplify the process of extracting the benzene polycarboxylic acid in the black carbon nitrate solution, and finally, the concentration of the derivatized benzene polycarboxylic acid is detected by a gas chromatography-mass spectrometry combined platform and is converted into the concentration of black carbon. Make up for the short plate that the past benzene polycarboxylic acid method can only analyze the black carbon in the environmental sample.
Description
Technical Field
The invention relates to the field of research on atmospheric particle toxicants, in particular to a method for detecting black carbon in an animal biological sample.
Background
With the rapid development of economy in China, the industrialization and the urban process in China are accelerated, the total pollutant emission amount is high all the year around, and atmospheric pollution becomes an inevitable serious problem affecting the health of residents. The main particulate atmospheric pollutants affecting the health of residents are PM2.5 (particles with an aerodynamic diameter of less than 2.5 microns) which can enter the lungs and are mainly produced by fuel combustion, transportation, industrial production, building and road dust emission and the like, and black carbon is a key component constituting the PM 2.5.
Related epidemiological studies have shown that black carbon exposure is associated with low birth weight occurring early in life ([1 ]]Pedersen M, et al, ambient air polarization and low birthweight a European court study (ESCAE) Lancet Respir Med 2013; 1: 695-one 704.), cognitive dysfunction in children ([2 ]]Sunyer J.The neurological effects of air pollution in children.Eur Respir J 2008；32:535–537；[3]Sanen ND, et al, Nawrot TS, Recent vertical respiratory tract to particulate matter air polarization in association with a nuclear biological performance in a panel study of primary schoolhildren, Environ Int 2016; 95: 112-]Nawrot TS, et al, public health opportunity of triggerers of mycological attack a comparative rank assessment, Lancet 2011; 377: 732-]Guerra S, et al.relationship between circulating CC16 concentrations, lung function, and level of respiratory important disease access the life span a pro-active post.Lancet Respir. Med 2015; 3: 613-]raw-Nielsen O, et al, Air polarization and illumination cancer introduction in 17European countries, pro-active analytes from the European students of countries for Air polarization Effects (ESCAE), Lancet Oncol 2013; 14: 813-822.) and even studies have shown that the black carbon particles can penetrate the blood brain barrier of animals ([7 ]]
G, et al, transition of inert ultrafine particles to the blue. inert Toxicol 2004; 16: 437-445.) and penetrate the blood-fetal barrier of human body to influence the growth and development of fetus in uterus and after birth (8)]BovéH,et al.Ambient black carbon particles reach the fetal side of human placenta.Nat Commun.2019；10(1):3866.Published 2019Sep 17)。
Epidemiological studies can only reveal correlations between black carbon exposure and disease outcome at the environmental monitoring level, and the spread of its conclusions is limited. In recent two years, although foreign research has been conducted on black carbon exposure from the biological monitoring level, the detection technology is limited to characterizing the light absorption characteristics and morphology of black carbon and lacks of material structure information at the molecular level ([9] Saenen, n.d. et al. children's environmental carbon load: a novel marker reflecting residual atmospheric oxygen, am.j.respir. crit.car.med.2017, 196, 873-881); in addition, the instrument cost of the detection method is high, so that the detection technology is poor in popularization, and the development of the black carbon detection method which is low in cost, wide in applicability, simple in operation and easy to popularize is urgently needed.
Disclosure of Invention
The invention aims to provide a method for detecting black carbon in an animal biological sample in order to visually know the distribution of black carbon exposed in different tissues or organs. According to the method, an animal biological sample is collected, black carbon particles in the sample are nitrified and decomposed into benzene polycarboxylic acid in a small molecular state, the concentration of the benzene polycarboxylic acid is detected by using a gas chromatography-mass spectrometry combined platform, and finally the concentration of the benzene polycarboxylic acid is converted into the concentration of black carbon.
The invention comprises the following steps:
1) sample pretreatment: taking a proper amount of frozen animal samples, and putting the frozen animal samples into a clean fume hood for warm thawing;
2) high-temperature high-pressure nitrolysis: adding 0.5-3 g of an animal sample and concentrated nitric acid in a quadruple proportion into an inner cup of a polytetrafluoroethylene high-pressure reaction kettle, screwing a stainless steel outer sleeve, putting the stainless steel outer sleeve into a preheated oven, taking out a digestion tank after the temperature in the oven is lower than room temperature after the nitration is finished, and transferring digestion liquid in the reaction kettle to a glass test tube in a fume hood;
3) solid phase extraction: after the solid phase extraction column is activated, adding 0.5-1mL of digestion solution into the small column until the digestion solution is naturally dripped, centrifuging the extraction column, vacuumizing to dry the small column, adding 5mL of methanol into the small column for elution to obtain a first eluent, and centrifuging and collecting the small column to obtain a second eluent;
4) derivation and purification: mixing the first eluent and the second eluent obtained in the step 3), putting the mixture into a nitrogen blowing instrument, concentrating the mixture until the mixture is dry, adding the purified extracting solution after the mixture is completely derived, uniformly mixing, centrifuging, and collecting the upper-layer solution;
5) putting the upper layer solution collected in the step 4) into a nitrogen blowing instrument for concentration till the upper layer solution is dry, selecting a proper chromatographic column for vacuumizing, and then injecting a sample obtained after redissolving the organic solvent into a GC-MS computer with a temperature rise program for analysis.
In step 1), the animal sample may be selected from tissues, organs or body fluids of various animals as well as humans; the frozen animal samples can be stored in a refrigerator at-80 ℃.
In step 2), the weight ratio of the animal sample to the concentrated nitric acid can be 1: 4; the preheating temperature of the oven can be 170-180 ℃; the temperature of the nitrolysis can be 170-180 ℃, and the time of the nitrolysis can be 7-8 h.
In step 3), the extraction column can use Oasis HLB, Waters 186000117, 20cc Vac cartridge, 1g Sorbent per cartridge,60 μm Particle Size; the activation condition can be that 20mL of methanol and 5mL of 0.1M hydrochloric acid are added for activation; the extraction column centrifugation can be carried out for 10min at 4 ℃ and 3000 rpm; the vacuumizing can be realized by adopting a water circulation multi-purpose vacuum pump or other vacuum filtration devices; the elution condition is 5mL of methanol naturally dripped dry, and the small column centrifugation condition can be 3000rpm centrifugation for 15 min.
In step 4), 0.5mL of methanol, 0.5mL of xylene and a proper amount of derivatization reagent can be added into the derivatization conditions; the derivatization reagent can adopt trimethyl silyl diazomethane ether solution; the method for complete derivatization comprises the steps of dropwise adding an excessive derivatization reagent, standing at room temperature for 30min, and then derivatizing once again; the phenomenon of complete derivatization is that the solution does not generate bubbles any more or the solution turns yellow; the purified extract can be aqueous solution obtained by mixing n-hexane, water, acetic acid and 0.5mol/L NaOH at volume ratio of 1: 0.05: 0.10, shaking, mixing, collecting n-hexane layer, and extracting twice; the centrifugation conditions can be 4 ℃, 3000rpm and 15 min.
In the step 5), the on-machine analysis refers to qualitative and quantitative detection of the derivatized solution by using gas chromatography-tandem mass spectrometry, and the appropriate chromatographic column can adopt an Agilent DB-5MS nonpolar gas chromatographic column; the temperature raising program is that the temperature is maintained at 60 ℃ for 1min, the temperature is raised to 300 ℃ at 10 ℃/min, and the temperature is maintained at 300 ℃ for 2 min; the organic solvent can adopt n-hexane.
In the steps 4) and 5), the temperature of the nitrogen blowing instrument is set to be 40-60 ℃.
The invention provides a method for evaluating black carbon detection in different tissues after black carbon exposure, which has the key points that the molecular state of benzene polycarboxylic acid in an aqueous solution is maintained by utilizing a strong acid condition, the adsorption of target molecules is realized based on an action mechanism mainly based on pi-pi adsorption between the molecular benzene polycarboxylic acid and a stationary phase, and meanwhile, the strong acid operation condition is favorable for the chelation removal and elution of metal ions and other interferents. The solid phase extraction technology is utilized to greatly simplify the process of extracting the benzene polycarboxylic acid in the black carbon nitrate solution, and finally, the concentration of the derivatized benzene polycarboxylic acid is detected by a gas chromatography-mass spectrometry combined platform and is converted into the concentration of black carbon. Different from other methods, the method for detecting the black carbon concentration in the environmental sample is improved, and the method for detecting the black carbon concentration by the benzene polycarboxylic acid is expanded and applied to the animal biological sample for the first time. The short plate which can compensate the prior benzene polycarboxylic acid method and only can analyze the black carbon in the environmental sample provides firmer evidence for influencing the individual health by environmental pollution (especially the black carbon). The core protection point of the invention is that the method is simple, has wide applicability and can provide an effective method for detecting the black carbon in different animal biological samples.
Therefore, the invention has the following outstanding technical effects:
1. the invention is based on the traditional gas chromatography-mass spectrometry platform and has strong popularization.
2. The invention utilizes the information of human tissues or animal tissues to improve the accuracy data of the influence of air pollution (especially black carbon) on different individuals.
3. The invention can analyze the concentration of black carbon in different tissues in the same organism and reveal the migration possibility of the black carbon among the same tissue or organs.
Drawings
FIG. 1 is a GC-MS quantitative ion extraction chromatogram of a target in a 4000. mu.g/L mixed standard.
FIG. 2 is a GC-MS quantitative ion extraction chromatogram of a target in an actual human serum sample.
FIG. 3 is a GC-MS quantitative ion extraction chromatogram of a target in a human placenta real sample.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The embodiment of the invention comprises the following steps:
(1) sample pretreatment: taking a proper amount of animal samples stored in a refrigerator at minus 80 ℃, and putting the animal samples into a clean fume hood for warm thawing. The animal sample is tissue, organ or body fluid of various animals and human beings.
(2) High-temperature high-pressure nitrolysis: adding 0.5-3 g of the animal sample and concentrated nitric acid in a quadruple proportion into an inner cup of a polytetrafluoroethylene high-pressure reaction kettle, screwing a stainless steel outer sleeve, and putting the stainless steel outer sleeve into an oven preheated to 170-180 ℃. Digesting for 7-8h, taking out the digestion tank after the temperature in the oven is lower than the room temperature, and transferring the digestion solution in the reaction kettle to a glass test tube in a fume hood.
(3) Solid phase extraction: adding 20ml of methanol and 5ml of 0.1M hydrochloric acid into the column sequentially to activate the solid phase extraction column, adding 0.5-1ml of digestion solution into the column, naturally dripping the digestion solution, centrifuging the extraction column, and vacuumizing to dry the column. And adding 5ml of methanol into the small column for elution to obtain a first eluent, and centrifugally collecting the small column to obtain a second eluent. The solid phase extraction column was Oasis HLB (Waters 186000117, 20cc Vac Cartridge, 1g Sorbent per cart, 60 μm Particle Size). The vacuum-pumping instrument is a water circulation multipurpose vacuum pump or other vacuum pumping filtration devices.
(4) Derivation and purification: and mixing the first eluent and the second eluent, putting the mixture into a nitrogen blowing instrument, concentrating the mixture to be dry, adding 0.5ml of methanol and 0.5ml of dimethylbenzene, and adding a proper amount of derivative reagent to completely derive. Then adding purified extract, mixing, centrifuging at 4 deg.C and 3000rpm for 15 min. The upper solution was collected. The derivative reagent is trimethyl silyl diazomethane. The conditions for complete derivatization are that the solution does not generate bubbles any more and the color turns yellow. The purified extract is aqueous solution prepared by mixing n-hexane, water, acetic acid, and 0.5mol/L NaOH at volume ratio of 1: 0.05: 0.10.
(5) And (3) putting the collected upper-layer solution into a nitrogen blowing instrument, concentrating to be dry, redissolving the organic solvent, and carrying out qualitative and quantitative detection on the solution subjected to derivatization by using a gas chromatography-tandem mass spectrometry. The centrifugation condition is 4 ℃, the rotating speed is 3000rpm, and the centrifugation is carried out for 15 min.
Specific examples are given below.
Example 1:
the design of the example is based on the detection of the black carbon concentration in blood of a mouse under the exposure of PM2.5 in the real environment of the mouse, and the specific steps are as follows:
first, mouse actual environment PM2.5 exposure experiment
The method comprises the following steps of intercepting PM2.5 particulate matters on a filter membrane by adopting an atmospheric fine particulate matter sampler, ultrasonically preparing an obtained particulate matter sample and a buffer solution (phosphate buffer solution or normal saline) into suspension with a certain concentration for trachea instillation, and converting the concentration of the PM2.5 suspension according to the Chinese air quality standard and the average weight of mice. Mice were acclimatized for a period of time and then exposed to atmospheric particulates by tracheal instillation.
Second, nitrolysis of mouse blood samples
After acute exposure in an experimental period, adding concentrated nitric acid into mouse blood at a ratio of 1: 4, loading into a Teflon nitrolysis tank, sealing, and putting into an oven for nitrolysis at 170 ℃ for 7 h.
Third, passing column of blood nitrate solution
And sequentially adding 20mL of methanol and 5mL of 0.1M hydrochloric acid solution to activate the extraction column, adding 1mL of nitrate solution, naturally dripping to dry, centrifuging the extraction column at 3000rpm for 10min, vacuumizing the extraction column until water in the column is drained, dripping 5mL of methanol to elute, centrifuging the extraction column at 3000rpm for 10min, and collecting residual eluent to obtain a target methanol solution.
Fourthly, derivation and purification of target object
And blowing the target methanol solution to be dried by nitrogen at 45 ℃, adding 0.5mL of methanol, 0.5mL of dimethylbenzene and excessive trimethylsilyl diazomethane, reacting at room temperature for 30min after violent oscillation, then dropwise adding a proper amount of trimethylsilyl diazomethane, standing for 30min, dropwise adding 1 drop of acetic acid, 2mL of n-hexane, 2mL of water and 0.5mol/L of NaOH in sequence, and violently oscillating. After two extractions, centrifugation was carried out, and the n-hexane layer was retained.
Fifth, detection of target
The method is characterized in that the benzene polycarboxylic acid is detected by using a gas chromatography-mass spectrometry combined platform, a single quadrupole gas mass combined system of Agilent is used in the United states, and retention time correction, mass spectrum characteristic peak ion information and a sample related ion information table are carried out by MassHunter software in a full scan mode and a selective ion scan mode.
Before testing, the stability of the instrument is evaluated by a blank solvent n-hexane, and the peak change caused by the attenuation of the instrument is corrected by inserting the low, medium and high-concentration mixed standard substance in the test queue at equal intervals.
In the embodiment of the invention, a GC-MS quantitative ion extraction chromatogram of a target object in a 4000 mu g/L mixed standard is shown in figure 1, a GC-MS quantitative ion extraction chromatogram of a target object in an actual human serum sample is shown in figure 2, and a GC-MS quantitative ion extraction chromatogram of a target object in an actual human placenta sample is shown in figure 3. As can be seen from the figure, the molecular structures of different BPCAs methyl esterification products are different, and the generated main characteristic ion is the ion of each substance after the molecular ion loses 1-OCH 3 group. The corresponding target can be characterized according to the characteristic ions and the chromatographic retention time, and (semi-) quantified according to the size of chromatographic peak in the actual sample and the size of the standard concentration-chromatographic peak. From fig. 1 (the chromatogram mass spectrum of the target of the standard), it can be seen that the chromatogram mass spectrum peak of each standard can obtain baseline separation, and the peak shape is symmetrical without tailing. From fig. 2 (chromatogram mass spectrum of target in human serum sample) and 3 (chromatogram mass spectrum of target in human placenta tissue sample), it can be seen that the chromatogram baseline obtained in the actual sample is stable, and both benzene polycarboxylic acid and nitrobenzene polycarboxylic acid are well separated, indicating that the separation condition meets the detection requirement.
The invention provides a technical method for detecting black carbon in an animal biological sample. Which comprises the following steps: s1, collecting a biological sample; s2, nitrolysis of the biological sample; s3, derivatization and purification of the nitrolysis product; and S4, detecting the target object by gas chromatography-mass spectrometry. The method utilizes a solid phase extraction technology to extract benzene polycarboxylic acid obtained after the nitration of the black carbon in the biological sample, provides a new method for detecting the black carbon in the biological sample, simplifies the sample pretreatment process and improves the accuracy of the detection of the black carbon concentration compared with other black carbon detection technologies, and is suitable for other chromatographic-mass spectrometry platforms.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (4)
1. A method for detecting black carbon in an animal biological sample is characterized by comprising the following steps:
1) sample pretreatment: taking a proper amount of frozen animal samples, and putting the frozen animal samples into a clean fume hood for warm thawing;
2) high-temperature high-pressure nitrolysis: adding 0.5-3 g of an animal sample and concentrated nitric acid in a quadruple proportion into an inner cup of a polytetrafluoroethylene high-pressure reaction kettle, screwing a stainless steel outer sleeve, putting the stainless steel outer sleeve into a preheated oven, taking out a digestion tank after the temperature in the oven is lower than room temperature after the nitration is finished, and transferring digestion liquid in the reaction kettle to a glass test tube in a fume hood; the weight ratio of the animal sample to the concentrated nitric acid is 1: 4;
3) solid phase extraction: after the solid phase extraction column is activated, adding 0.5-1mL of digestion solution into the small column until the digestion solution is naturally dripped, centrifuging the extraction column, vacuumizing to dry the small column, adding 5mL of methanol into the small column for elution to obtain a first eluent, and centrifuging and collecting the small column to obtain a second eluent; the extraction column adopts Oasis HLB, Waters 186000117, 20cc Vac card, 1g Sorbent per card, 60 μm Particle Size; the activation condition is that 20mL of methanol and 5mL of 0.1M hydrochloric acid are added for activation; the extraction column centrifugation is to centrifuge the extraction column at 4 ℃ and 3000rpm for 10 min; the vacuumizing adopts a water circulation multi-purpose vacuum pump or other vacuum pumping and filtering devices to vacuumize; the elution condition is that 5mL of methanol is naturally dripped dry, and the small column centrifugation condition is that 3000rpm is used for centrifugation for 15 min;
4) derivation and purification: mixing the first eluent and the second eluent obtained in the step 3), putting the mixture into a nitrogen blowing instrument, concentrating the mixture until the mixture is dry, adding the purified extracting solution after the mixture is completely derived, uniformly mixing, centrifuging, and collecting the upper-layer solution;
the derivatization condition is that 0.5mL of methanol, 0.5mL of dimethylbenzene and a proper amount of derivatization reagent are added; the derivation reagent adopts trimethyl silyl diazomethane ethyl ether solution; the method for complete derivatization comprises the steps of dropwise adding an excessive derivatization reagent, standing at room temperature for 30min, and then derivatizing once again; the phenomenon of complete derivatization is that the solution does not generate bubbles any more or the solution turns yellow;
the purified extracting solution is an aqueous solution obtained by mixing n-hexane, water, acetic acid and 0.5mol/L NaOH according to a volume ratio of 1: 0.05: 0.10, shaking and mixing uniformly, taking an n-hexane layer, and extracting twice; the centrifugation conditions are that the temperature is 4 ℃, the rotating speed is 3000rpm, and the centrifugation is carried out for 15 min;
5) putting the upper layer solution collected in the step 4) into a nitrogen blowing instrument for concentration to dryness, selecting a proper chromatographic column for vacuumizing, and then feeding a sample obtained after redissolving the organic solvent into a GC-MS computer with a temperature rise program for analysis; the on-machine analysis is to perform qualitative and quantitative detection on the derivatized solution by using gas chromatography-tandem mass spectrometry, and the appropriate chromatographic column adopts an Agilent DB-5MS nonpolar gas chromatographic column; the temperature raising program is that the temperature is maintained at 60 ℃ for 1min, the temperature is raised to 300 ℃ at 10 ℃/min, and the temperature is maintained at 300 ℃ for 2 min; the organic solvent adopts n-hexane.
2. The method according to claim 1, wherein in step 1), the animal sample is selected from the group consisting of tissues, organs, and body fluids of various animals and humans; the frozen animal samples were stored in a-80 ℃ freezer.
3. The method for detecting the black carbon in the animal biological sample according to claim 1, wherein in the step 2), the temperature for preheating the oven is 170-180 ℃; the temperature of the nitrolysis is 170-180 ℃, and the time of the nitrolysis is 7-8 h.
4. The method for detecting black carbon in an animal biological sample according to claim 1, wherein the temperature of the nitrogen blower is set to 40 to 60 ℃ in step 4) or 5).
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