CN106483230A - A kind of method for quick of urine Hydroxyl Polycyclic Aromatic - Google Patents
A kind of method for quick of urine Hydroxyl Polycyclic Aromatic Download PDFInfo
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Abstract
The invention discloses a kind of method for quick of urine Hydroxyl Polycyclic Aromatic, comprise the steps：By urine sample centrifugation and carrying out enzymolysis processing to supernatant makes OH PAHs dissociate, and obtains the urine sample of pretreatment；Add dispersant acetone and the positive undecyl alcohol of extractant of mix homogeneously in the urine sample of pretreatment, be layered after mixing, positive undecyl alcohol layer is suspended in surface；Sample is cooled to positive undecyl alcohol layer solidification, the positive undecyl alcohol layer taking out solidification is dissolved in organic solvent, carries out chromatography.Compared with prior art, wherein pretreatment process carries out fast injection extraction using micro organic solvent, and processing procedure only needs to complete for 15 minutes；The use of quantity of solvent is the 1/30 of conventional solid extraction; process time is only the 1/16 of traditional method; greatly reduce the processing cost of great amount of samples and analysis time on epidemiology, simultaneously also more environmental protection, be conducive to protection healthy to analysis operation personnel.
Description
Technical field
The present invention relates to a kind of method for quick, particularly to a kind of quick detection side of urine Hydroxyl Polycyclic Aromatic
Method.
Background technology
In urine, OH-PAHs is the important biomolecule mark of carcinogenecity environmental organic pollutant PAHs, sudden and violent to PAHs in human body
Significant in dew and health risk assessment research (as PAHs molecule epidemic disease-ology research).
In urine, the testing process of OH-PAHs mainly includes sample pre-treatments and Instrumental Analysis two parts.Wherein, locate before sample
Reason process can directly affect sensitivity/test limit, repeatability and the analyze speed of whole analysis method.At present, document report
In urine, the pretreatment technology of OH-PAHs mainly includes：Solid-Phase Extraction (Solid phase extraction, SPE), the micro- extraction of solid phase
Take (Solid-phase microextraction, SPME), liquid-liquid extraction (Liquid-liquid extraction, LLE),
Liquid-liquid micro-extraction (Liquid-liquid microextraction, LLME), affine in immunity extraction (Immunosorbent
Extraction) etc.., although the needs of detection can be substantially met, time-consuming for pretreatment mode, You Jirong for solid phase extraction (SPE)
Agent usage amount is big, needs specific experimental facilitiess and has higher technical requirements to operator it is difficult to meet dividing of a large amount of samples
Analysis work is it is impossible to realize the routine clinical detection to OH-PAHs.
2006, Assidi[1]Propose with liquid-liquid dispersions extraction (DLLME) method extract micro in aqueous solution
Organic compound, the method is simple to operate, quick, and the extractant of needs is few, and is provided that the good response rate, but can not use
The extraction of organic compound in the complex matrices such as urine sample.2008, Leong[2]Et al. DLLME method is improved,
The method that he combines the solid organic drop of suspension (SFO), is used density to be less than the low-toxic organic solvent of water as extractant.
Organic drop that suspends is placed in after solidifying under low temperature it is easy to be collected, and compensate for the deficiency of traditional DLLME method, the method
It is widely used in the extraction of polarity and apolar substance in urine, blood and environmental sample, but correlation technique is not yet realized
Extraction to OH-PAHs[3,4].2012, the method for Wang liquid-liquid dispersions extraction extracted 8 kinds of OH-PAHs in deposit, makes
With chlorobenzene as extractant[5].Correlation technique is expected to be used for extracting the OH-PAHs in urine, but chlorobenzene toxicity is larger, is unfavorable for
Operator and Environmental security.
List of references：
1.Rezaee M,Assadi Y,Milani Hosseini MR,Aghaee E,Ahmadi F and Berijani
S:Determination of organic compounds in water using dispersive liquid-liquid
microextraction.J Chromatogr A.1116:1-9,2006.
2.Leong MI and Huang SD:Dispersive liquid-liquid microextraction
method based on solidification of floating organic drop combined with gas
chromatography with electron-capture or mass spectrometry detection.J
Chromatogr A.1211:8-12,2008.
3.Ahmadi-Jouibari T,Fattahi N and Shamsipur M:Rapid extraction and
determination of amphetamines in human urine samples using dispersive liquid-
liquid microextraction and solidification of floating organic drop followed
by high performance liquid chromatography.J Pharm Biomed Anal.94:145-51.
4.Chen B and Huang Y:Dispersive liquid-phase microextraction with
solidification of floating organic droplet coupled with high-performance
liquid chromatography for the determination of Sudan dyes in foodstuffs and
water samples.J Agric Food Chem.62:5818-26.
5.Wang X,Lin L,Luan T,Yang L and Tam NF:Determination of hydroxylated
metabolites of polycyclic aromatic hydrocarbons in sediment samples by
combining subcritical water extraction and dispersive liquid-liquid
microextraction with derivatization.Anal Chim Acta.753:57-63.
Content of the invention
It is an object of the invention to provide a kind of method for quick of urine Hydroxyl Polycyclic Aromatic, the method also pole simultaneously
For environmental protection, it is also a kind of high-throughout detection method simultaneously.
The technical solution used in the present invention is：
A kind of method for quick of urine Hydroxyl Polycyclic Aromatic, comprises the steps：
1) urine sample pretreatment：By urine sample centrifugation and carrying out enzymolysis processing to supernatant makes OH-PAHs dissociate, and obtains pretreatment
Urine sample；
2) extract：Add dispersant acetone and the positive undecyl alcohol of extractant of mix homogeneously in the urine sample of pretreatment, mix
After be layered, positive undecyl alcohol layer is suspended in surface；
3) sample is cooled to positive undecyl alcohol layer solidification, the positive undecyl alcohol layer taking out solidification is dissolved in organic solvent, enters
Row chromatography.
Preferably, the volumetric mixture ratio of acetone and positive undecyl alcohol is 20：(1～4), more preferably 20：(1～3).
Preferably, acetone and positive undecyl alcohol mixed liquor are 1 with the volumetric mixture ratio of urine sample：(5～40), further, third
The volumetric mixture ratio of ketone and positive undecyl alcohol is 20：(1～3).
Preferably, the operation of enzymolysis processing is as follows：
1) add pH buffer in urine sample supernatant and adjust the optimum pH of the pH of supernatant to enzyme；
2) add appropriate glucosiduronic acid enzyme/sulfatase, vibrate after mixing to enzymolysis completely.
Preferably, the pH buffer using during enzymolysis processing is Acetic acid-sodium acetate buffer system, and the pH of reaction system is 5
～6.
Preferably, before extraction, by the pH regulator of the urine sample of pretreatment to 4～6.
Preferably, before extraction, the mass of ion concentration of the urine sample of pretreatment is adjusted to 15～25%.
The invention has the beneficial effects as follows：
Compared with prior art, invention extracts-floats drop solidification method fast enriching, high-efficient liquid phase color using dispersion liquid
Spectrum-fluorescence detection method, the fast and effeciently OH-PAHs in detection urine, wherein pretreatment process adopt micro organic molten
Agent (400 μ L acetone and the positive undecyl alcohol of 40 μ L) carries out fast injection extraction, and processing procedure only needs to complete for 15 minutes；Using molten
Dosage is the 1/30 of conventional solid extraction, and process time is only the 1/16 of traditional method, greatly reduces a large amount of on epidemiology
The processing cost of sample and analysis time, also more environmental protection simultaneously, be conducive to protecting the body to analysis operation personnel to be good for
Health.
Brief description
Fig. 1 is the impact to 6 kinds of mark-on OH-PAHs response rate for the urine ph values；
Fig. 2 is the impact to the response rate for the volume of extractant (positive undecyl alcohol)；
Fig. 3 is the impact selecting to the response rate of dispersant；
Fig. 4 is the impact to the response rate for the volume of dispersant；
Fig. 5 is the impact to the response rate for the addition of salt.
Specific embodiment
A kind of method for quick of urine Hydroxyl Polycyclic Aromatic, comprises the steps：
1) urine sample pretreatment：By urine sample centrifugation and carrying out enzymolysis processing to supernatant makes OH-PAHs dissociate, and obtains pretreatment
Urine sample；
2) extract：Add dispersant acetone and the positive undecyl alcohol of extractant of mix homogeneously in the urine sample of pretreatment, mix
After be layered, positive undecyl alcohol layer is suspended in surface；
3) sample is cooled to positive undecyl alcohol layer solidification, the positive undecyl alcohol layer taking out solidification is dissolved in organic solvent, enters
Row chromatography.
Preferably, the volumetric mixture ratio of acetone and positive undecyl alcohol is 20：(1～4), more preferably 20：(1～3).
Preferably, acetone and positive undecyl alcohol mixed liquor are 1 with the volumetric mixture ratio of urine sample：(5～40), further, third
The volumetric mixture ratio of ketone and positive undecyl alcohol is 20：(1～3).
Preferably, the operation of enzymolysis processing is as follows：
1) add pH buffer in urine sample supernatant and adjust the optimum pH of the pH of supernatant to enzyme；
2) add appropriate glucosiduronic acid enzyme/sulfatase, vibrate after mixing to enzymolysis completely.
Preferably, the pH buffer using during enzymolysis processing is Acetic acid-sodium acetate buffer system, and the pH of reaction system is 5
～6.
Adjust the pH value of urine, increase or decrease the total amount of proton in urine, the extraction of OH-PAHs can be conducive to.Preferably
, before extraction, by the pH regulator of the urine sample of pretreatment to 4～6.
Add the ionic strength that saline solution increases in urine in urine, be conducive to OH-PAHs to be present in molecular forms
It is easy to extract in urine.Preferably, before extraction, the mass of ion concentration of the urine sample of pretreatment is adjusted to 15～25%.
With reference to experiment, further illustrate technical scheme.
The preparation of object standard solution
The list mark concentration being purchased from Cambridge Isotope Laboratories is 50mg/L, as storing solution；OH-
PAHs standard is used in mixed way liquid：The standard reserving solution measuring each monomer of OH-PAHs is in 10mL volumetric flask, fixed with methanol dilution
Hold, obtain the hybrid standard that OH-PAHs concentration is 5mg/L and use liquid.The mixed mark of dilution obtains concentration and is respectively 10,50,250 μ g/
L, as the concentration of mark-on urine sample.Standard specimen is sealed in -20 DEG C of refrigerators and keeps in Dark Place.
Sample pretreatment
1) sample centrifugation：Take out cold preservation sample to put to room temperature, take the urine sample more than 5mL, after 3000r/min centrifugation, take
The supernatant；
2) enzymolysis of sample：Accurately measure 5mL urine sample (supernatant after centrifugation) in tool plug graduated centrifuge tube, add-back
Yield indicant uses solution 10 μ L, adds the buffer solution of 0.5mL hydrochloric acid and 1.5mL Sodium Acetate Trihydrate and acetic acid after mixing, adjusts pH
It is worth for 5.5, plus 20 μ L glucosiduronic acid enzymes/sulfatase, it is placed in reaction 16h in constant temperature oscillation case, 37 DEG C of constant temperature, vibration after mixing
Case hunting speed 100r/min.
The extraction of sample
1) take good urine sample 5ml of above-mentioned enzymolysis, be separately added into dispersant and the extractant positive ten of different proportion mix homogeneously
One alcohol, draws dispersant and the extractant of mix homogeneously afterwards, is rapidly injected in urine sample, mix and extracted with syringe；
2) it is centrifuged after the completion of extracting, makes positive undecyl alcohol be suspended in surface, sample is refrigerated to positive undecyl alcohol solidification；
3) take out the positive undecyl alcohol of solidification, with methanol dissolving, carry out chromatograph after the nylon membrane removal particulate matter crossing 0.2 μm and divide
Analysis.
Below based on the extraction processing flow process of above-mentioned sample, change partial condition therein, determine different extraction conditionss pair
The impact of the OH-PAHs response rate.
The impact to the mark-on compound response rate for the pH
Be in the urine sample of 50 μ g/L in mark-on (6 kinds of OH-PAHs) concentration, adjust urine pH value be respectively 2,3,4,5,6,
7th, 8 and 9, the NaCl adding 2.0g adjusts concentration of salt solution, takes 400 μ L acetone to mix with the positive undecyl alcohol of 40 μ L, extraction time
For 5min, compare the response rate of mark-on compound.Experimental result as shown in figure 1, it can be seen that during pH 3～6,6 kinds
OH-PAHs is respectively provided with the preferable response rate, and pH is optimal when 5.
The commensurability impact to the mark-on compound response rate of extractant
It is in the urine sample of 50 μ g/L in mark-on (6 kinds of OH-PAHs) concentration, the pH value adjusting urine is 5, adds 2g NaCl
Adjust concentration of salt solution, take dispersant to be the extractant (positive 11 respectively with 30,40,50,60 and 70 μ L volumes for the 400 μ L acetone
Alcohol) mixing, extraction time is 5min, compares the response rate of mark-on compound.Experimental result is as shown in Fig. 2 can from figure
Go out, the addition of positive undecyl alcohol has a certain impact to the response rate of 6 kinds of OH-PAHs, addition is respectively provided with 30～70 μ L
The preferably response rate, when particularly its consumption is 40 μ L, has optimal comprehensive recovery.
The impact to the response rate for the dispersant
It is in the urine sample of 50 μ g/L in mark-on (6 kinds of OH-PAHs) concentration, the pH value adjusting urine is 5, adds 2g NaCl
Adjust concentration of salt solution, the volume taking dispersant is 400 μ L, and three kinds of solvents (methanol, acetonitrile and acetone) are respectively with 40 μ L just
Undecyl alcohol mixes, and extraction time is 5min, compares the response rate of mark-on compound.Experimental result is as shown in figure 3, permissible from figure
Find out, when dispersant is for acetone, 6 kinds of OH-PAHs can be made all to obtain the good response rate.
The impact to the response rate for the dispersant volume
It is in the urine sample of 50 μ g/L in mark-on (6 kinds of OH-PAHs) concentration, the pH value adjusting urine is 5, adds 2g NaCl
Adjust concentration of salt solution, take the volume of dispersant acetone to be respectively 200,300,400,500 and 600 μ L, respectively with 40 μ L just
Undecyl alcohol mixes, and extraction time is 5min, compares the response rate of mark-on compound.Experimental result is as shown in figure 4, permissible from figure
Find out, in 200～400 μ L, the response rate of 6 kinds of OH-PAHs all can accept the consumption of acetone, considers, the body of acetone
When amassing as 400 μ L, the response rate of 6 kinds of OH-PAHs is optimal.
The impact to the response rate for the amount of saline solution
Be in the urine sample of 50 μ g/L in mark-on (6 kinds of OH-PAHs) concentration, adjust urine pH value be 5, respectively add 0.5,
1.0th, 1.5 and 2.0g NaCl adjusts concentration of salt solution, takes 400 μ L acetone to mix with the positive undecyl alcohol of 40 μ L, extraction time is
5min, compares the response rate of mark-on compound.Experimental result as shown in figure 4, it can be seen that the addition of salt 1～
During 2g, the response rate of 6 kinds of OH-PAHs all can accept, and when the addition of salt is 2,6 kinds of OH-PAHs can obtain optimal returning
Yield.
The impact to the response rate for the extraction time
It is in the urine sample of 50 μ g/L in mark-on (6 kinds of OH-PAHs) concentration, the pH value adjusting urine is 5, adds 2.0g's
NaCl adjusts concentration of salt solution, takes 400 μ L acetone to mix with the positive undecyl alcohol of 40 μ L, and extraction time is respectively 2,5,10 and
20min, compares the response rate of mark-on compound.Find the increase with extraction time, the response rate of compound does not almost change,
It is taken as that dispersion liquid extraction process is very quick, in order to reach sufficient extraction, final choice extraction time is 5min.
To sum up, for obtaining optimal effect of extracting, the extraction conditionss of selection are：Urine sample after every 5ml enzymolysis processing, is adjusted
The pH value of urine is 5, and the NaCl adding 2.0g adjusts concentration of salt solution, takes 400 μ L acetone to mix with the positive undecyl alcohol of 40 μ L, extraction
The time is taken to be 5min.
Using the extraction conditionss of above-mentioned optimization, take out processing the positive undecyl alcohol of solidification obtaining, be dissolved in 400 μ L methanol,
The nylon membrane crossing 0.2 μm removes particulate matter, enters liquid chromatograph detection and analysis.
Liquid chromatograph and detector condition
Chromatographic column：Agilent ZORBAX SB-C18 pillar, internal diameter 4.6mm, long 250mm, stainless steel column.Post is filled：
C18 bound porous silica gel, 5 μm of particle diameter；Column temperature：25℃；Eluent gradient drip washing ratio and flow velocity are shown in Table 1；Detection wavelength is shown in Table
2；Sample size：20μL.
Table 1 mobile phase ratio and flow velocity
Table 2 ultraviolet light detects parameter
The configuration of following object standard specimens is obtained for solvent by different Concentraton gradient (totally 7 test points) with methanol, draws
Standard curve simultaneously detects its range of linearity of calculating.As linear coefficient (R2)>When 0.999, show linearly preferable, it is fixed thus to carry out
Amount calculates.Wherein, RSD is the standard deviation of 3 detections of same concentration, and LOD is minimal detectable concentration, and LOQ is that minimum quantitation is dense
Degree, cycles of concentration be urine process after volume compared with original sample volume minification.Experimental result is as shown in table 3.
Table 3 DLLME-SFO method analyzes the analysis feature of human urine
Respective standard product are separately added in urine specimen by following spiked levels, after sample process and extraction, calculate
The response rate of respective objects thing.Experimental result is as shown in table 4.
The response rate under the various spiked levels of table 4
Under the extraction conditionss of above-mentioned optimization, using the detection of high performance liquid chromatography fluorescence detector, 6 kinds of Hydroxyl Polycyclic Aromatics
Enrichment times can reach 52～65 times；The response rate of each compound reaches 70.4%～129%；Method detection limit (S/N=3)
In 0.5～1.0 μ g/L.
Claims (9)
1. a kind of method for quick of urine Hydroxyl Polycyclic Aromatic, comprises the steps：
Urine sample pretreatment：By urine sample centrifugation and carrying out enzymolysis processing to supernatant makes OH-PAHs dissociate, and obtains the urine sample of pretreatment；
Extraction：Add dispersant acetone and the positive undecyl alcohol of extractant of mix homogeneously in the urine sample of pretreatment, be layered after mixing,
Positive undecyl alcohol layer is suspended in surface；
Sample is cooled to positive undecyl alcohol layer solidification, the positive undecyl alcohol layer taking out solidification is dissolved in organic solvent, carries out chromatograph
Analysis.
2. method for quick according to claim 1 it is characterised in that：The volumetric mixture ratio of acetone and positive undecyl alcohol is
20：（1～4）.
3. method for quick according to claim 1 and 2 it is characterised in that：Acetone and positive undecyl alcohol mixed liquor and urine
The volumetric mixture ratio of sample is 1：（5～40）.
4. method for quick according to claim 1 it is characterised in that：The operation of enzymolysis processing is as follows：
Add pH buffer in urine sample supernatant and adjust the optimum pH of the pH of supernatant to enzyme；
Add appropriate glucosiduronic acid enzyme/sulfatase, vibrate after mixing to enzymolysis completely.
5. method for quick according to claim 4 it is characterised in that：PH buffer is Acetic acid-sodium acetate buffer body
System, the pH of reaction system is 5～6.
6. method for quick according to claim 1 it is characterised in that：The volumetric mixture ratio of acetone and positive undecyl alcohol is
20：（1～3）.
7. the method for quick according to claim 1 or 6 it is characterised in that：Acetone and positive undecyl alcohol mixed liquor and urine
The volumetric mixture ratio of sample is 1：（10～15）.
8. method for quick according to claim 1 it is characterised in that：Before extraction, the pH of the urine sample of pretreatment is adjusted
Save to 4～6.
9. method for quick according to claim 1 it is characterised in that：Before extraction, by the ion of the urine sample of pretreatment
Mass concentration is adjusted to 15～25%.
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| CN110779996A (en) * | 2019-10-22 | 2020-02-11 | 南方医科大学 | Method for measuring content of volatile N-nitrosamine compound in plasma by gas chromatography-mass spectrometry |
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