CN107101989A - Construction method based on Parameter adjustable control self-assembled structures substrate and its SERS detection methods for drugs - Google Patents
Construction method based on Parameter adjustable control self-assembled structures substrate and its SERS detection methods for drugs Download PDFInfo
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- CN107101989A CN107101989A CN201710158329.4A CN201710158329A CN107101989A CN 107101989 A CN107101989 A CN 107101989A CN 201710158329 A CN201710158329 A CN 201710158329A CN 107101989 A CN107101989 A CN 107101989A
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- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The present invention provides the construction method based on Parameter adjustable control self-assembled structures substrate and its SERS detection methods for drugs, including：Synthetic gold nanorods colloidal sol is carried out after eccentric cleaning, it is 10% 90% gold nanorods solution to be dispersed in again again after concentration and mass concentration is formed in ultra-pure water；Gold nanorods solution is dropped on treated silicon chip；And be inclined in use for laboratory simulation climate case, evaporate mechanism to induce gold nanorods colloidal sol to carry out self assembly on substrate using solvent, obtain SERS substrates；The human body fluid consumed illegal drugs is taken again, its extract carried out after pre-treatment is centrifuged, then take its organic layer solution；Organic layer solution is added drop-wise in SERS substrates, SERS detections are carried out using Portable Raman spectrometer.The present invention so that sensitivity and practicality are accomplished in the SERS detections to drug numerator, and has detection reappearance by being self-assembly of uniform SERS substrates.
Description
Technical field
The invention belongs to SERS detection technique fields, and in particular to based on constructing for Parameter adjustable control self-assembled structures substrate
Method and its SERS detection methods for drugs.
Background technology
2016 published according to the United Nations's drugs and crime problem office《World's drug issue report》：Global drugs make
It is still severe with situation, it is related to illicit drug number of users more than 2.47 hundred million.Worldwide popular drugs mainly have Ah
Tablet (heroin and opium), amphetamines (crystal methamphetamine and head-shaking pill etc.), hemp etc..And occur in that now
The new psychoactive drug substance of one class, i.e., the Abused drug occurred with pure form or formulation forms, the international poison of these materials Bu Shou
The control of product pact, but publilc health may be constituted a threat to.Wherein, the seizures of amphetamines, output and
Consumption figure, in increase year by year, is the drugs of the use being number two in world wide widely, wherein with crystal methamphetamine
(i.e. methamphetamine) is most representative.In addition, the personnel of abuse cassie ketone drugs are also quickly increasing, drugs control problem is also given
Bring new challenge.In face of such severe form, increase to system poison, traffic in drugs and the hitting dynamics of drug abuse, drug containment it is climing
Prolong and arrived very urgent stage, and fast and effectively the exploitation of illicit drugs inspection method will be played in beat drugs crime
Important effect.
1974, an accidental chance, Fleischmann et al. electrochemically carried out coarse to silver electrode surface
After change processing, absorption is obtained when being characterized with Raman spectrometer to it in the high-quality of coarse silver electrode surface Pyridine Molecules
Raman spectrogram, this initial phenomenon is not paid attention to especially.1977, Van Duyne et al. were carried out point to this phenomenon
Analysis, it is indicated that this is to be referred to as table after the enhancement effect that a kind of surface with roughening has certain inevitable relation, this effect
Face strengthens Raman scattering (surface-enhanced Raman scattering, SERS) effect or SERS
(surface-enhanced Raman spectroscopy, SERS) technology.Because of its high sensitivity, nothing since SERS self-discoveries
The advantage such as damage, fingerprint characteristic, detection speed be fast, is often used as a kind of very promising spectroscopy instruments.
The general testing cost of common illicit drugs inspection method is high, time-consuming, need the personnel of specialty, the appearance of SERS technologies
The deficiency of the above method can be made up.The method of relatively more extensive detection drugs now is by the way that the metal prepared is molten
Matrix bottom is added dropwise on silicon chip, then determinand is added dropwise in substrate, and this traditional method has one in actual mechanical process
Individual obvious the drawbacks of, the coffee toroidal effect of substrate is than more serious when exactly detecting, it is impossible to accomplish the reproduction of detection process well
Property, this has been limited for our practices and commercialization.The detection side of our drugs in SERS technologies are to human body fluid
On the basis of method, the application study that drugs SERS is detected is used for based on Parameter adjustable control self-assembled structures substrate, in the lab
Simulation climate case operation principle, to selected SERS substrates, using solvent-induced evaporation mechanism, at the same carry out humidity, temperature and
The technological parameter regulation and control such as gravity induction, carry out self assembly on treated silicon chip.Intentionally get a kind of base of even compact
Counterdie, and with our portable Raman in conjunction with so as to realize the reappearance and practicality of SERS detections.
The content of the invention
The technical problem to be solved in the present invention is the coffee toroidal effect that removal or reduction substrate are formed in film forming, stunt
For a kind of construction method based on Parameter adjustable control self-assembled structures substrate and its SERS detection methods for drugs, in simulation
Climate box operation principle, using solvent-induced evaporation mechanism, is adjusted while carrying out the technological parameters such as humidity, temperature and gravity induction
Control, self assembly is carried out on treated silicon chip, a kind of basilar memebrane of even compact, and the portable Raman with us is obtained
In conjunction with, ensure detection sensitivity on the premise of realize SERS detection reappearance and practicality.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical programs.
Based on the construction method of Parameter adjustable control self-assembled structures substrate, it comprises the following steps：
(1) synthetic gold nanorods colloidal sol is carried out after eccentric cleaning, and be dispersed in again again after being concentrated ultrapure
The gold nanorods solution that volume fraction is 10-90% is formed in water；
(2) 1-10 μ L gold nanorods solution is taken to drop on cleaning and the silicon chip through more than half hydrophilic half hydrophobic treatments；
(3) silicon chip is inclined in use for laboratory simulation climate case, evaporates mechanism to induce gold nano using solvent
Rod colloidal sol carries out self assembly on substrate, obtains SERS substrates.
Gold nanorods colloidal sol concentration in further scheme, the step (1) is 10 times of original content.
The silicon chip through more than half hydrophilic half hydrophobic treatments refers to silicon chip first through chloroazotic acid in further scheme, the step (2)
Soak at least 2h after clean, then with fresh chloroazotic acid immersion 1h after clean, and with ultrasonic cleaning instrument clean after, then with it is substantial amounts of surpass
Pure water is cleaned, and is finally dried up with nitrogen.
Silicon chip in further scheme, the step (3), which is obliquely installed, to be referred to the silicon chip for having gold nanorods solution will be added dropwise
Plane is set with the horizontal 0-90 degree angle.
The temperature range of setting is 20 DEG C -40 in use for laboratory simulation climate case in further scheme, the step (3)
DEG C, humidity range be 30%-60%；And there is fine gas to exchange with external environment condition inside simulation climate case.
Solvent evaporation mechanism in further scheme, the step (3) is to induce gold using the effect of simulation climate case
Ultra-pure water in nanometer rods colloidal sol carries out self assembly in silicon chip surface volatilization, so as to obtain SERS substrates.
Another goal of the invention of the present invention, which is to provide the SERS substrates that above-mentioned construction method formed, is used for drugs
SERS detection methods, its step is as follows：
(1) human body fluid consumed illegal drugs is taken, organic solvent is added and is extracted, then extract is centrifuged, it is taken
Organic layer solution；
(2) organic layer solution is added drop-wise in SERS substrates, SERS detections is carried out using Portable Raman spectrometer.
Human body fluid is urine in further scheme, the step (1)；The organic solvent is one in alcohols or ketone
Kind, the addition of organic solvent is to add 0.2-0.6mL per in 0.8mL human body fluids.
Drugs include amphetamine, cocaine, m orphine, can treated in human body fluid in further scheme, the step (1)
Cause, hydrochloric acid opium poppy alkali, barbiturates, hemp, THC, narcotine, caffeine, ketalar, Sauteralgyl, U.S. sand
Ketone, Clozapine, diphenoxylate, caffeine, totokaine, stabilize, oxazepan, surazepam, librium, Xanax,
Triazole storehouse, Lorazepam or fenfluramine.
Use for laboratory simulation climate case is the simple environmental cabinet built according to laboratory condition oneself, is set in climate box
Temperature and humidity, and ensure that climate box has fine gas to exchange with external environment condition, the temperature range of setting is 20 DEG C -40
DEG C, humidity range be 30%-60%.
Solvent evaporation mechanism principle be solvent in solution when silicon chip surface volatilizees, self-assembly can be induced
Form ordered structure.So-called self assembly refers to that elementary cell spontaneously forms ordered structure, and there is this structure good photoelectricity to imitate
Should.This patent is exactly the effect using simulation climate case, and it is ultrapure in gold nanorods colloidal sol to induce to evaporate mechanism using solvent
Water carries out self assembly in substrate surface volatilization, so as to obtain SERS substrates.
The synthetic method of gold nanorods colloidal sol is seed mediated growth method, is existing, specifically can refer to Dong,
Ronglu.Detection and direct readout of drugs in human urine using dynamic
surface-enhanced Raman spectroscopy and support vector machines,Anal Chem,87
(2015)2937-2944。
It mainly has following two preparation process：
One is：
(1) 10ml CTAC and the mixed liquor of sodium bromide are added in 25ml three-necked flasks (with magneton),
(2) 0.1mL HAuCl is added4Mother liquor, magnetic agitation (500r/min is maintained at 25 DEG C -27 DEG C)；
(3) it is rapidly added 60 μ L NaBH4, stir and be maintained at 25 DEG C -27 DEG C standby, stopping stirrings after a few minutes.
Two are：
(1) 20ml stopper test tubes are used；
(2) CTAC and sodium bromide mixed liquor for adding 10ml are maintained in 25 DEG C of water-baths；
(3) 0.2mL HAuCl is first added4Mother liquor；
(4) volume V AgNO is taken from small flask3In the test tube for adding step, the volume of addition is V1=120 μ L, gently
Vibration is mixed, and adds HNO30.1mL adjusts PH；
(5) 0.06mL sodium ascorbates are added to mix into test tube；
(6) 12 μ L seed solutions are finally taken to be mixed into growth-promoting media；
(7) the static 4h. in 27 DEG C of -29 DEG C of water-baths
The present invention can accomplish the reappearance that drugs SERS is detected in human urine well, and the analysis of its principles of science is：
1st, the gold nanorods colloidal sol synthesized using classical approach, carries out eccentric cleaning, and disperse again by gold nanorods colloidal sol
Into required concentration, the gold nanorods after disperseing are dropped on the silicon chip after half hydrophilic half hydrophobic treatment, in vitro
In simulation climate case, solvent-induced evaporation mechanism is utilized；Gold nano rod can be self-assembled into monolayer distribution and particle on silicon chip
Between can form the nanometer film in " gap ", form uniform, high activity SERS " focus ".
2nd, we are by gold nanorods nanometer film that prepare individual layer, uniform and fine and close, so as to accomplish reality
Detection in reappearance.
The beneficial effects of the present invention are：
(1) the SERS substrates constructed by the present invention are due to being uniform, individual layer arrangement and having " gap " gold nanorods
Film, so that with higher sensitivity, repeatability and practicality.And with higher stability, can store about 6 months.
(2) method and step of the invention for constructing substrate is simple and practical, is conducive to being applied to actual production and practicality
It is central, and carry out commercialization transformation.
(3) what the present invention was detected is that human body fluid includes the drug numerator in urine, blood, saliva, to meet actual inspection
It is applied widely the need for surveying sample difference.
(4) present invention obtained by substrate apply to drug numerator SERS detection have higher sensitivity, stability, and
And with good reappearance, to the detection limits of various drugs under 100ppb, meet actually detected standard.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is that SERS substrates that volume formed for the 1 μ L gold nanorods solution gold under different proportion is added dropwise in embodiment 1
The optical scanner electron microscope (SEM) of nanometer film；
Fig. 2 is that the SERS that volume is formed by 2 μ L, 4 μ L, 6 μ L, 8 μ L gold nanorods solution has been added dropwise in embodiment 1 respectively
The optical scanner electron microscope (SEM) of substrate.
Fig. 3 is the Raman spectrogram of SERS substrates, 10ppm head-shaking pills and the head-shaking pill standard sample of embodiment 3.
Embodiment
The invention will be further described with reference to embodiments, but the present invention is not limited to following embodiments.
Embodiment 1
(1) silicon chip is sequentially passed through after chloroazotic acid and fresh chloroazotic acid immersion treatment, then with substantial amounts of ultra-pure water clean after, use nitrogen
It is standby after air-blowing is dry；
(2) synthetic gold nanorods are centrifuged into (7500r) with ultra-pure water to clean after twice, ultra-pure water is dispersed in again
In, dispersion concentration is 60wt% gold nanorods solution；
(3) gold nanorods solution is added drop-wise on five silicon chips after (1) step process respectively, the volume difference of dropwise addition
For 1 μ L, 2 μ L, 4 μ L, 6 μ L, 8 μ L, silicon chip is inverted after dripping and is placed in use for laboratory simulation climate case, is steamed using solvent
Hair mechanism induces the gold nanorods colloidal sol to form gold nano film, as SERS substrates on silicon chip；
Wherein：Fig. 1 is that SERS substrates that volume formed by the 1 μ L gold nanorods solution Jenner under different proportion is added dropwise
The optical scanner electron microscope (SEM) of rice film, from figure 1 it appears that the SERS substrates that the present invention is constructed are uniform and fine and close.
Fig. 2 is that the SERS substrates that volume is formed by 2 μ L, 4 μ L, 6 μ L, 8 μ L gold nanorods solution have been added dropwise respectively
Optical scanner electron microscope (SEM), from figure 2 it can be seen that under the conditions of different control parameters, the substrate of gained into
Film effect is all fine.
(4) human body fluid consumed illegal drugs is taken, organic solvent alcohols is added or ketone is extracted, then extract is entered
Row centrifugation, takes its organic layer solution；Wherein the addition of organic solvent is to add 0.2mL per in 0.8mL human body fluids.
(5) organic layer solution is added drop-wise in one of SERS substrates, after the solvent volatilization of sample is dry, with portable
Raman carries out SERS detections, then is compareed to determine the classification of drugs with the Raman spectrogram of standard sample by it.
Embodiment 2
(1) silicon chip is sequentially passed through into chloroazotic acid and after the immersion of fresh chloroazotic acid handles successively, then with substantial amounts of ultra-pure water it is clean after,
The silicon chip for being made clean is dried up with nitrogen；
(2) synthetic gold nanorods are centrifuged into (7500r) with ultra-pure water to clean after twice, ultra-pure water is dispersed in again
In, be dispersed into mass concentration be respectively 20%, 40%, 60%, 80%, 100% 5 group of gold nanorods solution；
(3) five groups of gold nanorods solution are dripped on the silicon chip after (1) step process respectively, it is 4 μ L that volume, which is added dropwise,
Silicon chip is inverted after dripping and is placed in use for laboratory simulation climate case, induction filming, as SERS substrates is evaporated；
(4) human body fluid consumed illegal drugs is taken, organic solvent alcohols is added or ketone is extracted, then extract is entered
Row centrifugation, takes its organic layer solution；Wherein the addition of organic solvent is to add 0.6mL per in 0.8mL human body fluids.
(5) organic layer solution is added drop-wise in one of SERS substrates, after the solvent volatilization of sample is dry, with portable
Raman carries out SERS detections, then is compareed to determine the classification of drugs with the Raman spectrogram of standard sample by it.
Embodiment 3
(1) silicon chip is sequentially passed through into chloroazotic acid and after the immersion of fresh chloroazotic acid handles successively, then with substantial amounts of ultra-pure water it is clean after,
It is standby after being dried up with nitrogen；
(2) synthetic gold nanorods are centrifuged into (7500r) with ultra-pure water to clean after twice, ultra-pure water is dispersed in again
In, dispersion concentration is 60wt% gold nanorods solution；
(3) gold nanorods solution is dripped on the silicon chip after (1) step process, dropwise addition volume is 4 μ L, after dripping
45 degree of angles of silicon chip inclination are placed in the simulation climate case in laboratory, induction filming, as SERS substrates is evaporated；
(4) human urine for consuming illegal drugs head-shaking pill is taken, organic solvent alcohols is added or ketone is extracted, then to extraction
Take liquid to be centrifuged, take its organic layer solution；Wherein the addition of organic solvent is to add 0.3mL per in 0.8mL human urines.
(5) organic layer solution is added drop-wise in SERS substrates, after the solvent volatilization of sample is dry, carried out with portable Raman
SERS is detected, then is compareed to determine the classification of drugs with the Raman spectrogram of head-shaking pill standard sample by it.
As shown in figure 3, the respectively Raman of the SERS substrates of the present embodiment, 10ppm head-shaking pills and head-shaking pill standard sample
Spectrogram, as can be seen from Figure 3, SERS substrates produced by the present invention have good illicit drugs inspection effect, and with good
Detection sensitivity.
Embodiment 4
(1) silicon chip is sequentially passed through into chloroazotic acid and after the immersion of fresh chloroazotic acid handles successively, then with substantial amounts of ultra-pure water it is clean after,
It is standby after being dried up with nitrogen；
(2) synthetic gold nanorods are centrifuged into (7500r) with ultra-pure water to clean after twice, ultra-pure water is dispersed in again
In, dispersion concentration is 60wt% gold nanorods solution；
(3) gold nanorods solution is dripped on the silicon chip after (1) step process, dropwise addition volume is 4 μ L, after dripping
By silicon chip inclination, 90 degree are placed in the simulation climate case in laboratory, evaporate induction filming, as SERS substrates；
(4) human body fluid consumed illegal drugs is taken, organic solvent alcohols is added or ketone is extracted, then extract is entered
Row centrifugation, takes its organic layer solution；Wherein the addition of organic solvent is to add 0.5mL per in 0.8mL human body fluids.
(5) organic layer solution is added drop-wise in one of SERS substrates, after the solvent volatilization of sample is dry, with portable
Raman carries out SERS detections, then is compareed to determine the classification of drugs with the Raman spectrogram of standard sample by it.
Above is present pre-ferred embodiments, are not that the technical scope of the present invention is imposed any restrictions.Therefore it is every
Technical spirit according to the present invention belongs to this hair to any subtle modifications, equivalent variations and modifications made for any of the above embodiments
It is bright protect in the range of.
Claims (9)
1. the construction method based on Parameter adjustable control self-assembled structures substrate, it is characterised in that：Comprise the following steps：
(1) synthetic gold nanorods colloidal sol is carried out after eccentric cleaning, and be dispersed in again in ultra-pure water again after being concentrated
Form the gold nanorods solution that volume fraction is 10-90%；
(2) 1-10 μ L gold nanorods solution is taken to drop on cleaning and the silicon chip through more than half hydrophilic half hydrophobic treatments；
(3) silicon chip is inclined in use for laboratory simulation climate case, evaporates mechanism to induce gold nanorods molten using solvent
Glue carries out self assembly on substrate, obtains SERS substrates.
2. construction method according to claim 1, it is characterised in that：Gold nanorods colloidal sol concentration in the step (1)
For 10 times of original content.
3. construction method according to claim 1, it is characterised in that：Through more than half hydrophilic half hydrophobic places in the step (2)
The silicon chip of reason refers to clean after first soaking at least 2h through chloroazotic acid to silicon chip, then with being cleaned after fresh chloroazotic acid immersion 1h, and with ultrasonic
After cleaning device cleaning, then cleaned, finally dried up with nitrogen with substantial amounts of ultra-pure water.
4. construction method according to claim 1, it is characterised in that：Silicon chip in the step (3), which is obliquely installed, to be referred to
The silicon chip plane for having gold nanorods solution will be added dropwise with the horizontal the setting of 0-90 degree angle.
5. construction method according to claim 1, it is characterised in that：Use for laboratory simulation climate in the step (3)
In case the temperature range of setting be 20 DEG C -40 DEG C, humidity range be 30%-60%；And simulation climate case inside and external rings
There is fine gas exchange in border.
6. construction method according to claim 1, it is characterised in that：Solvent evaporation mechanism in the step (3) is profit
Effect with simulation climate case carries out self assembly to induce the ultra-pure water in gold nanorods colloidal sol in silicon chip surface volatilization, so that
Obtain SERS substrates.
7. a kind of SERS substrates of construction method formation as claimed in claim are used for the SERS detection methods of drugs, its feature
It is：Step is as follows：
(1) human body fluid consumed illegal drugs is taken, organic solvent is added and is extracted, then extract is centrifuged, takes its organic
Layer solution；
(2) organic layer solution is added drop-wise in SERS substrates, SERS detections is carried out using Portable Raman spectrometer.
8. SERS detection methods according to claim 1, it is characterised in that：Human body fluid is urine in the step (1)；
The organic solvent is one kind in alcohols or ketone, and the addition of organic solvent is to add 0.2- per in 0.8mL human body fluids
0.6mL。
9. SERS detection methods according to claim 1, it is characterised in that：Drugs in human body fluid in the step (1)
Including amphetamine, cocaine, m orphine, codeine, hydrochloric acid opium poppy alkali, barbiturates, hemp, THC, narcotine,
Caffeine, ketalar, Sauteralgyl, methadone, Clozapine, diphenoxylate, caffeine, totokaine, stable, propax
Fixed, surazepam, librium, Xanax, triazole storehouse, Lorazepam or fenfluramine.
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| CN109534317A (en) * | 2017-09-21 | 2019-03-29 | 中国科学院物理研究所 | A kind of preparation method of carbon nano-tube film |
| CN113275583A (en) * | 2021-05-11 | 2021-08-20 | 安徽大学 | Preparation method and detection method of SERS substrate for pesticide residues |
| CN113866154A (en) * | 2021-10-25 | 2021-12-31 | 福建师范大学 | Method for identifying cancer lesion by SERS wet method |
| CN114226743A (en) * | 2021-10-08 | 2022-03-25 | 西安邮电大学 | Preparation method of island film-shaped nano cubic array structure |
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| CN106053426A (en) * | 2016-05-13 | 2016-10-26 | 中国科学院合肥物质科学研究院 | Method for detecting drugs in human body fluids based on surface enhanced Raman spectrum technology |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534317A (en) * | 2017-09-21 | 2019-03-29 | 中国科学院物理研究所 | A kind of preparation method of carbon nano-tube film |
| CN109534317B (en) * | 2017-09-21 | 2021-11-23 | 中国科学院物理研究所 | Preparation method of carbon nanotube film |
| CN113275583A (en) * | 2021-05-11 | 2021-08-20 | 安徽大学 | Preparation method and detection method of SERS substrate for pesticide residues |
| CN113275583B (en) * | 2021-05-11 | 2022-07-01 | 安徽大学 | Preparation method and detection method of SERS substrate for pesticide residues |
| CN114226743A (en) * | 2021-10-08 | 2022-03-25 | 西安邮电大学 | Preparation method of island film-shaped nano cubic array structure |
| CN114226743B (en) * | 2021-10-08 | 2023-11-21 | 西安邮电大学 | Preparation method of island film-shaped nano cubic array structure |
| CN113866154A (en) * | 2021-10-25 | 2021-12-31 | 福建师范大学 | Method for identifying cancer lesion by SERS wet method |
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