CN111398249A - Method for rapidly detecting drugs on site - Google Patents

Method for rapidly detecting drugs on site Download PDF

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Publication number
CN111398249A
CN111398249A CN202010355570.8A CN202010355570A CN111398249A CN 111398249 A CN111398249 A CN 111398249A CN 202010355570 A CN202010355570 A CN 202010355570A CN 111398249 A CN111398249 A CN 111398249A
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China
Prior art keywords
substrate
sample
sol
drugs
prepared
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CN202010355570.8A
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Chinese (zh)
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粟勇
袁丁
吴红彦
夏征
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Beijing Htnova Detection Technology Co ltd
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Beijing Htnova Detection Technology Co ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • 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
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The invention provides a method for rapidly detecting drugs on site, which comprises the following steps: step 1, synthesizing metal nano sol: preparing metal nano sol by adopting a method of reducing metal ions by using a reducing agent; step 2, preparation of an activity enhancement substrate: dispersing the metal nano sol prepared in the step 1 on a substrate, and preparing an activity enhancement substrate by adopting a circulating dispersion-drying method; step 3, preparation of an active substrate to which the sample is attached: dispersing a sample on the activity enhancement substrate prepared in the step 2 to prepare an active substrate attached with the sample; step 4, sample detection: and (4) detecting the active substrate attached with the sample prepared in the step (3) by adopting a Raman spectrometer to obtain a result. The method adopts the chemically synthesized nano-particle sol with lower cost to rapidly prepare the substrate for detection on site, adopts a simpler and more convenient circulating dispersion-drying mode to prepare the active substrate, and is easy to operate.

Description

Method for rapidly detecting drugs on site
Technical Field
The invention relates to the technical field of surface-enhanced Raman spectroscopy detection, in particular to a method and equipment for rapidly detecting drugs on site by adopting the surface-enhanced Raman spectroscopy technology.
Background
Raman spectroscopy (Raman spectroscopy), is a scattering spectrum. The Raman spectroscopy is an analysis method for analyzing a scattering spectrum with a frequency different from that of incident light to obtain information on molecular vibration and rotation based on a Raman scattering effect found by indian scientists c.v. Raman (man), and is applied to molecular structure research.
The vibration and rotation energy level of the substance can be known through the analysis of the Raman spectrum, so that the substance can be identified and the property of the substance can be analyzed. Currently, raman spectroscopy is widely used in the fields of jewelry identification, archaeology, medicine, customs inspection, drug identification, and the like. As most drugs are micromolecular organic matters and Raman spectrum signals exist generally, the drugs can be identified by adopting a Raman spectrum technology, so that the most direct law enforcement basis is provided for law enforcement personnel.
Generally, a portable laser raman spectrometer with a wavelength of 785nm is mostly used as a laser light source, however, when the raman spectrometer with the wavelength is used for detecting drugs, the raman spectrometer with the wavelength is easily interfered by fluorescence signals of some drugs, like heroin which is one of the most common drugs, and the raman spectrometer with the laser light source with the wavelength of 785nm is difficult to detect due to the interference of the fluorescence signals of the drugs. Fentanyl and magical have the same problems except for heroin. Therefore, for the detection of drugs with strong fluorescence signals, a Surface Enhanced Raman Scattering (SERS) method is mostly adopted at present.
The SERS technology for testing drugs is mostly a method using an active substrate, and generally a silicon wafer or a metal material is used as a substrate to prepare an active enhanced substrate. The method has relatively high requirements on synthesis conditions and methods, and the prepared enhanced substrate has poor stability, short service life and high test cost. And for a specific reinforced substrate, the reinforcing effect is fixed, and the detection effect of different samples has certain difference.
Therefore, a method for detecting drugs by using the surface enhanced raman spectroscopy, which has low cost, adjustable enhancement effect and convenient and rapid field use, is urgently needed.
Disclosure of Invention
The invention aims to solve the problems and the defects, provides a method for rapidly detecting drugs on site by adopting a surface-enhanced Raman spectroscopy technology, avoids the problems of poor stability of a substrate, fixed enhancement effect and inconvenient storage, and has low manufacturing cost and better enhancement test effect.
According to an aspect of the present invention, there is provided a method for rapidly detecting drugs on site, comprising:
step 1, synthesizing metal nano sol: preparing metal nano sol by adopting a method of reducing metal ions by using a reducing agent;
step 2, preparation of an activity enhancement substrate: dispersing the metal nano sol prepared in the step 1 on a substrate, and preparing an activity enhancement substrate by adopting a circulating dispersion-drying method, wherein the circulating times can be flexibly selected;
step 3, preparation of an active substrate to which the sample is attached: dispersing the sample on the activity enhancement substrate prepared in the step 2 to prepare an active substrate attached with the sample;
step 4, sample detection: and (4) detecting the active substrate attached with the sample prepared in the step (3) by adopting a Raman spectrometer to obtain a result.
In the step 1, silver nitrate is dissolved in water, heated and refluxed, a reducing agent sodium citrate is added, refluxed for 40min, and cooled to room temperature to synthesize silver nano sol.
Or, in the step 1, dissolving chloroauric acid in water, heating and refluxing, adding a reducing agent sodium citrate, refluxing for 40min, cooling to room temperature, and synthesizing gold nano sol.
In step 2, dispersing the metal nano sol on a substrate without enhanced activity, and drying; dispersing the metal nano sol on the dried substrate again, and drying; the above dispersion-drying process is repeated to produce the activity-enhanced substrate.
In the step 3, dissolving a sample to be detected in a solvent to prepare a sample solution; and (3) dispersing the sample solution prepared in the step (3) on the activity enhancement substrate prepared in the step (2), taking out and drying to prepare the active substrate attached with the sample.
Or, in step 3, after the active substrate is wetted in the solvent, the solid sample is dipped and dried, and the active substrate attached with the sample is prepared.
The solvent comprises one or more of water, methanol, ethanol and acetone.
The dispersion mode in step 2 and step 3 is selected from one or more of immersion, smearing, spraying and dropping.
In step 4, the parameters of raman spectrum acquisition are set as: excitation wavelength of 785nm, power of 150mW, and scanning range of 300cm-1～2500cm-1Integration time 4 s.
In the step 1, a centrifugal method is adopted to concentrate the nano metal sol by 5-10 times. Or the mass ratio of reactants is adjusted, and the concentration of the nano metal sol is increased to 5-10 times of the original concentration.
Compared with the prior art, the invention has the beneficial effects that:
1) the method adopts the chemically synthesized nano-particle sol with lower cost to rapidly prepare the substrate for detection on site, adopts a simpler and more convenient circulating immersion-drying mode to prepare the active substrate, and is easy to operate; and the enhancing effect of the active substrate can be adjusted by adjusting the cycle number;
2) the method has high reliability of the detection result of the drugs with strong fluorescent signals, and can particularly realize the rapid detection of the drugs with strong fluorescent signals such as heroin, fentanyl and the like;
3) the method has the advantages of wide sampling range and accurate detection.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart illustrating a method for rapidly detecting drugs on site according to an embodiment of the present invention;
FIG. 2 is a photograph of activity enhancement test strips with different immersion-drying times;
FIG. 3 shows the enhancement effect of activity enhancing test paper on heroin for different immersion-drying times;
figure 4 enhancement of fentanyl by silver nanoagents at different concentrations.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments of the present invention may be arbitrarily combined with each other without conflict.
The invention provides a method for rapidly detecting drugs on site, which comprises the following steps:
step 1, synthesizing metal nano sol: preparing metal nano sol by adopting a method of reducing metal ions by using a reducing agent;
step 2, preparation of an activity enhancement substrate: dispersing the metal nano sol prepared in the step 1 on a substrate, and preparing an activity enhancement substrate by adopting a circulating dispersion-drying method;
step 3, preparation of an active substrate to which the sample is attached: dispersing the sample on the activity enhancement substrate prepared in the step 2 to prepare an active substrate attached with the sample;
step 4, sample detection: and (4) detecting the active substrate attached with the sample prepared in the step (3) by adopting a Raman spectrometer to obtain a result.
In the step 1, silver nitrate is dissolved in water, heated and refluxed, a reducing agent sodium citrate is added, refluxed for 40min, and cooled to room temperature to synthesize silver nano sol.
Or, in the step 1, dissolving chloroauric acid in water, heating and refluxing, adding a reducing agent sodium citrate, refluxing for 40min, cooling to room temperature, and synthesizing gold nano sol.
In step 2, dispersing the metal nano sol on a substrate without enhanced activity, and drying; dispersing the metal nano sol on the dried substrate again, and drying; the above dispersion-drying process is repeated to produce the activity-enhanced substrate.
In the step 3, dissolving a sample to be detected in a solvent to prepare a sample solution; and (3) dispersing the sample solution prepared in the step (3) on the activity enhancement substrate prepared in the step (2), taking out and drying to prepare the active substrate attached with the sample.
Or, in step 3, after the active substrate is wetted in the solvent, the solid sample is dipped and dried, and the active substrate attached with the sample is prepared.
The solvent comprises one or more of water, methanol, ethanol and acetone.
The dispersion mode in step 2 and step 3 is selected from one or more of immersion, smearing, spraying and dropping.
In step 4, the parameters of raman spectrum acquisition are set as: excitation wavelength of 785nm, power of 150mW, and scanning range of 300cm-1～2500cm-1Integration time 4 s.
In the step 1, a centrifugal method is adopted to concentrate the nano metal sol by 5-10 times; or the mass ratio of reactants is adjusted, and the concentration of the nano metal sol is increased to 5-10 times of the original concentration.
Example one
Taking a silver active substrate as an example, the sol dispersion mode adopts immersion, and the operation method of the invention is shown in figure 1:
step 1, synthesizing silver nano sol, namely synthesizing the silver nano sol by adopting a method of reducing silver nitrate with sodium citrate, weighing 17mg of silver nitrate solid, dissolving the silver nitrate solid in 100m L of water, heating the silver nitrate solid to 110 ℃ by adopting an oil bath, refluxing, measuring 2m L of sodium citrate water solution with the mass fraction of 1%, adding the sodium citrate water solution into a reaction system at one time, continuously refluxing and reacting for 40min, removing the reaction system from an oil bath pot, naturally cooling the reaction system to room temperature, and preparing gray-green silver nano sol.
Step 2, preparation of an activity enhancement substrate: an activity-enhancing substrate was prepared using a repeated immersion-drying process. Immersing the substrate without enhanced activity in the silver sol for 5 seconds, and taking out and drying; immersing the dried substrate in the silver sol for 5 seconds, and taking out and drying; the above immersion-drying process was repeated to obtain an activated silver enhanced substrate.
The substrate used in this step includes, but is not limited to, rough-surface porous materials such as ground glass, silica gel plate, chromatography paper, filter paper, printing paper, kraft paper, and the like.
Step 3, preparation of an active substrate to which the sample is attached: the sampling is also carried out in an immersion mode. Firstly, dissolving a sample to be detected in a solvent, putting the activity enhancement substrate prepared in the step 2 into a sample solution, immersing for 5 seconds, taking out and drying to obtain the active substrate attached with the sample.
The solvent used in this step includes, but is not limited to, water, methanol, ethanol, acetone.
Step 4, sample detection: and (4) detecting the active substrate attached with the sample prepared in the step (3) by adopting a Raman spectrometer to obtain a result.
Wherein, the parameters of Raman spectrum collection are set as follows: the excitation wavelength is 785nm, the power is 150mW, the scanning range is 300cm < -1 > to 2500cm < -1 >, and the integration time is 4 s.
Example two: test effect of different repeated immersion-drying times on heroin
Step 1, synthesizing silver nano sol, namely synthesizing the silver nano sol by adopting a method of reducing silver nitrate with sodium citrate, weighing 17mg of silver nitrate solid, dissolving the silver nitrate solid in 100m L water, heating the silver nitrate solid to 110 ℃ by adopting an oil bath, refluxing, weighing 2m L of sodium citrate water solution with the mass fraction of 1%, adding the sodium citrate water solution into a reaction system at one time, continuously refluxing and reacting for 40min, removing the reaction system from an oil bath, and naturally cooling the reaction system to room temperature to prepare the gray-green silver nano sol.
Step 2, preparation of an activity enhancement substrate: an activity-enhancing substrate was prepared using a repeated immersion-drying process. Immersing the filter paper without enhanced activity in the silver sol for 5 seconds, and taking out and drying to obtain an enhanced substrate subjected to immersion-drying once; the above operations were repeated to obtain the reinforced substrate immersed-dried twice, three times, four times, five times, respectively, as shown in fig. 2.
And 3, preparing the active substrate attached with the sample, namely, sampling in a soaking mode, soaking the enhanced substrates with different enhancement effects prepared in the step 2 in a heroin ethanol solution of 1mg/m L for 5 seconds, taking out and drying to obtain the active substrate attached with the heroin.
Step 4, sample detection: and (3) detecting the active substrate attached with the sample prepared in the step (3) by using a Raman spectrometer to obtain a result, wherein a test spectrum curve is shown as an attached figure 3.
Example three: test effect of nano sol with different concentrations on fentanyl
Step 1, synthesizing silver nano sol with different concentrations, namely synthesizing the silver nano sol by adopting a method of reducing silver nitrate with sodium citrate, respectively weighing 17mg, 34mg, 51mg, 68mg and 85mg of silver nitrate solid, dissolving the silver nitrate solid in 100m L water, heating the silver nitrate solid to 110 ℃ by adopting an oil bath, refluxing, respectively weighing sodium citrate aqueous solutions with mass fractions of 1% of 2m L, 4m L, 6m L, 8m L and 10m L, adding the sodium citrate aqueous solutions into a corresponding reaction system at one time, continuously refluxing for 40min, removing the reaction system from an oil bath pot, naturally cooling the reaction system to room temperature, and respectively preparing gray-green silver nano sol Ag1, Ag2, Ag3, Ag4 and Ag 5.
And 2, preparing the activity enhancement substrate, namely preparing the activity enhancement substrate in a dropping sample-drying mode, respectively transferring the five silver nano sols of 1 mu L obtained in the step 1, respectively dropwise adding the five silver nano sols onto 5 ground glass sheets, and drying to obtain the activity enhancement substrates with different enhancement effects.
And 3, preparing the active substrate attached with the sample, namely, sampling in a dropping mode, respectively transferring a fentanyl ethanol solution of 10mg/m L to obtain a solution with the concentration of 1 mu L, respectively dropping the solution on the 5 pieces of ground glass dropwise added with the silver nano sol in the step 2, wherein the dropping position is the same as that of the silver nano sol, and drying to obtain the active substrate attached with fentanyl.
Step 4, sample detection: and (3) detecting the active substrate attached with the sample prepared in the step (3) by using a Raman spectrometer to obtain a result, wherein a test spectrum curve of the result is shown as an attached figure 4.
The method adopts the chemically synthesized nano-particle sol with lower cost to rapidly prepare the substrate for detection on site, adopts a simpler and more convenient circulating immersion-drying mode to prepare the active substrate, has adjustable reinforcing effect and is easy to operate; the method has high reliability of the detection result of the drugs with strong fluorescent signals, and can particularly realize the rapid detection of the drugs with strong fluorescent signals such as heroin, fentanyl and the like; the method has the advantages of wide sampling range and accurate detection.
Finally, it should be noted that: in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only for illustrating the technical solutions of the present invention, and are not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for rapidly detecting drugs on site is characterized by comprising the following steps:
step 1, synthesizing metal nano sol: preparing metal nano sol by adopting a method of reducing metal ions by using a reducing agent;
step 2, preparation of an activity enhancement substrate: dispersing the metal nano sol prepared in the step 1 on a substrate, and preparing an activity enhancement substrate by adopting a circulating dispersion-drying method;
step 3, preparation of an active substrate to which the sample is attached: dispersing a sample on the activity enhancement substrate prepared in the step 2 to prepare an active substrate attached with the sample;
step 4, sample detection: and (4) detecting the active substrate attached with the sample prepared in the step (3) by adopting a Raman spectrometer to obtain a result.
2. The method for rapidly detecting drugs on site according to claim 1, wherein in step 1, silver nitrate is dissolved in water, heated and refluxed, a reducing agent sodium citrate is added, refluxed for 40min, and cooled to room temperature to synthesize the silver nano sol.
3. The method for rapidly detecting drugs on site according to claim 1, wherein in step 1, chloroauric acid is dissolved in water, heated and refluxed, a reducing agent sodium citrate is added, refluxed for 40min, and cooled to room temperature to synthesize gold nano sol.
4. The method for rapidly detecting drugs in situ according to claim 1, wherein in step 2, the metal nanosol is dispersed on a substrate without enhanced activity and dried; dispersing the metal nano sol on the dried substrate again, and drying; and (4) recycling the dispersing-drying process to obtain the activity enhancement substrate.
5. The method for rapidly detecting drugs on site according to claim 1, wherein in step 3, the sample to be detected is dissolved in a solvent to prepare a sample solution; and (3) dispersing the sample solution prepared in the step (3) on the activity enhancement substrate prepared in the step (2), taking out and drying to prepare the active substrate attached with the sample.
6. The method for rapid in-situ detection of drugs according to claim 1, wherein in step 3, the active substrate is wetted in a solvent, dipped with a solid sample, and dried to obtain the active substrate with the sample attached.
7. The method for rapid in-situ detection of drugs according to claim 5 or 6, wherein the solvent comprises one or more of water, methanol, ethanol and acetone.
8. The method for rapidly detecting drugs in situ according to claim 1, wherein the dispersion manner in steps 2 and 3 is selected from one or more of immersion, smearing, spraying and dripping.
9. The method for rapidly detecting drugs on site according to claim 1, wherein in step 4, the parameters of Raman spectrum acquisition are set as follows: excitation wavelength of 785nm, power of 150mW, and scanning range of 300cm-1～2500cm-1Integration time 4 s.
10. The method for rapidly detecting drugs on site according to claim 1, wherein in step 1, the nano metal sol is concentrated by 5-10 times by using a centrifugal method; or the mass ratio of reactants is adjusted, and the concentration of the nano metal sol is increased to 5-10 times of the original concentration.
CN202010355570.8A 2020-04-29 2020-04-29 Method for rapidly detecting drugs on site Pending CN111398249A (en)

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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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