CN111060645A - SERS detection method for adulterated drugs - Google Patents
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Abstract
The invention provides a drug-doped SERS detection method, which can integrate separation and detection, is simple and convenient to operate, has high detection speed, high sensitivity and good specificity, and overcomes the defects of complex pretreatment process, long analysis period, high detection cost and the like of the traditional detection method.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to a drug-doped SERS detection method.
Background
The drugs are in various types, and especially, the artificially synthesized drugs often contain more byproducts and intermediate products, and even contain a large amount of additives and doping substances. Drugs generally do not exist in pure form, and the rapid and effective separation and detection method has important significance for controlling abuse and prevalence of drugs.
At present, the national drug detection standard methods are gas phase-mass spectrometry (GC-MS) and liquid phase-mass spectrometry (LC-MS), and the detection methods need large instruments, have long detection time and complex process, need professional operation, and have defects in the aspects of on-site and rapid drug detection. The common drug detection methods include a chemical method and an immunological method, and the methods have high false positive and are generally only suitable for preliminary screening in a laboratory.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the drug-doped SERS detection method, which can integrate separation and detection, is simple and convenient to operate, high in detection speed, high in sensitivity and good in specificity, and overcomes the defects of complex pretreatment process, long analysis period, high detection cost and the like in the traditional detection method.
The invention provides a drug-doped SERS detection method, which comprises the following steps:
(1) spotting the standard solution on a comparison thin-layer plate, spreading the standard solution by using a developing agent, spraying a color-developing agent to obtain a specific shift value Rf of the standard solution, marking a position point which is the same as the specific shift value Rf of the standard solution on a sample thin-layer plate made of the same material as the comparison thin-layer plate according to the specific shift value Rf of the standard solution, and spraying the color-developing agent and a reinforcing agent on the position point;
(2) and (3) spotting the sample solution doped with the drugs on a sample thin-layer plate, spreading the sample solution by using the same developing agent, detecting the sample solution at the position point where the color is developed by using a Raman spectrometer, and collecting and obtaining an SERS spectrum of the drugs contained in the doped drugs.
Preferably, the standard solution is a standard solution of methamphetamine, 3, 4-methylenedioxymethamphetamine, morphine and cocaine, and the concentration of the standard solution is preferably 5-10 wt%.
Preferably, the thin-layer plate is a homemade thin-layer plate, which is obtained by the following method: mixing 1 part of kaolin and 2-5 parts of polyvinyl alcohol aqueous solution with the content of 0.5-1.5 wt% according to the parts by weight, uniformly grinding, uniformly coating on a PVC plastic plate, drying in the shade, and baking at the temperature of 110-120 ℃ for 40-60min to obtain the self-made thin-layer plate.
Preferably, the developing solvent is a mixed solvent of chloroform, water and ethyl acetate with the volume ratio of 5-7:1.5-2.5: 0.5-1.5.
Preferably, the color developing agent is 0.5-1.5 wt% iodine chloroform solution or mixed solution of butyraldehyde liquid and concentrated sulfuric acid with volume ratio of 1:8-12, wherein the content of butyraldehyde liquid is 25-35 wt%.
Preferably, the color developing agent adopted by the standard solution after the standard solution is spread on the thin layer plate is 0.5-1.5 wt% of iodine in chloroform solution, and the color developing agent adopted by the sample solution after the sample solution is spread on the thin layer plate is butyraldehyde-concentrated sulfuric acid mixed solution.
Preferably, the enhancing agent is obtained by: uniformly mixing 80-100 parts of ultrapure water and 1-2 parts of chloroauric acid solution with the content of 0.8-1.5 wt% according to the volume parts, heating to boil, adding 5 parts of sodium citrate solution with the content of 0.8-1.5 wt%, and continuously heating for 30-60min to obtain the reinforcing reagent.
Preferably, the spraying of the enhancing agent is achieved by a spin coating method, which specifically comprises: dripping the reinforced sol at corresponding position, spreading to form uniform film layer, and drying at 70-90 deg.C to remove excessive solvent.
Preferably, the laser power of the Raman spectrometer is 200-300mW, and the integration time is 5-10 s.
The invention also provides an integrated SERS sensor for separation and detection of the doped drugs, which comprises a sample thin layer plate and a Raman spectrometer, wherein position points with the same specific displacement value Rf as the standard sample are marked on the sample thin layer plate, and a color developing agent and an enhancing reagent are sprayed on each position point;
when the method is used for detection, a sample solution doped with drugs is spotted on a sample thin-layer plate, and is spread by a spreading agent, a Raman spectrometer is used for detecting at a developing position, and an SERS spectrum of the drugs contained in the doped drugs is acquired.
Compared with the prior art, the invention has the following advantages:
(1) the Surface-Enhanced Raman Scattering (SERS) technology is introduced, the method has the advantages of excellent reproducibility, rapidness, in-situ performance, water interference resistance and nondestructive detection, meanwhile, the SERS does not have the separation capability, the complex sample can be simply, rapidly and effectively separated by introducing the thin-layer chromatography, and finally, the detection method integrating separation and detection is obtained.
(2) The thin-layer plate is a self-made thin-layer plate, and the chromatographic plate is a PVC plastic plate, so that the thin-layer plate is small in volume, light in weight and convenient to carry; the prepared material uses kaolin and polyvinyl alcohol, so that the preparation cost is low and the universality is high; the characteristic makes it suitable for quick batch detection on site.
(3) The whole separation and detection processing process is about 5-10 minutes, the mixture can be quickly and effectively separated, and the method has the characteristics of high sensitivity, no damage, fingerprint identification, small sample consumption, high detection speed and the like.
Drawings
FIG. 1 shows the SERS spectrum of methamphetamine contained in the adulterant of example 1.
Detailed Description
Example 1
Self-making a thin-layer plate: selecting a PVC plastic plate with the thickness of 18cm multiplied by 20cm, cleaning and drying for later use; mixing 1 part by weight of kaolin and 3 parts by weight of 1 wt% polyvinyl alcohol aqueous solution, fully and uniformly grinding, then coating the mixture on the PVC plastic plate, lightly shaking and uniformly spreading the mixture, and drying the mixture in the shade; drying the dried chromatographic plate in the shade in a 120 ℃ oven for 50 min; cooling to room temperature, cutting into two parts, drying and storing;
enhancing the reagent: uniformly mixing 90mL of ultrapure water and 1.5mL of 1 wt% chloroauric acid solution, heating to boil, adding 5mL of 1 wt% sodium citrate solution, continuing to heat for 40min to stop reaction, and cooling for later use;
formaldehyde-concentrated sulfuric acid solution: adding 1mL of 30 wt% butyraldehyde solution into 10mL of concentrated sulfuric acid, and mixing;
standard solution: respectively preparing standard substance solutions of methamphetamine, 3, 4-methylenedioxymethamphetamine (MDMA), morphine and cocaine with the concentrations of 5-10 wt%;
sample solution to be tested for adulteration of drugs: adding a small amount of glucose and caffeine into 1mL of 1ppm methamphetamine solution to obtain a sample solution to be tested, wherein the sample solution is doped with drugs;
a drug-doped SERS detection method comprises the following steps:
(1) drawing an initial line at 1-2cm of the self-made thin-layer chromatographic plate by using a pencil, drawing 4 sampling points (every 1.2cm) on the initial line, and drawing a termination line at 15cm of the initial line; respectively dripping 1 mu L of a standard solution of methamphetamine, 3, 4-methylenedioxymethamphetamine, morphine and cocaine on the sampling points at 4 sampling points by using a capillary tube, putting a chromatographic plate into a sealable vessel containing 20mL of a developing agent chloroform-water-ethyl acetate (volume ratio is 6:2:1), and taking out the developing agent after the developing agent rises to a stop line; spraying a chloroform solution of 1% iodine for color development, and recording the distance from a color development spot to an initial line;
(2) drawing a starting line, a stopping line and a sampling point at the same position by taking the self-made thin-layer chromatographic plate; making a round mark point with the diameter of 0.5mm on the thin-layer chromatographic plate according to the spot position of a methamphetamine, MDMA, morphine and cocaine standard product, adding 0.05mL of prepared formaldehyde-concentrated sulfuric acid solution as a color developing agent into the mark spot, dripping a reinforcing reagent on the mark point after air drying, spreading the mark point into a uniform film layer at a low speed by using a spin coater, and drying at 80 ℃ to remove redundant solvent, thus spin-coating the reinforcing reagent on the mark point; dripping 1 mu L of the drug-doped sample solution to be detected on a sampling point by using a capillary tube, putting a sample system plate into 20mL of developing agent chloroform-water-ethyl acetate (6:2:1), taking out the sample system plate after the developing agent rises to a termination line, drying the sample system plate, and preliminarily judging that the sample system plate contains methamphetamine, wherein reddish brown spots appear at the methamphetamine marking point of the sample system plate; and detecting the blue-violet spot by using a handheld Raman spectrometer, and acquiring an SERS spectrum under the conditions that the integration time is 5s, the laser power is 250mW and the excitation wavelength is 785nm, wherein the characteristic peak of the methamphetamine is obtained as shown in figure 1.
Example 2
Self-making a thin-layer plate: selecting a PVC plastic plate with the thickness of 18cm multiplied by 20cm, cleaning and drying for later use; mixing 1 part by weight of kaolin and 3 parts by weight of 1 wt% polyvinyl alcohol aqueous solution, fully and uniformly grinding, then coating the mixture on the PVC plastic plate, lightly shaking and uniformly spreading the mixture, and drying the mixture in the shade; drying the dried chromatographic plate in the shade in a 120 ℃ oven for 50 min; cooling to room temperature, cutting into two parts, drying and storing;
enhancing the reagent: uniformly mixing 90mL of ultrapure water and 1.5mL of 1 wt% chloroauric acid solution, heating to boil, adding 5mL of 1 wt% sodium citrate solution, continuing to heat for 40min to stop reaction, and cooling for later use;
formaldehyde-concentrated sulfuric acid solution: adding 1mL of 30 wt% butyraldehyde solution into 10mL of concentrated sulfuric acid, and mixing;
standard solution: respectively preparing standard substance solutions of methamphetamine, 3, 4-methylenedioxymethamphetamine (MDMA), morphine and cocaine with the concentrations of 5-10 wt%;
sample solution to be tested for adulteration of drugs: adding a small amount of starch and caffeine into 1mL of 1ppm MDMA solution to obtain a sample solution to be tested, wherein the sample solution is doped with drugs;
a drug-doped SERS detection method comprises the following steps:
(1) drawing an initial line at 1-2cm of the self-made thin-layer chromatographic plate by using a pencil, drawing 4 sampling points (every 1.2cm) on the initial line, and drawing a termination line at 15cm of the initial line; respectively dripping 1 mu L of a standard solution of methamphetamine, 3, 4-methylenedioxymethamphetamine, morphine and cocaine on the sampling points at 4 sampling points by using a capillary tube, putting a chromatographic plate into a sealable vessel containing 20mL of a developing agent chloroform-water-ethyl acetate (volume ratio is 6:2:1), and taking out the developing agent after the developing agent rises to a stop line; spraying a chloroform solution of 1% iodine for color development, and recording the distance from a color development spot to an initial line;
(2) drawing a starting line, a stopping line and a sampling point at the same position by taking the self-made thin-layer chromatographic plate; making a circular mark point with the diameter of 0.5mm on the thin-layer chromatographic plate according to the spot position of a methamphetamine, MDMA, morphine and cocaine standard product, dripping 0.1mL of prepared formaldehyde-concentrated sulfuric acid solution as a color developing agent on the mark point, dripping a reinforcing reagent on the mark point after air drying, spreading the reinforcing reagent into a uniform film layer at a low speed by using a spin coater, drying at 80 ℃ to remove redundant solvent, and thus spin-coating the reinforcing reagent on the mark point; dripping 1 mu L of the sample solution of the adulterant to be detected on a sample point by using a capillary, putting a sample system plate into 20mL of developing agent chloroform-water-ethyl acetate (6:2:1) until the developing agent rises to a termination line, taking out, airing, and primarily judging that the MDMA is contained, wherein a blue-purple spot appears at an MDMA mark point of the sample plate; and detecting the blue-violet spots by using a handheld Raman spectrometer, and acquiring an SERS spectrum under the conditions that the integration time is 5s and the laser power is 250mW, so that the characteristic peak of the MDMA is obtained.
Example 3
Self-making a thin-layer plate: selecting a PVC plastic plate with the thickness of 18cm multiplied by 20cm, cleaning and drying for later use; mixing 1 part by weight of kaolin and 2 parts by weight of 1.5 wt% of polyvinyl alcohol aqueous solution, fully and uniformly grinding, then coating the mixture on the PVC plastic plate, lightly shaking and uniformly spreading the mixture, and drying the mixture in the shade; drying the dried chromatographic plate in the shade in a drying oven at 110 ℃ for 60 min; cooling to room temperature, cutting into two parts, drying and storing;
enhancing the reagent: uniformly mixing 80mL of ultrapure water and 2mL of chloroauric acid solution with the content of 0.8 wt%, heating to boil, adding 5mL of sodium citrate solution with the content of 1.5 wt%, continuing to heat for 30min to stop reaction, and cooling for later use;
formaldehyde-concentrated sulfuric acid solution: adding 1mL of 25 wt% butyraldehyde solution into 12mL of concentrated sulfuric acid, and mixing to obtain the product;
standard solution: respectively preparing standard substance solutions of methamphetamine, 3, 4-methylenedioxymethamphetamine (MDMA), morphine and cocaine with the concentrations of 5-10 wt%;
sample solution to be tested for adulteration of drugs: adding a small amount of ibuprofen and rock candy into 1mL of 1ppm morphine solution to obtain a sample solution to be tested, wherein the sample solution is doped with drugs;
a drug-doped SERS detection method comprises the following steps:
(1) drawing an initial line at 1-2cm of the self-made thin-layer chromatographic plate by using a pencil, drawing 4 sampling points (every 1.2cm) on the initial line, and drawing a termination line at 15cm of the initial line; dripping 1 mu L of standard solutions of methamphetamine, 3, 4-methylenedioxymethamphetamine, morphine and cocaine on the sampling points at 4 sampling points respectively by using a capillary tube, putting a chromatographic plate into a sealable vessel containing 20mL of developing agent chloroform-water-ethyl acetate (volume ratio is 5:2.5:0.5), and taking out the developing agent after the developing agent rises to a stop line; spraying a chloroform solution of 1% iodine for color development, and recording the distance from a color development spot to an initial line;
(2) drawing a starting line, a stopping line and a sampling point at the same position by taking the self-made thin-layer chromatographic plate; making a round mark point with the diameter of 0.5mm on the thin-layer chromatographic plate according to the spot position of a methamphetamine, MDMA, morphine and cocaine standard product, adding 0.05mL of prepared formaldehyde-concentrated sulfuric acid solution as a color developing agent into the mark spot, dripping a reinforcing reagent on the mark point after air drying, spreading the mark point into a uniform film layer at a low speed by using a spin coater, and drying at 70 ℃ to remove redundant solvent, thus spin-coating the reinforcing reagent on the mark point; dripping 1 mu L of the to-be-detected drug-doped sample solution into a sample point by using a capillary, putting a sample system plate into 20mL of developing agent chloroform-water-ethyl acetate (5:2.5:0.5), taking out the developing agent after the developing agent rises to a termination line, drying the developing agent, and preliminarily judging that morphine is contained, wherein reddish brown spots appear at morphine marking points of the sample plate; and detecting the purple red spots by using a handheld Raman spectrometer, and acquiring an SERS spectrum under the conditions that the integration time is 5s and the laser power is 300mW, wherein the characteristic peak of morphine is obtained by referring to the graph shown in FIG. 1.
Example 4
Self-making a thin-layer plate: selecting a PVC plastic plate with the thickness of 18cm multiplied by 20cm, cleaning and drying for later use; mixing 1 part by weight of kaolin and 5 parts by weight of 0.5 wt% polyvinyl alcohol aqueous solution, fully and uniformly grinding, then coating the mixture on the PVC plastic plate, lightly shaking and uniformly spreading the mixture, and drying the mixture in the shade; drying the dried chromatographic plate in the shade in a 120 ℃ oven for 40 min; cooling to room temperature, cutting into two parts, drying and storing;
enhancing the reagent: uniformly mixing 100mL of ultrapure water and 1mL of chloroauric acid solution with the content of 1.5 wt%, heating to boil, adding 5mL of sodium citrate solution with the content of 0.8 wt%, continuing to heat for 60min to stop reaction, and cooling for later use;
formaldehyde-concentrated sulfuric acid solution: adding 1mL of 35 wt% butyraldehyde solution into 8mL of concentrated sulfuric acid, and mixing;
standard solution: respectively preparing standard substance solutions of methamphetamine, 3, 4-methylenedioxymethamphetamine (MDMA), morphine and cocaine with the concentrations of 5-10 wt%;
sample solution to be tested for adulteration of drugs: adding a small amount of magnesium sulfate and starch into 1mL of 1ppm cocaine solution to obtain a sample solution to be tested, wherein the sample solution is doped with drugs;
a drug-doped SERS detection method comprises the following steps:
(1) drawing an initial line at 1-2cm of the self-made thin-layer chromatographic plate by using a pencil, drawing 4 sampling points (every 1.2cm) on the initial line, and drawing a termination line at 15cm of the initial line; dripping 1 mu L of standard solutions of methamphetamine, 3, 4-methylenedioxymethamphetamine, morphine and cocaine on the sampling points at 4 sampling points respectively by using a capillary tube, putting a chromatographic plate into a sealable vessel containing 20mL of developing agent chloroform-water-ethyl acetate (volume ratio is 7:1.5:1.5), and taking out the developing agent after the developing agent rises to a stop line; spraying a chloroform solution of 1% iodine for color development, and recording the distance from a color development spot to an initial line;
(2) drawing a starting line, a stopping line and a sampling point at the same position by taking the self-made thin-layer chromatographic plate; making a circular mark point with the diameter of 0.5mm on the thin-layer chromatographic plate according to the spot position of a methamphetamine, MDMA, morphine and cocaine standard product, dripping 0.1mL of prepared formaldehyde-concentrated sulfuric acid solution as a color developing agent on the mark point, dripping a reinforcing reagent on the mark point after air drying, spreading the reinforcing reagent into a uniform film layer at a low speed by using a spin coater, drying at 90 ℃ to remove redundant solvent, and thus spin-coating the reinforcing reagent on the mark point; dripping 1 mu L of the drug-doped sample solution to be detected on a sample point by using a capillary tube, putting a sample system plate into 20mL of developing agent chloroform-water-ethyl acetate (7:1.5:1.5), taking out the sample system plate until the developing agent rises to a termination line, airing the sample system plate, and preliminarily judging that the sample system plate contains cocaine, wherein reddish brown spots appear at cocaine marking points of the sample system plate; and detecting the yellowish-red spots by using a handheld Raman spectrometer, and acquiring an SERS spectrum under the conditions that the integration time is 10s and the laser power is 200mW, so that the characteristic peak of the cocaine is obtained.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications thereof should be included in the technical scope of the present invention.
Claims (9)
1. The SERS detection method for the doped drugs is characterized by comprising the following steps:
(1) spotting the standard solution on a comparison thin-layer plate, spreading the standard solution by using a developing agent, spraying a color-developing agent to obtain a specific shift value Rf of the standard solution, marking a position point which is the same as the specific shift value Rf of the standard solution on a sample thin-layer plate made of the same material as the comparison thin-layer plate according to the specific shift value Rf of the standard solution, and spraying the color-developing agent and a reinforcing agent on the position point;
(2) and (3) spotting the sample solution doped with the drugs on a sample thin-layer plate, spreading the sample solution by using the same developing agent, detecting the sample solution at the position point where the color is developed by using a Raman spectrometer, and collecting and obtaining an SERS spectrum of the drugs contained in the doped drugs.
2. The method for SERS detection of doped drugs according to claim 1, wherein the standard solution is a standard solution of methamphetamine, 3, 4-methylenedioxymethamphetamine, morphine, cocaine, preferably with a concentration of 5-10 wt%.
3. The drug-doped SERS detection method according to claim 1 or 2, wherein the thin-layer plate is a self-made thin-layer plate and is obtained by the following method: mixing 1 part of kaolin and 2-5 parts of polyvinyl alcohol aqueous solution with the content of 0.5-1.5 wt% according to the parts by weight, uniformly grinding, uniformly coating on a PVC plastic plate, drying in the shade, and baking at the temperature of 110-120 ℃ for 40-60min to obtain the self-made thin-layer plate.
4. The drug-doped SERS detection method according to any one of claims 1 to 3, wherein the developing solvent is a mixed solvent of chloroform, water and ethyl acetate in a volume ratio of 5-7:1.5-2.5: 0.5-1.5.
5. The method for SERS detection of doped drugs according to any one of claims 1 to 4, wherein the color developer is 0.5 to 1.5 wt% iodine in chloroform or a mixed solution of butyraldehyde solution and concentrated sulfuric acid in a volume ratio of 1:8 to 12, wherein the content of butyraldehyde solution is 25 to 35 wt%.
6. The method for SERS detection of doped drugs according to claim 5, wherein the color developing agent adopted by the standard solution after being spread on the thin layer plate is 0.5-1.5 wt% iodine solution in chloroform, and the color developing agent adopted by the sample solution after being spread on the thin layer plate is butyraldehyde-concentrated sulfuric acid mixed solution.
7. The method for SERS detection of doped drugs according to any of claims 1 to 6, wherein the enhancing reagent is obtained by: uniformly mixing 80-100 parts by volume of ultrapure water and 1-2 parts by volume of a chloroauric acid solution with the content of 0.8-1.5 wt%, heating to boil, adding 5 parts by volume of a sodium citrate solution with the content of 0.8-1.5 wt%, and continuously heating for 30-60min to obtain the reinforcing reagent; preferably, the spraying of the enhancing agent is achieved by a spin coating method, which specifically comprises: dripping the reinforced sol at corresponding position, spreading to form uniform film layer, and drying at 70-90 deg.C to remove excessive solvent.
8. The method for SERS detection of doped drugs as recited in any one of claims 1-7, wherein the laser power of the Raman spectrometer is 200-300mW, and the integration time is 5-10 s.
9. The SERS sensor integrating the separation and detection of the doped drugs is characterized by comprising a sample thin layer plate and a Raman spectrometer, wherein position points with the same specific displacement value Rf as a standard sample are marked on the sample thin layer plate, and a color developing agent and an enhancing reagent are sprayed on each position point;
when the method is used for detection, a sample solution doped with drugs is spotted on a sample thin-layer plate, and is spread by a spreading agent, a Raman spectrometer is used for detecting at a developing position, and an SERS spectrum of the drugs contained in the doped drugs is acquired.
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Application publication date: 20200424 |