CN112240881A - Method for rapidly detecting trace fentanyl by using Raman spectroscopy - Google Patents
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- CN112240881A CN112240881A CN202011058592.4A CN202011058592A CN112240881A CN 112240881 A CN112240881 A CN 112240881A CN 202011058592 A CN202011058592 A CN 202011058592A CN 112240881 A CN112240881 A CN 112240881A
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Abstract
The invention provides a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which obtains a detection result by comparing Raman frequency shift values with the common molecular structure characteristics of the fentanyl substances, and comprises the following steps: mixing a sample to be detected, a coagulant and a Raman sensitization substrate in a certain proportion to serve as a detection sample, and carrying out laser excitation on the detection sample by using a Raman detector to obtain Raman spectrum frequency shift data T of the sample; and comparing the obtained Raman spectrum frequency shift data T of the sample with the Raman spectrum frequency shift value of the common molecular structure characteristic of the fentanyl substance provided by the invention, and if the Raman spectrum frequency shift data T of the sample has not less than 2 Raman spectrum frequency shift values which are the same as the reference Raman spectrum frequency shift value of the common molecular structure characteristic of the fentanyl substance, judging that the sample to be detected contains trace fentanyl substance. The detection limit of the fentanyl substance in the method is 100 ng/ml.
Description
Technical Field
The invention relates to a method for rapidly detecting trace fentanyl substances by using Raman spectroscopy, which realizes rapid detection of the trace fentanyl substances by using a Raman spectroscopy surface enhancement technology.
Background
The Raman spectrum method is a detection method for rapidly and nondestructively identifying the types and the compositions of substances, so the characteristic can be suitable for various fields of chemical substance identification, public security explosion prevention, drug enforcement, customs smuggling, judicial identification and the like, and the rapid detection capability of some supervision medicines such as fentanyl and the like is brought forward in order to meet the increasing detection requirements of the supervision departments such as public security, customs and the like.
At present, the technical means used by fentanyl in judicial supervision mainly comprises methods such as colloidal gold immunochromatography, fluorescence immunochromatography gas/liquid-mass spectrometry and the like.
Compared with a colloidal gold immunochromatography method and a fluorescence immunochromatography method, the Raman spectroscopy can greatly improve the detection accuracy in the detection result based on various characteristic fingerprint spectrums corresponding to the molecular structure of the object to be detected while maintaining the rapid detection capability, and reduce the risks of false positive interference and false negative. Compared with a gas phase/liquid phase-mass spectrometry method, the Raman spectrometry method greatly reduces the detection process and the detection time while maintaining high-precision detection, and improves the detection efficiency.
The fentanyl substances are characterized by having a central chemical structure of fentanyl, the difference comes from different acyl substitutions, the difference of Raman vibration energy caused by the different acyl substitutions is very small, and the resolution and the test method of the existing spectrometer are seriously challenged to realize the simultaneous screening of 27 fentanyl substances.
Disclosure of Invention
The invention of the present application aims to: the method solves the problem of accurately performing qualitative detection on the trace fentanyl by using a Raman method, and provides the detection method for rapidly detecting the trace fentanyl substances by using the Raman spectroscopy.
In order to achieve the purpose of the invention, the following technical scheme is adopted in the application:
the invention relates to a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which comprises the following steps: the Raman spectrum detection method for detecting the molecular structure main body characteristics of trace fentanyl substances in a sample by using a one-step method comprises the following steps,
(1) diluting a 100ug/ml fentanyl standard sample with methanol as a solvent to 100ng/ml by adding a proper amount of purified water, and uniformly mixing by shaking to obtain a sample C to be detected;
(2) mixing the sample C to be detected with a Raman sensitization substrate, adding a proper amount of a coagulant, oscillating and uniformly mixing to obtain a detection sample, wherein: the ratio of the Raman sensitization substrate, the coagulant and the sample C to be detected is 1: 1 to 3: 4: 5, and a Raman detector is used for detecting the sample C to be detected to obtain Raman frequency shift spectrum data T of the sample C to be detected;
(3) and (3) comparing the Raman frequency shift spectrum data T of the detection sample obtained in the step (2) with the Raman frequency shift value of the common molecular structural feature of the fentanyl substance, and if at least 2 Raman frequency shift values in the Raman frequency shift spectrum data T of the detection sample are the same as the Raman frequency shift value of the common molecular structural feature of the fentanyl substance, determining that the detection sample contains trace amount of the fentanyl substance.
The invention relates to a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which comprises the following steps: the Raman frequency shift value of the common molecular structure characteristic of the fentanyl substance is 622cm-1、1000cm-1、1032cm-1、1160cm-1、1606cm-1。
The invention relates to a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which comprises the following steps: the fentanyl substance is: 4-fluorobutyrylfentanyl, 4-fluoroisobutyrylfentanyl, butyrylfentanyl, isobutyrylfentanyl hydrochloride, furfentanyl hydrochloride, valerylfentanyl hydrochloride, beta-hydroxythiofentanyl, cis-3-methylfentanyl hydrochloride, olfentanyl, p-fluorofentanyl, sufentanil citrate, acetylfentanyl, beta-hydroxy-3-methylfentanyl, 4-anilino-N-phenylethylpiperidine, remifentanil hydrochloride, α -methylfentanyl hydrochloride, N-phenylethyl-4-piperidone, carfentanil, β -hydroxyfentanyl, 3-methylthiofentanyl, alfentanil, fentanyl, alfafalfentanil, acrylfentanyl hydrochloride, thiofentanyl hydrochloride, alfafathifentanyl, and tetrahydrofurfentanyl.
The invention relates to a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which comprises the following steps: the lowest detection limit of the detection sample is 100 ng/ml.
The invention relates to a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which comprises the following steps: in the step (3), the detection sample is irradiated with laser light of a Raman detector with the wavelength of 532nm, 633nm or 785nm and the intensity of 50-500mw, and a Raman frequency shift spectrum is excited to obtain Raman frequency shift spectrum data T.
The invention relates to a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which comprises the following steps: the Raman sensitization substrate is silver particles with the particle size of 1nm to 100 nm.
The invention relates to a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which comprises the following steps: the coagulant is sodium chloride solution with pH of 2-12.
The invention relates to a method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy, which comprises the following steps: the error of the Raman frequency shift value of the Raman frequency shift spectrum data T of the detection sample and the Raman frequency shift value of the common molecular structure characteristic of the fentanyl substance is less than or equal to 2cm-1。
Compared with the existing fentanyl detection method, the method for rapidly detecting trace fentanyl by using the Raman spectroscopy can simultaneously screen all chemical substances containing fentanyl substances while keeping high-precision detection by using the Raman spectroscopy, greatly reduces the detection process and detection time, and improves the detection efficiency.
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FIG. 1 is a Raman frequency shift spectrum of a trace amount of fentanyl detected from a sample;
figure 2 is a raman shift spectrum of a standard sample of fentanyl from 27 fentanyl species.
Figure 3 is a list of 27 fentanyl species contained in the experiment.
Detailed Description
It should be noted that the raman frequency shift value is the wave number at which the material peaks in the raman spectrum, and is referred to as the raman frequency shift value of the material.
The method for rapidly detecting trace fentanyl by using Raman spectroscopy comprises the following steps,
(1) diluting a 100ug/ml fentanyl standard sample with methanol as a solvent to 100ng/ml by adding a proper amount of purified water, and uniformly mixing by shaking to obtain a sample C to be detected;
(2) mixing the sample C to be detected with a Raman sensitization substrate, adding a proper amount of a coagulant, oscillating and uniformly mixing to obtain a detection sample, wherein: the proportion of the Raman sensitization substrate, the coagulant and the sample C to be detected is 1: 1-3: 4: 5, the Raman sensitization substrate is silver particles with the particle size of 1 nm-100 nm, the detection sample is irradiated by laser of a Raman detector with the wavelength of 532nm, 633nm or 785nm and the intensity of 50-500mw, and the detection sample is detected to obtain Raman frequency shift spectrum data T of the detection sample;
(3) comparing the Raman frequency shift spectrum data T of the detection sample obtained in the step (2) with Raman frequency shift values of the following 5 fentanyl substance common molecular structure characteristics, wherein the 5 Raman frequency shift values are respectively: 622cm-1、1000cm-1、1032cm-1、 1160cm-1、1606cm-1. If at least 2 Raman frequency shift values in the Raman frequency shift spectrum data T of the detection sample are the same as the Raman frequency shift value of the common molecular structure characteristic of the fentanyl substance, the detection sample contains trace fentanyl substance. For example: in FIG. 1, in the Raman frequency shift spectrum data T of a trace fentanyl sample of 100ng/ml under excitation of a laser at a laser wavelength of 785nm and a power of 300mW, the abscissa represents the Raman frequency shift and the ordinate represents the number of photons. The Raman frequency shift spectrum data T of the sample obtained in the figure 1 and the Raman frequency shift value of the common molecular structure characteristic of the fentanyl substance are as follows: 622cm-1、1000cm-1、 1032cm-1、1160cm-1、1606cm-1. The error of Raman frequency shift should be less than or equal to 2cm-1As is evident from FIG. 1, 1000cm-1And 1032cm-1Has two Raman frequency shift values at the wavenumber, and can be referred to the Raman frequency shift spectrum of the fentanyl standard sample of FIG. 2, and the two have the spectrumHas a length of 1000cm-1And 1032cm-1The coincidence of the Raman frequency shift values at the two positions realizes the purpose of detecting the trace fentanyl substance contained in the sample.
The embodiments described are merely preferred embodiments of the present patent, which are not intended to limit the scope of the present patent, and it will be understood by those skilled in the relevant art that various changes in form and details may be made therein without departing from the spirit and scope of the present patent. Any modification, equivalent replacement, improvement and the like made within the spirit and scope of the present invention shall be included in the protection scope of the present invention.
Claims (8)
1. A method for rapidly detecting trace fentanyl substances by using a Raman spectroscopy is characterized by comprising the following steps: the Raman spectrum detection method for detecting the molecular structure main body characteristics of trace fentanyl substances in a sample by using a one-step method comprises the following steps,
(1) diluting a 100ug/ml fentanyl standard sample with methanol as a solvent to 100ng/ml by adding a proper amount of purified water, and uniformly mixing by shaking to obtain a sample C to be detected;
(2) mixing the sample C to be detected with a Raman sensitization substrate, adding a proper amount of a coagulant, oscillating and uniformly mixing to obtain a detection sample, wherein: the ratio of the Raman sensitization substrate, the coagulant and the sample C to be detected is 1: 1 to 3: 4: 5, and a Raman detector is used for detecting the sample C to be detected to obtain Raman frequency shift spectrum data T of the sample C to be detected;
(3) and (3) comparing the Raman frequency shift spectrum data T of the detection sample obtained in the step (2) with the Raman frequency shift value of the common molecular structural feature of the fentanyl substance, and if at least 2 Raman frequency shift values in the Raman frequency shift spectrum data T of the detection sample are the same as the Raman frequency shift value of the common molecular structural feature of the fentanyl substance, determining that the detection sample contains trace amount of the fentanyl substance.
2. The method for rapidly detecting trace fentanyl by raman spectroscopy as recited in claim 1, wherein: the fentanyl substance isThe Raman frequency shift value of the structural characteristic of the sex molecule is 622cm-1、1000cm-1、1032cm-1、1160cm-1、1606cm-1。
3. The method for rapidly detecting trace fentanyl by raman spectroscopy as recited in claim 2, wherein: the fentanyl substance is: 4-fluorobutyrylfentanyl, 4-fluoroisobutyrylfentanyl, butyrylfentanyl, isobutyrylfentanyl hydrochloride, furfentanyl hydrochloride, valerylfentanyl hydrochloride, beta-hydroxythiofentanyl, cis-3-methylfentanyl hydrochloride, olfentanyl, p-fluorofentanyl, sufentanil citrate, acetylfentanyl, beta-hydroxy-3-methylfentanyl, 4-anilino-N-phenylethylpiperidine, remifentanil hydrochloride, α -methylfentanyl hydrochloride, N-phenylethyl-4-piperidone, carfentanil, β -hydroxyfentanyl, 3-methylthiofentanyl, alfentanil, fentanyl, alfafalfentanil, acrylfentanyl hydrochloride, thiofentanyl hydrochloride, alfafathifentanyl, and tetrahydrofurfentanyl.
4. The method for rapidly detecting trace amounts of fentanyl by raman spectroscopy as recited in claim 3, wherein: the lowest detection limit of the detection sample is 100 ng/ml.
5. The method for rapidly detecting trace amounts of fentanyl by raman spectroscopy as recited in claim 4, wherein: in the step (3), the detection sample is irradiated with laser light of a Raman detector with the wavelength of 532nm, 633nm or 785nm and the intensity of 50-500mw, and a Raman frequency shift spectrum is excited to obtain Raman frequency shift spectrum data T.
6. The method for rapidly detecting trace amounts of fentanyl by raman spectroscopy as recited in claim 5, wherein: the Raman sensitization substrate is silver particles with the particle size of 1nm to 100 nm.
7. The method for rapid detection of trace fentanyl using raman spectroscopy as recited in claim 6, wherein: the coagulant is sodium chloride solution with pH of 2-12.
8. The method for rapid detection of trace amounts of fentanyl by raman spectroscopy according to claim 7, wherein: the error of Raman frequency shift value between the Raman frequency shift spectrum data T of the detection sample and the Raman frequency shift value of the common molecular structure characteristic of the fentanyl substance is less than or equal to 2cm-1。
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