CN112113947A - Feed pretreatment method for Raman detection, reagent pack, detection method and kit thereof - Google Patents
Feed pretreatment method for Raman detection, reagent pack, detection method and kit thereof Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 67
- 238000001069 Raman spectroscopy Methods 0.000 title claims abstract description 54
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 23
- 238000002203 pretreatment Methods 0.000 title claims abstract description 21
- 239000006228 supernatant Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 18
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- 150000007529 inorganic bases Chemical class 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 5
- AKUVRZKNLXYTJX-UHFFFAOYSA-N 3-benzylazetidine Chemical compound C=1C=CC=CC=1CC1CNC1 AKUVRZKNLXYTJX-UHFFFAOYSA-N 0.000 claims description 72
- 229960001657 chlorpromazine hydrochloride Drugs 0.000 claims description 72
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- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims description 43
- 239000000758 substrate Substances 0.000 claims description 25
- 238000000746 purification Methods 0.000 claims description 20
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- 238000000034 method Methods 0.000 claims description 11
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- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims description 7
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 7
- HFZLSTDPRQSZCQ-UHFFFAOYSA-N 1-pyrrolidin-3-ylpyrrolidine Chemical compound C1CCCN1C1CNCC1 HFZLSTDPRQSZCQ-UHFFFAOYSA-N 0.000 claims description 6
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 6
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- JGFBQFKZKSSODQ-UHFFFAOYSA-N Isothiocyanatocyclopropane Chemical compound S=C=NC1CC1 JGFBQFKZKSSODQ-UHFFFAOYSA-N 0.000 claims description 6
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 6
- PWLNAUNEAKQYLH-UHFFFAOYSA-N butyric acid octyl ester Natural products CCCCCCCCOC(=O)CCC PWLNAUNEAKQYLH-UHFFFAOYSA-N 0.000 claims description 6
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- 238000005119 centrifugation Methods 0.000 claims description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 6
- 229940017219 methyl propionate Drugs 0.000 claims description 6
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 6
- UUIQMZJEGPQKFD-UHFFFAOYSA-N n-butyric acid methyl ester Natural products CCCC(=O)OC UUIQMZJEGPQKFD-UHFFFAOYSA-N 0.000 claims description 6
- 229920002223 polystyrene Polymers 0.000 claims description 6
- 229940090181 propyl acetate Drugs 0.000 claims description 6
- HUAZGNHGCJGYNP-UHFFFAOYSA-N propyl butyrate Chemical compound CCCOC(=O)CCC HUAZGNHGCJGYNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 10
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- 238000001237 Raman spectrum Methods 0.000 description 36
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- 238000012360 testing method Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 10
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- 239000010931 gold Substances 0.000 description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
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- 229910000510 noble metal Inorganic materials 0.000 description 7
- 241001465754 Metazoa Species 0.000 description 6
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- 229910021642 ultra pure water Inorganic materials 0.000 description 6
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- 238000004381 surface treatment Methods 0.000 description 2
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- 150000001413 amino acids Chemical class 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
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- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 229960001399 clenbuterol hydrochloride Drugs 0.000 description 1
- OPXKTCUYRHXSBK-UHFFFAOYSA-N clenbuterol hydrochloride Chemical compound Cl.CC(C)(C)NCC(O)C1=CC(Cl)=C(N)C(Cl)=C1 OPXKTCUYRHXSBK-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
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- 229910001866 strontium hydroxide Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a feed pretreatment method for Raman detection, a reagent pack, a detection method and a kit thereof. The pretreatment method of the feed comprises the following steps: a) mixing the feed to be detected with an extracting agent for extraction to obtain an extracting solution; the extractant is a miscible solution of inorganic base, an ester solvent with carbon atom number not more than 8 and water; b) adding water into the extractive solution, mixing, layering, and collecting supernatant as the solution to be detected for Raman detection. The extracting agent can effectively extract antibiotics and prohibited drugs without extracting other interfering substances, and water is used as a purifying extracting agent to purify the extracting solution, so that the interference of a complex matrix in the feed is greatly reduced, a good response effect is realized for Raman detection, and a low-content object to be detected can be detected. And the pretreatment method is simple and quick and has low requirement on equipment.
Description
Technical Field
The invention relates to the technical field of Raman detection, in particular to a feed pretreatment method, a reagent pack, a detection method and a kit for Raman detection.
Background
With the rapid development of animal husbandry, the centralized breeding degree of animals is greatly improved, and the use of animal feed and veterinary drugs is widely popularized. In order to ensure the quality safety of edible animals, 40 medicines such as clenbuterol hydrochloride are prohibited from being used in the Chinese Ministry of agriculture bulletin No. 176 'catalog of medicine varieties prohibited from being used in feed and animal drinking water'. However, the problems of antibiotics abuse and use of prohibited veterinary drugs still exist, and the animal husbandry development and the health of people are seriously affected. Therefore, it is an urgent problem to provide a rapid and sensitive detection means for ensuring human health.
However, the traditional detection method aiming at antibiotics and prohibited veterinary drugs in the feed has strict requirements on pretreatment conditions and complicated steps.
Disclosure of Invention
On the basis, the feed pretreatment method, the reagent pack, the detection method and the kit for the Raman detection are needed to be provided for solving the problems that the traditional detection method for antibiotics and prohibited veterinary drugs in the feed has strict requirements on pretreatment conditions and complicated steps.
A feed pretreatment method for Raman detection comprises the following steps:
a) mixing the feed to be detected with an extracting agent for extraction to obtain an extracting solution; the extractant is a miscible solution of inorganic base, an ester solvent with the carbon atom number not more than 8 and water;
b) and adding water into the extracting solution, uniformly mixing, layering, and taking supernatant as a to-be-detected solution for Raman detection.
In one embodiment, between the step a) and the step b), a step of adding a purification bag to the extracting solution for adsorption is further included.
In one embodiment, the purification package comprises at least one of surface aminated polystyrene, silica gel, graphitized carbon black, and anhydrous magnesium sulfate.
In one embodiment, the layering mode is centrifugation, the rotation speed of the centrifugation does not exceed 4000rpm, and the time of the centrifugation does not exceed 5 min.
In one embodiment, the layering mode is standing, and the standing time is not more than 10 min.
In one embodiment, the ester solvent having not more than 8 carbon atoms is at least one selected from the group consisting of methyl acetate, ethyl acetate, propyl acetate, butyl acetate, ethyl formate, propyl formate, butyl formate, methyl propionate, ethyl propionate, butyl propionate, methyl butyrate, ethyl butyrate, propyl butyrate, and butyl butyrate.
In one embodiment, the dosage ratio of the feed to be detected to the extracting agent is 1g (0.5-10) mL; the volume ratio of the extracting solution to the water is 1 (0.5-2).
In one embodiment, the mass of the inorganic base is 0.05-0.5% of the mass of the extractant.
The invention provides a feed pretreatment reagent kit for Raman detection, which comprises an extracting agent, wherein the extracting agent is a miscible solution of inorganic base, an ester solvent with the carbon atom number not more than 8 and water, and the ester solvent with the carbon atom number not more than 8 is selected from at least one of methyl acetate, ethyl acetate, propyl acetate, butyl acetate, ethyl formate, propyl formate, butyl formate, methyl propionate, ethyl propionate, butyl propionate, methyl butyrate, ethyl butyrate, propyl butyrate and butyl butyrate.
In one embodiment, the purification device further comprises a purification bag, wherein the purification bag comprises at least one of surface aminated polystyrene, silica gel, graphitized carbon black and anhydrous magnesium sulfate.
The invention provides a method for detecting chlorpromazine hydrochloride in feed, which comprises the following steps:
extracting the feed to be detected according to any feed pretreatment method for Raman detection; and combining the supernatant with the SERS substrate, and performing surface enhanced Raman spectroscopy.
The invention provides a kit for detecting chlorpromazine hydrochloride in feed, which comprises the following reagents:
(1) a SERS substrate;
(2) any one of the feed pretreatment reagent packages for Raman detection.
The feed matrix is complex, contains a large amount of substances such as crude protein, crude fat, crude fiber and the like, and greatly interferes the extraction of antibiotics and prohibited drugs in the feed, so that the pretreatment requirement on the feed is higher. Based on the method, through continuous research, the miscible solution of inorganic base, the ester solvent with the carbon atom number not more than 8 and water is selected as the extracting agent, so that antibiotics and prohibited drugs can be effectively extracted without extracting other interfering substances, and the extracting solution is purified by adopting the water as the purifying extracting agent, so that the interference of complex matrixes in the feed is greatly reduced, and the method has a good response effect on Raman detection. Furthermore, a purification bag is added into the extracting solution to adsorb macromolecular protein and cellulose to reduce interference, so that a low-content object to be detected can be detected. And the pretreatment method is simple and quick and has low requirement on equipment.
In particular, the structural characteristics of the chlorpromazine hydrochloride molecule enable the change of the polarizability to be small, the Raman absorption signal to be weak, and the chlorpromazine hydrochloride with low concentration is more difficult to detect. The extracting agent disclosed by the invention has specific selection on chlorpromazine hydrochloride, can effectively extract chlorpromazine hydrochloride without extracting other interfering substances, can detect chlorpromazine hydrochloride with a lower content, and can realize rapid detection of chlorpromazine hydrochloride in feed, wherein the detection time of each sample is not more than 8 min. In addition, the detection limit of the chlorpromazine hydrochloride in the feed to be detected can be as low as 0.1mg/kg and is far lower than the national 1mg/kg detection standard only after the simple pretreatment. Meanwhile, the detection method has simple steps, short analysis time and good selectivity, and is particularly suitable for quickly detecting chlorpromazine hydrochloride in compound feed, concentrated feed and additive premix feed. And the detection method does not need large instruments, and realizes the rapid and accurate detection of the chlorpromazine hydrochloride in the on-site feed.
Drawings
FIG. 1 is a flow chart of a method for detecting chlorpromazine hydrochloride in feed according to an embodiment of the invention;
FIG. 2 is a Raman spectrum of chlorpromazine hydrochloride standard samples of different concentrations according to one embodiment of the present invention;
FIG. 3 is a standard graph of chlorpromazine hydrochloride according to an embodiment of the invention;
fig. 4 is an SEM image of the SERS chip 1 according to an embodiment of the present invention;
fig. 5 is an SEM image of the SERS chip 2 according to an embodiment of the present invention;
FIG. 6 is a Raman spectrum of chlorpromazine hydrochloride in feed according to an embodiment of the invention;
FIG. 7 is a Raman spectrum of chlorpromazine hydrochloride at different concentrations in a feed according to an embodiment of the invention;
fig. 8 is a raman spectrum obtained by detection using the SERS chip 1 according to the embodiment of the present invention;
fig. 9 is a raman spectrum obtained by detection using the SERS chip 2 according to an embodiment of the present invention;
fig. 10 is a standard curve diagram of chlorpromazine hydrochloride standard and detection samples according to an embodiment of the invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings, which illustrate embodiments of the present invention. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Surface-enhanced Raman scattering (SERS) mainly refers to an abnormal optical enhancement phenomenon on the Surface of a nanoscale rough metal (such as gold, silver, copper, and transition metals) or a particle system.
Referring to fig. 1, a feed pretreatment method for raman detection according to an embodiment of the present invention includes the following steps:
s10, mixing the feed to be detected with an extracting agent for extraction to obtain an extracting solution, wherein the extracting agent is a miscible solution of inorganic base, an ester solvent with the carbon atom number not more than 8 and water.
In one embodiment, after step S10, the method further comprises the step of adding a purification bag to the extraction solution.
In one embodiment, the purification package comprises at least one of surface aminated polystyrene, silica gel, graphitized carbon black, and anhydrous magnesium sulfate. The interference on detection is reduced by adding the purifying bag into the extracting solution to adsorb macromolecular protein and cellulose in the feed. In a preferred mode, the purification bag further comprises alumina or sodium chloride.
In one embodiment, the ester solvent having not more than 8 carbon atoms is at least one selected from the group consisting of methyl acetate, ethyl acetate, propyl acetate, butyl acetate, ethyl formate, propyl formate, butyl formate, methyl propionate, ethyl propionate, butyl propionate, methyl butyrate, ethyl butyrate, propyl butyrate, and butyl butyrate.
In one embodiment, the inorganic base is 0.05 to 0.5% by mass of the extractant. The inorganic base is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, magnesium hydroxide, calcium hydroxide, lithium hydroxide, rubidium hydroxide, strontium hydroxide, and aluminum hydroxide.
In one embodiment, the mass of water is not more than 0.5% of the mass of the ester solvent having not more than 8 carbon atoms.
Through continuous research, the extractant contains a small amount of inorganic base, so that acidic substances such as amino acid in the feed can be neutralized, and the interference of the matrix on Raman detection can be further reduced. And the selected ester solvent with the carbon atom number not more than 8 has excellent extraction effect on the substances to be detected in the feed and has good response effect on Raman spectrum.
Preferably, the step of extracting is ultrasonic extracting, and the time of ultrasonic extracting is not more than 4 min. The method can achieve high-efficiency extraction in a short time, thereby achieving the purpose of rapid detection.
In one embodiment, the dosage ratio of the feed to be detected to the extractant is 1g (0.5-10) mL. Preferably, the dosage ratio of the feed to be detected to the extracting agent is 1g:2 mL. The extractant preferably completely soaks the feed to be detected, but the amount of the extractant cannot be excessively larger than that of the feed to be detected, and the extractant can be extracted efficiently by continuously researching and obtaining the optimal dosage.
And S20, adding water into the extracting solution, uniformly mixing, layering, and taking the supernatant as a to-be-detected solution for Raman detection.
In one embodiment, the layering is performed by centrifugation at a speed of not more than 4000rpm for a period of not more than 5 min. The invention has low requirement on the rotating speed of centrifugation and can use a portable centrifuge. In another embodiment, the layering is by standing for a period of no more than 10 min.
In one embodiment, the volume ratio of the extract to water is 1 (0.5-2). Preferably, the volume ratio of the extract to water is 1: 0.5. The volume ratio of the above extractive solution to water is excellent.
In one embodiment, the blending is performed by shaking and shaking.
The invention also provides a feed pretreatment reagent bag for Raman detection, which comprises an extracting agent. The extraction reagent is a miscible solution of inorganic base, ester solvent with carbon number not more than 8 and water. The ester solvent with carbon number not more than 8 is at least one selected from methyl acetate, ethyl acetate, propyl acetate, butyl acetate, ethyl formate, propyl formate, butyl formate, methyl propionate, ethyl propionate, butyl propionate, methyl butyrate, ethyl butyrate, propyl butyrate and butyl butyrate.
In one embodiment, the feed pretreatment reagent kit for raman detection further comprises a purification kit. The purification bag comprises at least one of polystyrene with aminated surface, silica gel, graphitized carbon black and anhydrous magnesium sulfate.
The invention also provides a kit for detecting chlorpromazine hydrochloride in feed, which comprises the following reagents:
(1) a SERS substrate;
(2) any one of the above feed pretreatment reagent packages for raman detection.
The invention also provides an embodiment of a method for detecting chlorpromazine hydrochloride in feed, which comprises the following steps:
extracting the feed to be detected according to any one of the feed pretreatment methods for Raman detection; and then combining the supernatant with the SERS substrate to perform surface enhanced Raman spectroscopy test.
It can be understood that the Raman spectrum of the sample obtained by the detection method can determine whether the sample contains chlorpromazine hydrochloride. Specifically, for example, the obtained raman spectrum of the sample is compared with the spectrum of the chlorpromazine hydrochloride standard substance to realize qualitative detection.
The shift of qualitative characteristic peak of chlorpromazine hydrochloride is 786 +/-5 cm-1、1091±5cm-1、1165±5cm-1、1234±5cm-1、1304±5cm-11562 +/-5 cm-1. If the qualitative characteristic peak of the chlorpromazine hydrochloride appears in the Raman spectrum of the obtained sample at the same time, the sample is positive, otherwise, the sample is negative as long as one qualitative characteristic peak does not appear. Wherein, positive means that the sample contains chlorpromazine hydrochloride, and negative means that the sample does not contain chlorpromazine hydrochloride.
In one embodiment, the selection of the SERS substrate is not limited, for example: SERS reagent, SERS chip, etc. The SERS reagent is nanogold sol or nano silver sol, and can also be other types of SERS reagents which can be made by the user or purchased in the market.
In one embodiment, when the SERS substrate is a SERS chip, the step of combining the supernatant with the SERS substrate to perform the surface enhanced raman spectroscopy includes: and (3) placing the SERS chip in the supernatant, taking out, cleaning and drying, and then carrying out Raman spectrum test.
In one embodiment, the SERS chip includes a substrate and a plurality of noble metal nanoclusters uniformly distributed on the substrate, each noble metal nanocluster being confined in a corresponding nanodrop on the substrate; the noble metal nano-cluster is formed by self-assembling 3-8 noble metal nano-particles; the average particle size of the noble metal nano-particles is 30 nm-120 nm; the average distance between each nano particle is 1nm to 2 nm.
In one embodiment, the noble metal nanoparticles are selected from one or more of gold nanoparticles, silver nanoparticles, copper nanoparticles, and platinum nanoparticles.
In one embodiment, the substrate of the SERS chip of the present invention is an AAO template having a plurality of nano-pits, and the noble metal nanoclusters are self-assembled in the nano-pits of the AAO template.
The supernatant obtained by the feed to be detected after the simple pretreatment is combined with the SERS chip developed by the applicant, an SERS signal with high sensitivity, stability and repeatability can be obtained, and the method is particularly suitable for the rapid and high-sensitivity detection of chlorpromazine hydrochloride in the feed.
In one embodiment, when the SERS substrate is a SERS reagent, the step of combining the supernatant with the SERS substrate to perform the surface enhanced raman spectroscopy comprises: and adding the SERS reagent and the salt solution into the supernatant, uniformly mixing, and then carrying out Raman spectrum test.
In one embodiment, the volume ratio of the supernatant, the SERS reagent and the salt solution is (1-4): 0.5-4): 0.2-5, and the concentration of the salt solution is 1 wt% to 20 wt%. Preferably, the volume ratio of the supernatant, the SERS reagent and the salt solution is 2:1: 1.
In one embodiment, in the step of performing the raman spectroscopy, the laser energy of the raman spectroscopy is 50mW to 500mW, the spectrum scanning time is 1000mS to 20000mS, the number of scanning is 1 to 10, and the smoothing parameter is 1 to 5. The Raman spectrum parameters for detecting the chlorpromazine hydrochloride in the feed can be obtained by continuously searching the optimal detection effect and comprehensively considering factors such as the detection efficiency.
In one embodiment, the method for detecting chlorpromazine hydrochloride in the feed further comprises the following steps:
preparing chlorpromazine hydrochloride standard solutions with different concentrations, and respectively testing the Raman spectra of the chlorpromazine hydrochloride standard solutions with different concentrations;
and (4) performing Raman spectrum test on the supernatant to obtain a Raman spectrum and performing Raman spectrum of the standard solution of chlorpromazine hydrochloride with different concentrations to obtain the concentration of chlorpromazine hydrochloride in the feed.
The invention provides establishment of a chlorpromazine hydrochloride standard substance gallery in an embodiment.
Standard solutions of chlorpromazine hydrochloride having concentrations of 100ppm, 10ppm, 1ppm, 100ppb, 10ppb, 1ppb and 0.1ppb were prepared, 200. mu.L of each of the standard solutions was placed in a test bottle, 100. mu.L of gold sol was added, 100. mu.L of 1 wt% NaCl solution was added, and the test was carried out by a Raman spectrometer. Obtaining a standard characteristic peak spectrum of chlorpromazine hydrochloride, establishing a standard substance database on software, and establishing 786 +/-5 cm of data by using a characteristic peak position method-1，1091±5cm-1，1165±5cm-1，1234±5cm-1，1304±5cm-1，1562±5cm-1And positive appeared at the same time. The Raman spectrum of the chlorpromazine hydrochloride standard is shown in FIG. 2, wherein the abscissa is Raman peak Shift (Raman Shift) in cm-1The ordinate is Intensity (Intensity), unit: a.u.
The present invention also provides an embodiment of the quantitative assay: according to a certain specific wavelength of Raman spectrum of a standard solution of chlorpromazine hydrochloride (such as 1234 cm)-1) Half of the intensity of (c) was plotted against the negative logarithm of the concentration to obtain a standard curve, as shown in fig. 3. Then according to the chlorpromazine hydrochloride content in the feed to be detected at 1234cm-1And calculating the concentration of chlorpromazine hydrochloride in the feed according to the intensity.
The following are specific examples.
Preparing nano gold sol:
a100 mL three-necked flask was charged with 1mL of a 1 wt% aqueous chloroauric acid solution and diluted to 100mL, then heated to boiling, and a 1 wt% sodium citrate solution was added under constant reflux and vigorous stirring. The solution gradually changed from light yellow to wine red. Timing after color change, keeping the boiling state of the system for 15min under stirring, and then naturally cooling to room temperature to obtain the nano gold sol.
Preparing nano silver sol:
Preparation of the SERS chip:
providing a substrate: an aluminum oxide template prepared by an anodic oxidation method is taken as a substrate, and cut into a square sheet with the length of 4mm and the width of 4mm, wherein the aluminum oxide template is of a double-layer structure, the lower layer is a metal aluminum layer with the thickness of about 0.3mm, the upper layer is an aluminum oxide layer with the thickness of about 80nm, a plurality of nano concave parts are microscopically disordered and macroscopically uniformly distributed on the whole surface of the substrate, the number of the nano concave parts on each square centimeter on the substrate is about 108-109, the caliber of each nano concave part is about 90nm, the depth of each nano concave part is about 80nm and is slightly smaller than the thickness of the aluminum oxide layer, and the distance between every two adjacent nano concave parts is about 20 nm.
And cleaning and/or carrying out surface treatment on the surface of the substrate, soaking the substrate in the nano silver sol for 3 hours, self-assembling nano silver particles into nano concave parts of the substrate, forming a silver nano cluster formed by self-assembling 3-10 silver nanoparticles into each concave part, taking out and drying to obtain the SERS chip 1, wherein an SEM image of the SERS chip 1 is shown in figure 4.
Or cleaning and/or carrying out surface treatment on the surface of the substrate, soaking the substrate in the nano gold sol for 3 hours, self-assembling the nano gold particles into nano concave parts of the substrate, forming a gold nano cluster formed by self-assembling 3-10 gold nanoparticles in each concave part, taking out and drying to obtain the SERS chip 2, wherein an SEM image of the SERS chip 2 is shown in FIG. 5.
In the following examples, pig feed was tested by adding different amounts of chlorpromazine hydrochloride standard substances. (1000 ppb at 1ppm, 1g/kg at 1 ppm)
Example 1
Preparing a miscible solution of sodium hydroxide, ethyl acetate and ultrapure water, wherein the mass fraction of the sodium hydroxide is 0.1 wt%, the mass fraction of the ultrapure water is 0.1 wt%, and the balance is ethyl acetate.
Weighing 1g pig feed, pulverizing (the amount of chlorpromazine hydrochloride is 100ppm), adding 2ml miscible solution, ultrasonic extracting for 2min, and retaining supernatant to obtain extractive solution. Taking 1mL of the extract, adding 0.5mL of ultrapure water, centrifuging at 4000rpm for 2min, and keeping the supernatant.
And putting 200 mu L of the supernatant into a test bottle, adding 100 mu L of nano gold sol, adding 100 mu L of 1 wt% NaCl solution, and testing by using a Raman spectrometer. The chlorpromazine hydrochloride-labeled raman spectrum is positive as shown in a in fig. 6. In FIG. 6, the abscissa is the Raman Shift (Raman Shift) in cm-1Intensity (Intensity) in a.u. is plotted on the ordinate.
Example 2
The difference from example 1 is that: the addition amount of chlorpromazine hydrochloride is 10 ppm; and adding a graphitized carbon purification bag into the obtained extracting solution. The chlorpromazine hydrochloride-labeled raman spectrum is positive as shown in a in fig. 7. In FIG. 7, the abscissa is the Raman Shift (Raman Shift) in cm-1Intensity (Intensity) in a.u. is plotted on the ordinate.
Example 3
The difference from example 2 is that: the addition amount of chlorpromazine hydrochloride is 1 ppm; replacing ethyl acetate with ethyl formate; and replacing the anhydrous graphitized carbon purification bag with an anhydrous magnesium sulfate purification bag. The chlorpromazine hydrochloride-labeled raman spectrum is positive as shown in b in fig. 7.
Example 4
The difference from example 2 is that: the amount of chlorpromazine hydrochloride added was 100ppb (0.1 mg/kg). The chlorpromazine hydrochloride-labeled raman spectrum is positive as shown in c in fig. 7.
Example 5
The difference from example 2 is that: the chlorpromazine hydrochloride standard was not added. The raman spectrum was negative as shown by d in fig. 7.
Example 6
Preparing a miscible solution of sodium hydroxide, ethyl acetate and ultrapure water, wherein the mass fraction of the sodium hydroxide is 0.1 wt%, the mass fraction of the ultrapure water is 0.1 wt%, and the balance is ethyl acetate.
Weighing 1g of pig feed, pulverizing (the addition amount of chlorpromazine hydrochloride is 10ppm), adding 2mL of miscible solution, performing ultrasonic extraction for 2min, and retaining supernatant to obtain extractive solution. And adding graphitized carbon and magnesium sulfate purification bags into the extracting solution. Then, 1mL of ultrapure water was added to 1mL of the extract, and the mixture was centrifuged at 4000rpm for 2min to retain the supernatant.
And (3) placing the SERS chip 1 in 200 mu L of supernatant, taking out after 10min, washing with ethanol, drying, and testing by using a Raman spectrometer. The Raman spectrum of chlorpromazine hydrochloride is positive as shown in FIG. 8. Wherein the abscissa is Raman Shift (Raman Shift) in cm-1Intensity (Intensity) in a.u. is plotted on the ordinate.
Example 7
The difference from example 6 is that: the addition amount of chlorpromazine hydrochloride is 1 ppm; replacing ethyl acetate with ethyl butyrate; the SERS chip 2 was placed in 200. mu.L of the supernatant. The Raman spectrum of chlorpromazine hydrochloride is positive as shown in FIG. 9. Wherein the abscissa is Raman Shift (Raman Shift) in cm-1Intensity (Intensity) in a.u. is plotted on the ordinate.
And (3) quantitative detection: the chlorpromazine hydrochloride (actual sample) in the feed of the embodiment 1-4 is placed at 1234cm-1Intensity of (f) was compared to a standard sample curve, as shown in fig. 10, where the abscissa is the negative logarithm of the concentration and the ordinate is the Intensity (Intensity) in a.u. Therefore, the detection method can simultaneously realize the quantitative detection of the chlorpromazine hydrochloride in the feed.
Comparative example 1
The difference from example 1 is that: ethyl acetate was replaced with ethanol. And (3) testing results: no Raman spectrum peak of chlorpromazine hydrochloride appears.
Comparative example 2
The difference from example 1 is that: the ethyl acetate was replaced with acetonitrile. And (3) testing results: no Raman spectrum peak of chlorpromazine hydrochloride appears.
Comparative example 3
The difference from example 1 is that: instead of preparing a miscible solution, 2ml of miscible solution were replaced directly with 2ml of ethyl acetate. The raman spectrum of chlorpromazine hydrochloride is positive as shown in b in fig. 6.
Comparative example 4
The difference from example 4 is that: ethyl acetate was replaced with n-hexane. And (3) testing results: no Raman spectrum peak of chlorpromazine hydrochloride appears.
Comparative example 5
The difference from example 4 is that: instead of preparing a miscible solution, 2ml of miscible solution were replaced directly with 2ml of ethyl acetate. And (3) testing results: no Raman spectrum peak of chlorpromazine hydrochloride appears.
Analysis of results
When the addition amount of the chlorpromazine hydrochloride in the feed is 100ppm, the ethyl acetate is replaced by ethanol in the comparative example 1, and finally, the Raman spectrum peak of the chlorpromazine hydrochloride does not appear in Raman detection, but only the Raman spectrum peak of the ethanol appears. In the comparative example 2, ethyl acetate is replaced by acetonitrile, and finally, the Raman spectrum peak of chlorpromazine hydrochloride does not appear in Raman detection, but only appears in the Raman spectrum peak of acetonitrile. Comparative example 3 extraction was carried out with pure ethyl acetate and the raman peak of chlorpromazine hydrochloride is shown as b in fig. 6, with a significantly lower peak intensity than in example 1 (a in fig. 6). When the addition amount of the chlorpromazine hydrochloride in the feed is 100ppb, the Raman spectrum peak of the chlorpromazine hydrochloride is not detected in the case that the ethyl acetate is replaced by the normal hexane in the comparative example 4, and the Raman spectrum peak of the chlorpromazine hydrochloride is not detected in the case that the pure ethyl acetate is adopted for extraction in the comparative example 5.
Therefore, as shown in fig. 7, the extraction agent specifically selected for chlorpromazine hydrochloride is selected for extraction, and water is used as the purification extraction agent for purifying the extraction solution, so that the interference of a complex matrix in the feed is greatly reduced, and the Raman detection response is good. Furthermore, a purification bag is added into the extracting solution to adsorb macromolecular protein and cellulose to reduce interference, so that a low-content object to be detected can be detected. The rapid detection of the chlorpromazine hydrochloride in the feed is realized, and the detection limit of the chlorpromazine hydrochloride in the feed is as low as 0.1mg/kg and is far lower than the national 1mg/kg detection standard.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (12)
1. A feed pretreatment method for Raman detection is characterized by comprising the following steps:
a) mixing the feed to be detected with an extracting agent for extraction to obtain an extracting solution; the extractant is a miscible solution of inorganic base, an ester solvent with the carbon atom number not more than 8 and water;
b) and adding water into the extracting solution, uniformly mixing, layering, and taking supernatant as a to-be-detected solution for Raman detection.
2. The feed pretreatment method for raman detection according to claim 1, further comprising a step of adding a purification bag to the extraction liquid between the step a) and the step b).
3. The feed pretreatment method for raman detection according to claim 2, wherein the purification bag comprises at least one of surface-aminated polystyrene, silica gel, graphitized carbon black, and anhydrous magnesium sulfate.
4. The feed pretreatment method for Raman detection according to claim 1, wherein the layering is performed by centrifugation at a rotation speed of not more than 4000rpm for a period of not more than 5 min.
5. The feed pretreatment method for Raman detection according to claim 1, wherein the layering is performed by standing, and the standing time is not more than 10 min.
6. The feed pretreatment method for raman detection according to claim 1, wherein the ester solvent having not more than 8 carbon atoms is at least one selected from the group consisting of methyl acetate, ethyl acetate, propyl acetate, butyl acetate, ethyl formate, propyl formate, butyl formate, methyl propionate, ethyl propionate, butyl propionate, methyl butyrate, ethyl butyrate, propyl butyrate, and butyl butyrate.
7. The feed pretreatment method for Raman detection according to claim 1, wherein the dosage ratio of the feed to be detected to the extracting agent is 1g (0.5-10) mL; the volume ratio of the extracting solution to the water is 1 (0.5-2).
8. The feed pretreatment method for raman detection according to claim 1, wherein the mass of the inorganic base is 0.05% to 0.5% of the mass of the extractant.
9. The feed pretreatment reagent kit for Raman detection comprises an extraction agent, and is characterized in that the extraction agent is a miscible solution of inorganic base, an ester solvent with the carbon atom number not more than 8 and water, wherein the ester solvent with the carbon atom number not more than 8 is selected from at least one of methyl acetate, ethyl acetate, propyl acetate, butyl acetate, ethyl formate, propyl formate, butyl formate, methyl propionate, ethyl propionate, butyl propionate, methyl butyrate, ethyl butyrate, propyl butyrate and butyl butyrate.
10. The kit for pretreatment of feed for raman detection according to claim 9, further comprising a purification kit comprising at least one of surface-aminated polystyrene, silica gel, graphitized carbon black, and anhydrous magnesium sulfate.
11. A method for detecting chlorpromazine hydrochloride in feed is characterized by comprising the following steps:
extracting a feed to be detected according to the feed pretreatment method for Raman detection of any one of claims 1 to 8; and combining the supernatant with the SERS substrate, and performing surface enhanced Raman spectroscopy.
12. A kit for detecting chlorpromazine hydrochloride in feed is characterized by comprising the following reagents:
(1) a SERS substrate;
(2) the feed pretreatment reagent pack for Raman detection according to any one of claims 9 to 10.
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Cited By (2)
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| CN110609027A (en) * | 2019-09-10 | 2019-12-24 | 中国检验检疫科学研究院 | Method for rapidly detecting chlorpromazine hydrochloride in feed |
| CN114166824A (en) * | 2021-12-08 | 2022-03-11 | 桂林医学院 | Method for analyzing drug content in health product by tracing auxiliary agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110609027A (en) * | 2019-09-10 | 2019-12-24 | 中国检验检疫科学研究院 | Method for rapidly detecting chlorpromazine hydrochloride in feed |
| CN114166824A (en) * | 2021-12-08 | 2022-03-11 | 桂林医学院 | Method for analyzing drug content in health product by tracing auxiliary agent |
| CN114166824B (en) * | 2021-12-08 | 2024-01-23 | 桂林医学院 | Method for analyzing drug content in health care product by tracing auxiliary agent |
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