CN116296728A - Method for extracting medicine from hair by dry method - Google Patents
Method for extracting medicine from hair by dry method Download PDFInfo
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- CN116296728A CN116296728A CN202310111170.6A CN202310111170A CN116296728A CN 116296728 A CN116296728 A CN 116296728A CN 202310111170 A CN202310111170 A CN 202310111170A CN 116296728 A CN116296728 A CN 116296728A
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- hair
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- 210000004209 hair Anatomy 0.000 title claims abstract description 112
- 239000003814 drug Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000004005 microsphere Substances 0.000 claims abstract description 72
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 72
- 238000000605 extraction Methods 0.000 claims abstract description 43
- 238000000227 grinding Methods 0.000 claims abstract description 38
- 229940079593 drug Drugs 0.000 claims abstract description 32
- 239000000203 mixture Substances 0.000 claims abstract description 32
- 231100000640 hair analysis Toxicity 0.000 claims abstract description 23
- 239000006184 cosolvent Substances 0.000 claims abstract description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011258 core-shell material Substances 0.000 claims description 6
- 238000005202 decontamination Methods 0.000 claims description 4
- 230000003588 decontaminative effect Effects 0.000 claims description 4
- 125000000524 functional group Chemical group 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000012792 core layer Substances 0.000 claims description 3
- 238000005238 degreasing Methods 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 10
- 239000000243 solution Substances 0.000 description 35
- 238000001035 drying Methods 0.000 description 15
- 238000001514 detection method Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- STJMRWALKKWQGH-UHFFFAOYSA-N clenbuterol Chemical compound CC(C)(C)NCC(O)C1=CC(Cl)=C(N)C(Cl)=C1 STJMRWALKKWQGH-UHFFFAOYSA-N 0.000 description 6
- 229960001117 clenbuterol Drugs 0.000 description 6
- 239000012634 fragment Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 210000002268 wool Anatomy 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 4
- 241001465754 Metazoa Species 0.000 description 3
- 241001494479 Pecora Species 0.000 description 3
- 229940125717 barbiturate Drugs 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000011141 high resolution liquid chromatography Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 206010044625 Trichorrhexis Diseases 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- GHQPBDDZGPAVJP-UHFFFAOYSA-N azanium;methanol;hydroxide Chemical compound N.O.OC GHQPBDDZGPAVJP-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- SVWLIIFHXFGESG-UHFFFAOYSA-N formic acid;methanol Chemical compound OC.OC=O SVWLIIFHXFGESG-UHFFFAOYSA-N 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000004896 high resolution mass spectrometry Methods 0.000 description 1
- 239000002117 illicit drug Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000006166 lysate Substances 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- -1 sulfonate ions Chemical group 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- 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
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/30—Combinations with other devices, not otherwise provided for
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B5/00—Other centrifuges
- B04B5/10—Centrifuges combined with other apparatus, e.g. electrostatic separators; Sets or systems of several centrifuges
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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- 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
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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- 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
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract
The invention discloses a method for extracting medicines from hair by a dry method, which comprises the following steps: obtaining a hair sample; adding magnetic solid phase extraction microspheres into a hair sample for first grinding to obtain a first mixture; adding a cosolvent into the mixture for second grinding to obtain a second mixture; separating the hair and the magnetic solid phase extraction microsphere in the second mixture by using a magnetic attraction mode to obtain the magnetic solid phase extraction microsphere adsorbed with the medicine; the addition amount of the magnetic solid phase extraction microsphere is 1/100-1/10 of the weight of the hair, and the dry extraction method changes the traditional mode of wet extraction of the medicine in the hair by using a large amount of solution, saves a large amount of extraction solvent, simplifies operation steps and improves extraction efficiency.
Description
Technical Field
The invention relates to the technical field of extraction of medicines in hair, in particular to a method for extracting medicines in hair by a dry method.
Background
Hair is a common test material used in illicit drug monitoring in animals and humans. At present, wet extraction methods are adopted for detecting forbidden drugs in hair. The conventional operation steps are as follows: firstly, grinding hair into fragments, then adding an extraction solvent into the hair fragments to transfer the medicine from the hair fragments to the extraction solvent, purifying and enriching the medicine in the extraction solvent by different purifying materials, and finally detecting the medicine concentration by different detecting means.
The invention patent with the application number of CN202210978031.9 discloses a method for detecting common drugs in hair, which comprises the following steps: s1: collecting a hair sample; s2: hair sample treatment: mixing and grinding a hair sample, a hair lysate and zirconia grinding beads to obtain a mixed solution; s3: and (5) detecting hair samples.
The invention patent with the application number of CN201810272590.1 discloses a quantitative detection method of barbiturates in hair, which comprises the following steps: step a, cleaning a hair sample to obtain a sample to be tested; step b, carrying out liquid nitrogen grinding on the sample to be detected to obtain a crushed sample, and carrying out ultrasonic extraction on the crushed sample by adopting methanol to obtain a solution to be detected; and c, detecting the solution to be detected in the step b by using a high-resolution liquid chromatography/mass spectrometry analysis method, obtaining detection data of the high-resolution liquid chromatography/mass spectrometry of barbiturates in the hair, and calculating the content of the barbiturates in the hair.
In summary, the existing technical method has obvious defects in practical application, and mainly comprises the following steps: (1) under the conventional grinding mode, the time and the labor are consumed for the hair breakage, the breakage degree is difficult to control, the drug in the hair is not uniformly exposed, and the detection error is large; (2) hair scraps have low density and swelling property, and a large amount of extraction solvent is needed for hair extraction; (3) the separation of hair debris from the extraction solvent is difficult, and typically after centrifugation, the hair debris can quickly re-suspend in the extraction solvent, severely interfering with subsequent cleansing operations.
Disclosure of Invention
The invention aims to provide a method for extracting medicines in hair by a dry method, which is characterized in that magnetic solid-phase extraction microspheres and a small amount of cosolvent are added into a hair sample, and grinding and mixing are carried out, so that medicines in the hair are transferred and adsorbed into holes on the surfaces of the magnetic solid-phase extraction microspheres under the action of the cosolvent 'bond bridge' and the functional groups on the surfaces of the magnetic solid-phase extraction microspheres, the separation between the medicines and the hair is realized, the traditional wet extraction mode of medicines in the hair by using a large amount of solution is changed, a large amount of extraction solvents are saved, the operation steps are simplified, and the extraction efficiency is improved.
The invention is realized by the following technical scheme:
a method for dry extraction of a drug from hair, comprising:
obtaining a hair sample;
adding magnetic solid phase extraction microspheres into a hair sample for first grinding to obtain a first mixture;
adding a cosolvent into the mixture for second grinding to obtain a second mixture;
separating the hair and the magnetic solid phase extraction microsphere in the second mixture by using a magnetic attraction mode to obtain the magnetic solid phase extraction microsphere adsorbed with the medicine;
wherein the addition amount of the magnetic solid phase extraction microsphere is 1/100-1/10 of the weight of the hair.
Preferably, the obtaining a hair sample comprises: hair was collected, decontaminated and dried to obtain hair samples.
Preferably, the hair is selected from humans or animals.
Preferably, the decontamination treatment comprises descaling and degreasing the hair with a rinse solution.
Preferably, the rinsing liquid adopts one or more of clear water, sodium dodecyl sulfonate solution, dilute hydrochloric acid solution or methanol solution.
Preferably, the drying treatment comprises drying in an oven at a drying temperature controlled between 50 and 70 ℃.
Preferably, the drying treatment includes natural evaporation drying or drying with filter paper.
Preferably, the grinding is performed using a mortar or a dedicated hair grinder.
Preferably, the magnetic solid phase extraction microsphere has a porous core-shell structure and a diameter of 0.1-10 mu m.
Preferably, the core layer of the porous core-shell structure is magnetic ferroferric oxide, and the shell layer is porous particles of silica modified with active functional groups.
Preferably, the cosolvent comprises a mixture of an organic solvent and a volatile acid or a volatile base.
Preferably, the number of addition times of the cosolvent is a plurality of times, and the second grinding time is 1 to 2 minutes.
Preferably, the cosolvent is added in an amount sufficient to moisten hair.
Preferably, the method further comprises completely volatilizing the cosolvent before separating the hair and the magnetic solid phase extraction microsphere in the second mixture by magnetic attraction.
Preferably, the separating the hair and the magnetic solid phase extraction microsphere in the second mixture by using a magnetic attraction mode to obtain the magnetic solid phase extraction microsphere adsorbed with the medicine comprises the following steps:
transferring the second mixture into a centrifuge tube, enabling the magnet to be clung to the wall of the centrifuge tube, and vibrating to separate the magnetic solid-phase extraction microspheres from the hair;
and (3) reversely buckling the centrifuge tube, and pouring out the hair to obtain the magnetic solid-phase extraction microsphere adsorbed with the medicine.
Preferably, the method further comprises purifying the magnetic solid phase extraction microsphere after the magnetic solid phase extraction microsphere with the drug adsorbed thereon is obtained.
Preferably, the purification treatment comprises the steps of adopting a solvent to remove impurities, eluting, drying and redissolving the magnetic solid-phase extraction microspheres to obtain a sample to be detected.
In summary, the extraction of the medicine from the hair is usually to add the extraction solution to the ground hair scraps, but the hair scraps have small density and swell, so that a large amount of extraction solution is consumed; hair scraps are easily clustered in an extraction solution and float on the surface of liquid, so that insufficient extraction and low efficiency are caused; the hair scraps are difficult to be completely separated from the extraction solution, so that the subsequent steps of purification, enrichment and the like are affected. The invention provides a method for extracting medicines in hair by a dry method, which comprises the steps of mixing the hair with magnetic solid-phase extraction microspheres for grinding, enabling the hair to be rapidly broken and broken by the shearing force generated in the grinding process of the hard spheres of the magnetic solid-phase extraction microspheres, simultaneously adding a cosolvent to enable the medicines in the hair to be adsorbed on the magnetic solid-phase extraction microspheres, transferring the mixture of the hair and the magnetic solid-phase extraction microspheres into a centrifuge tube, applying a magnetic field outside the centrifuge tube through a magnet, vibrating the centrifuge tube at a high frequency, and separating the magnetic solid-phase extraction microspheres adsorbed with the medicines from the hair under the action of the magnetic field, thereby realizing the purpose of separating the medicines in the hair by the dry method and effectively solving the defects of the medicines in the hair extracted by a conventional wet method.
Drawings
Fig. 1 is a flow chart of a method for dry extraction of a drug from hair.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
According to an exemplary embodiment of the present invention, there is provided a method for dry extraction of a drug from hair, as shown in fig. 1, the method comprising:
obtaining a hair sample;
adding magnetic solid phase extraction microspheres into a hair sample for first grinding to obtain a first mixture;
adding a cosolvent into the mixture for second grinding to obtain a second mixture;
separating the hair and the magnetic solid phase extraction microsphere in the second mixture by using a magnetic attraction mode to obtain the magnetic solid phase extraction microsphere adsorbed with the medicine;
wherein the addition amount of the magnetic solid phase extraction microsphere is 1/100-1/10 of the weight of the hair.
Hair grinding is generally carried out directly by using a grinding rod or a grinding ball, and because hair is soft and has strong toughness, a long time is usually required for breaking the inherent structure of hair and grinding the hair into fragments, and the fragments of the hair obtained by grinding are not uniform; according to the invention, the magnetic solid-phase extraction microsphere is added in the hair grinding process, has uniform and moderate shape and volume, is hard and porous in surface, is adhered to the surface of hair after being mixed with the hair, can generate strong shearing force on the hair during grinding, plays the role of a grinding aid, improves the hair grinding efficiency by 2-5 times, and has the advantages of full hair fragmentation, and the obtained hair fragments have small granularity and are uniform.
As an alternative embodiment, the obtaining a hair sample comprises: hair was collected, decontaminated and dried to obtain hair samples.
As an alternative embodiment, the hair is selected from humans or animals.
As an alternative embodiment, the decontamination treatment comprises descaling and degreasing the hair with a rinse solution.
As an alternative embodiment, the rinse solution is one or more of clear water, sodium dodecyl sulfonate solution, dilute hydrochloric acid solution or methanol solution.
Alternatively, the drying treatment comprises drying in an oven at a drying temperature controlled between 50 and 70 ℃.
As an alternative embodiment, the drying treatment includes natural evaporation drying or drying with filter paper.
As an alternative embodiment, the grinding is performed using a mortar or a dedicated hair grinder.
As an alternative embodiment, the magnetic solid phase extraction microsphere is of a porous core-shell structure, and the diameter is 0.1-10 mu m.
As an alternative embodiment, the core layer of the porous core-shell structure is magnetic ferroferric oxide, and the shell layer is porous particles of silica modified with active functional groups.
As an alternative embodiment, the magnetic solid phase extraction microsphere is added in an amount of 1/100 to 1/10 of the weight of the hair.
As an alternative embodiment, the co-solvent comprises a mixture of an organic solvent and a volatile acid or a volatile base.
After the hair is ground, a proper amount of cosolvent is dripped into the mixture of the hair and the magnetic solid phase extraction microsphere, and grinding is continued, so that the medicine to be detected is absorbed into holes on the surface of the magnetic solid phase extraction microsphere under the action of a bond bridge of the solution auxiliary agent after the medicine to be detected is exposed from the broken hair.
The cosolvent can dissolve the drug to be tested and can provide a solution suitable for the pH environment for the magnetic solid phase extraction microsphere to adsorb the drug to be tested.
As an alternative embodiment, the number of addition times of the cosolvent is multiple, and the second grinding time is 1-2 minutes.
For the medicine to be detected with poor magnetic solid phase extraction microsphere affinity, the cosolvent and grinding mode can be adopted for multiple times until a satisfactory extraction effect is obtained.
In an alternative embodiment, the cosolvent may be added in an amount sufficient to moisten the hair.
As an alternative embodiment, the step of completely volatilizing the cosolvent is further included before magnetically separating the hairs and the magnetic solid phase extraction microspheres in the second mixture.
As an alternative embodiment, the separating the hair and the magnetic solid phase extraction microsphere in the second mixture by using a magnetic attraction mode to obtain the magnetic solid phase extraction microsphere adsorbed with the drug, which comprises:
transferring the second mixture into a centrifuge tube, enabling the magnet to be clung to the wall of the centrifuge tube, and vibrating to separate the magnetic solid-phase extraction microspheres from the hair;
and (3) reversely buckling the centrifuge tube, and pouring out the hair to obtain the magnetic solid-phase extraction microsphere adsorbed with the medicine.
The hair scraps and the magnetic solid-phase extraction microspheres are mixed together after grinding, the magnetic solid-phase extraction microspheres are firmly adsorbed on the wall of the centrifugal tube by utilizing the magnetic attraction effect of the magnet on the magnetic solid-phase extraction microspheres, and the hair scraps are settled to the bottom of the centrifugal tube by utilizing the vibration and gravity effect, so that the dry separation of the hair scraps and the magnetic solid-phase extraction microspheres is realized.
The position of the magnet is positioned in the middle of the centrifuge tube, so that the magnetic solid-phase extraction microspheres are gathered in the middle section of the centrifuge tube, and hair scraps can fall to the lower end conveniently by gravity in the vibration process and are separated from the magnetic solid-phase extraction microspheres.
The traditional extraction process of the medicine residues in the hair comprises the steps of grinding the hair into scraps, adding an extraction solution for extraction, separating hair scraps, adding magnetic solid-phase extraction microspheres into the extraction solution for adsorbing the medicine to be detected in the solution, and then separating the solution from the magnetic solid-phase extraction microspheres by a magnetic attraction method, wherein the steps are more, the time is long, and the extraction efficiency is low. Compared with the prior art, the method integrates grinding and extraction into one step, does not need to extract solution in the whole process, realizes dry extraction, and has the advantages of simple operation, short time consumption and high extraction efficiency.
As an alternative embodiment, the method further comprises purifying the magnetic solid phase extraction microsphere after the magnetic solid phase extraction microsphere is obtained.
As an alternative embodiment, the purification treatment includes removing impurities from the magnetic solid phase extraction microsphere with a solvent, eluting, drying, and redissolving to obtain a sample to be detected.
The invention is further illustrated by the following examples of separation and detection of clenbuterol drugs in wool:
1. acquisition of wool samples
The 7-month-old male small-tailed han sheep is taken as an experimental sheep, and after the clenbutere Luo Shui solution with the weight of 15 mug/kg is orally infused for 1 time per day and continuously infused for 14 days, the back hair of the sheep is cut off to be taken as a clenbutere Luo Yangxing wool sample.
2. Wool sample decontamination and drying treatment
About 2g of a clenbuterol Luo Yangxing wool sample is placed in 100mL of 0.1% sodium dodecyl sulfonate solution, ultrasonic washing is carried out for 10min, the sodium dodecyl sulfonate solution is removed, then 100mL of clear water is added for ultrasonic rinsing for 5min, rinsing is carried out for 3 times continuously, the hair is taken out and placed on filter paper for natural airing, and scissors are used for cutting into pieces with the length of about 0.5cm for later use.
3. Hair milling
Weighing 0.2g of the dried hair sample, placing the hair sample in a mortar, adding 0.01g of magnetic solid phase extraction microsphere with the surface modified with sulfonate ions, and grinding the hair sample by using a grinding rod until the hair is broken into scraps.
4. Drug extraction
0.5mL of formic acid-methanol (volume ratio of 1:500) is added dropwise into the mixture of the hair scraps and the magnetic solid phase extraction microsphere, grinding is continued for 1min, and standing is carried out until the solution is completely volatilized.
5. Magnetic solid phase extraction microsphere separation
Transferring the mixture of the hair scraps and the magnetic solid phase extraction microspheres into a 50mL plastic centrifuge tube, placing the centrifuge tube on a magnet test tube rack, and positioning a magnet at the middle part of the side surface of the centrifuge tube; then, the magnet test tube rack is placed on the multi-tube vortex vibrator to vibrate for 5min, the magnet test tube rack is taken down from the multi-tube vortex vibrator, and then the magnet test tube rack is inverted and is beaten, and hair scraps are poured out.
6. Purification of
Taking down the centrifuge tube from the magnet test tube rack, adding 10mL of water-methanol (volume ratio is 1:1) mixed solution into the centrifuge tube to remove impurities adsorbed on the magnetic solid phase extraction microspheres, swirling the centrifuge tube for 1min, placing the centrifuge tube on the magnet test tube rack, standing, and sucking out the solution by using a suction tube after the magnetic solid phase extraction microspheres are gathered around the magnet; adding 2mL of ammonia water-methanol (volume ratio of 5:95) into the centrifuge tube, eluting the clenbuterol adsorbed on the magnetic solid-phase extraction microspheres, swirling for 1min, placing the centrifuge tube on a magnet test tube rack, standing, sucking out the solution by using a suction tube after the magnetic solid-phase extraction microspheres are gathered around a magnet, and transferring the solution into a 10mL centrifuge tube; the solution was dried with nitrogen, 0.2mL of the water-redissolved residue was added, and vortexed for 0.5min to obtain a sample redissolution.
7. Detection of
Taking the clenbuterol colloidal gold detection card, horizontally placing, sucking 50 mu L of sample complex solution, dripping the solution into a sample hole of the clenbuterol colloidal gold detection card, standing for 2min, and observing that the C and T positions on the detection card show red strips, so that the clenbuterol is a positive result.
It should be noted that in this document, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, 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 one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The foregoing is only a specific embodiment of the invention to enable those skilled in the art to understand or practice the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein. .
Claims (10)
1. A method for dry extraction of a drug from hair, comprising:
obtaining a hair sample;
adding magnetic solid phase extraction microspheres into a hair sample for first grinding to obtain a first mixture;
adding a cosolvent into the mixture for second grinding to obtain a second mixture;
separating the hair and the magnetic solid phase extraction microsphere in the second mixture by using a magnetic attraction mode to obtain the magnetic solid phase extraction microsphere adsorbed with the medicine;
wherein the addition amount of the magnetic solid phase extraction microsphere is 1/100-1/10 of the weight of the hair.
2. A method of dry extraction of a drug from hair according to claim 1, wherein obtaining a hair sample comprises: hair was collected, decontaminated and dried to obtain hair samples.
3. The method for extracting the medicine from the hair by the dry method according to claim 1, wherein the magnetic solid phase extraction microsphere has a porous core-shell structure and has a diameter of 0.1-10 μm.
4. A method for dry extraction of a drug from hair according to claim 3, wherein the core layer of the porous core-shell structure is magnetic ferroferric oxide and the shell layer is porous particles of silica modified with active functional groups.
5. A method of dry extraction of a medicament from hair according to claim 1, wherein the co-solvent comprises a mixture of an organic solvent and a volatile acid or base.
6. The method for dry extraction of a drug from hair according to claim 1, wherein the number of addition of the cosolvent is a plurality of times, and the second grinding time is 1 to 2 minutes.
7. The method for dry extraction of a drug from hair according to claim 1, wherein the separating the hair from the magnetic solid phase extraction microsphere in the second mixture by magnetic attraction to obtain the magnetic solid phase extraction microsphere with the drug adsorbed thereon comprises:
transferring the second mixture into a centrifuge tube, enabling the magnet to be clung to the wall of the centrifuge tube, and vibrating to separate the magnetic solid-phase extraction microspheres from the hair;
and (3) reversely buckling the centrifuge tube, and pouring out the hair to obtain the magnetic solid-phase extraction microsphere adsorbed with the medicine.
8. The method for dry extraction of drugs from hair according to claim 1, wherein the magnetic solid phase extraction microsphere with drugs adsorbed thereon is obtained and then further comprises purifying the magnetic solid phase extraction microsphere.
9. The method of claim 1, wherein the step of completely volatilizing the cosolvent is further included before magnetically separating the hair from the magnetic solid phase extraction microspheres in the second mixture.
10. A method of dry extraction of a medicament from hair according to any one of claims 1 to 9 wherein the decontamination treatment comprises descaling and degreasing the hair with a rinse solution employing one or more of clear water, sodium dodecyl sulphate solution, dilute hydrochloric acid solution or methanol solution.
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| CN112213412A (en) * | 2020-09-01 | 2021-01-12 | 四川警察学院 | Method for detecting drug and metabolite thereof in hair |
| CN112326819A (en) * | 2020-10-20 | 2021-02-05 | 司法鉴定科学研究院 | Analysis method for simultaneously determining etizolam, flunitrazepam and 7 amino flunitrazepam in hair |
| CN115165836A (en) * | 2022-08-16 | 2022-10-11 | 万华普曼生物工程有限公司 | Method for detecting common drugs in hair |
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| JPH11313670A (en) * | 1997-12-25 | 1999-11-16 | Tosoh Corp | Magnetic carrier, its production and extraction of nucleic acid by using the same |
| CN107449644A (en) * | 2017-07-10 | 2017-12-08 | 张红丽 | A kind of method of amphetamine and drugs such as morphine in rapid field examination hair |
| CN108283918A (en) * | 2018-02-13 | 2018-07-17 | 上海市刑事科学技术研究院 | Magnetic microsphere and its scared detection application |
| CN112213412A (en) * | 2020-09-01 | 2021-01-12 | 四川警察学院 | Method for detecting drug and metabolite thereof in hair |
| CN112326819A (en) * | 2020-10-20 | 2021-02-05 | 司法鉴定科学研究院 | Analysis method for simultaneously determining etizolam, flunitrazepam and 7 amino flunitrazepam in hair |
| CN115165836A (en) * | 2022-08-16 | 2022-10-11 | 万华普曼生物工程有限公司 | Method for detecting common drugs in hair |
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