CN114166835B - Method for analyzing drug content in health care product by tracing auxiliary agent - Google Patents
Method for analyzing drug content in health care product by tracing auxiliary agent Download PDFInfo
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- 239000003814 drug Substances 0.000 title claims abstract description 87
- 229940079593 drug Drugs 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 31
- 230000036541 health Effects 0.000 title claims description 79
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 35
- 238000002835 absorbance Methods 0.000 claims abstract description 30
- 238000001514 detection method Methods 0.000 claims abstract description 27
- 238000001212 derivatisation Methods 0.000 claims abstract description 26
- 238000006303 photolysis reaction Methods 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 18
- 230000015843 photosynthesis, light reaction Effects 0.000 claims abstract description 16
- 238000004737 colorimetric analysis Methods 0.000 claims abstract description 11
- 238000009835 boiling Methods 0.000 claims abstract description 5
- AKUVRZKNLXYTJX-UHFFFAOYSA-N 3-benzylazetidine Chemical group C=1C=CC=CC=1CC1CNC1 AKUVRZKNLXYTJX-UHFFFAOYSA-N 0.000 claims description 72
- 229960001657 chlorpromazine hydrochloride Drugs 0.000 claims description 72
- 239000000523 sample Substances 0.000 claims description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 65
- 239000007788 liquid Substances 0.000 claims description 64
- 238000010521 absorption reaction Methods 0.000 claims description 59
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical group CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 38
- -1 alcohol compound Chemical class 0.000 claims description 25
- 150000003254 radicals Chemical class 0.000 claims description 25
- 238000000926 separation method Methods 0.000 claims description 23
- 239000012086 standard solution Substances 0.000 claims description 22
- 238000005286 illumination Methods 0.000 claims description 21
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000011161 development Methods 0.000 claims description 10
- 238000012417 linear regression Methods 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 7
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
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- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000000546 pharmaceutical excipient Substances 0.000 claims description 5
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 4
- 239000006096 absorbing agent Substances 0.000 claims description 4
- 229910001447 ferric ion Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
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- 238000002360 preparation method Methods 0.000 claims description 2
- 239000002671 adjuvant Substances 0.000 claims 4
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- 238000004458 analytical method Methods 0.000 abstract description 5
- 230000035945 sensitivity Effects 0.000 abstract description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 24
- MNUOZFHYBCRUOD-UHFFFAOYSA-N hydroxyphthalic acid Natural products OC(=O)C1=CC=CC(O)=C1C(O)=O MNUOZFHYBCRUOD-UHFFFAOYSA-N 0.000 description 13
- 238000001819 mass spectrum Methods 0.000 description 12
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- 238000010586 diagram Methods 0.000 description 9
- YMVFQWULFRMLRA-UHFFFAOYSA-N 10-[3-(dimethylamino)propyl]phenothiazin-2-ol Chemical compound C1=C(O)C=C2N(CCCN(C)C)C3=CC=CC=C3SC2=C1 YMVFQWULFRMLRA-UHFFFAOYSA-N 0.000 description 8
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 8
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 6
- 230000007246 mechanism Effects 0.000 description 6
- 229950000688 phenothiazine Drugs 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
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- 239000007864 aqueous solution Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229940001470 psychoactive drug Drugs 0.000 description 4
- 239000004089 psychotropic agent Substances 0.000 description 4
- RDIMQHBOTMWMJA-UHFFFAOYSA-N 4-amino-3-hydrazinyl-1h-1,2,4-triazole-5-thione Chemical compound NNC1=NNC(=S)N1N RDIMQHBOTMWMJA-UHFFFAOYSA-N 0.000 description 3
- 150000001793 charged compounds Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
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- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- FPFSGDXIBUDDKZ-UHFFFAOYSA-N 3-decyl-2-hydroxycyclopent-2-en-1-one Chemical compound CCCCCCCCCCC1=C(O)C(=O)CC1 FPFSGDXIBUDDKZ-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
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- 235000013305 food Nutrition 0.000 description 2
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 2
- 239000002117 illicit drug Substances 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
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- 150000004893 oxazines Chemical class 0.000 description 2
- 238000007348 radical reaction Methods 0.000 description 2
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- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 239000012445 acidic reagent Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010523 cascade reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000000382 dechlorinating effect Effects 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003684 drug solvent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 150000002990 phenothiazines Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229960001836 promazine hydrochloride Drugs 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003860 sleep quality Effects 0.000 description 1
- 238000002470 solid-phase micro-extraction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000012795 verification 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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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
- G01N1/38—Diluting, dispersing or mixing samples
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- 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
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
A method for analyzing the content of medicine in health-care product by tracing the auxiliary agent includes such steps as generating photolysis reaction and free radicals, capturing the free radicals generated by medicine in photolysis to generate volatile first component, separating out the low-boiling point first component, developing the first component by derivatization reagent, and determining the content of medicine in health-care product by colorimetry or by measuring the ultraviolet-visible absorbance value. Compared with the prior art, the method for analyzing the drug content in the health-care product by tracing the auxiliary agent shortens the time required by sample pretreatment, greatly simplifies the detection and analysis process of the drug content in the health-care product, and has simple steps and high sensitivity.
Description
Technical Field
The invention relates to the field of illegal drug addition detection of health products, in particular to a method for tracing and analyzing the drug content in the health products by using auxiliary agents.
Background
The health food has regulating effect, and is a special food for treating diseases, and medicines cannot be added illegally. However, in recent years, with the increasing demand of health care products in the market, the phenomenon of forbidden addition of medicines in health care products is often restricted. For example: because the phenothiazine psychotropic drugs have a mental tranquilization effect, some illegal persons are in order to improve the efficacy of health-care products, such as improving sleep quality, so that the phenothiazine psychotropic drugs are illegally added into the health-care products. Therefore, the detection method for the content of the illegally added medicines in the health care products, which is simple, quick and accurate in development, is beneficial to the safety monitoring of food and medicines in the market, standardizes the market and ensures the health of people.
In the prior art, due to complex components in the health care product, in the detection process of illegal drug addition, a sample pretreatment process is often required, for example, sample pretreatment technologies such as solid phase extraction, solid phase microextraction, microwave extraction, supercritical fluid extraction and the like are adopted. Although development and application of the pretreatment technology improve the sensitivity and accuracy of detection of illegally added medicines in the health-care products, for a complex system in the health-care products, medicines in the health-care products are separated from the health-care products, physicochemical property analysis is needed to be carried out on a large number of components in the health-care products in the early stage, detection of the medicines can be realized only by pretreatment and elimination of a series of interference substances, and the method is long in time consumption, complicated in treatment process and unfavorable for rapid detection of the medicines.
Disclosure of Invention
Based on the above, the invention aims to provide a method for analyzing the content of the medicine in the health-care product by tracing with the auxiliary agent, which overcomes the difficulty of separating the to-be-detected substance from the complex system of the health-care product, has simple steps, easy operation, high sensitivity and quick detection, and is suitable for quick analysis of the content of the medicine in the health-care product.
A method for tracing and analyzing the content of medicines in a health product by using auxiliary agents comprises the following steps:
sample preparation: taking a certain amount of health care products, wherein medicines in the health care products can generate photolysis reaction and generate free radicals, adding medicine auxiliary agents into the health care products to obtain samples, carrying out light treatment, wherein the medicine auxiliary agents can capture the free radicals generated by the medicines in the health care products in the photolysis process and generate a first component, the boiling point of the first component in the sample after light treatment is the lowest, and the rest is marked as a first mixture;
gas-liquid separation and derivatization treatment: separating the first component from the first mixture in the illuminated sample by gas-liquid separation, absorbing the first component with a derivatizing agent to obtain an absorption solution, and developing color;
and (3) detection: and determining the content of the medicine in the health product by adopting a colorimetry method or by measuring an ultraviolet-visible absorbance value, wherein the ultraviolet-visible absorbance value is measured at a specific wavelength, and the specific wavelength is the wavelength at the absorption peak of the absorption liquid.
The invention utilizes the auxiliary agent of the medicine to capture the free radical generated in the photolysis process of the medicine in the health care product to generate a volatile first component, then combines the gas-liquid separation technology to separate the low boiling point first component from the first mixture, finally derives the first component and the derivatization reagent for color development, and adopts a colorimetry or determines the content of the medicine in the health care product by measuring the ultraviolet-visible absorbance value under specific wavelength. Different light sources and illumination time are selected according to different medicines in the health care product. Preferably, the light source and the illumination time can lead the medicine in the health care product to be completely photolyzed. The method for tracing and analyzing the content of the medicine in the health care product by the auxiliary agent shortens the time required by the pretreatment of the sample, greatly simplifies the detection and analysis process of the medicine in the health care product, and has simple steps and high sensitivity.
Further, the light source of illumination is one of sunlight, indoor natural light and ultraviolet light with the wavelength of 200-400nm, and the time of illumination is more than 2 hours. Generally, different light sources and illumination time are selected according to different medicines in the health care product, and the complete photolysis of the medicines in the health care product is ensured according to the selection of the light sources and the illumination time.
Further, the sample is a solution, the addition amount of the pharmaceutical auxiliary agent is at least 5% of the volume fraction of the sample solution, and the pharmaceutical auxiliary agent is an alcohol compound. If the addition amount of the drug auxiliary agent is too low, free radicals generated in the photodecomposition process of the drug in the health product can be captured, so that the subsequent detection can be influenced; the alcohol compound is used as a pharmaceutical auxiliary agent, the first component generated after the alcohol compound captures free radicals is a volatile component, is an aldehyde compound, has large chemical property difference with the components in the health care product, and has relatively active chemical property. Preferably, the alcohol compound is one of methanol, ethanol, propanol, isopropanol and butanol. The methanol, ethanol, propanol, isopropanol and butanol can further generate corresponding aldehydes with high volatility and low boiling point, and gas-liquid separation is facilitated.
Further, the derivatizing agent is one of acetylacetone, a phenol reagent, a schiff reagent and AHMT. The corresponding derivatizing reagent is selected according to aldehydes, and the derivatization color is developed.
Further, the derivatizing reagent also includes an acidic ferric ion reagent. The acidic ferric ion reagent further oxidizes the derivatized conjugate of the derivatizing reagent with the first component, stabilizing the color development.
Further, the drug is chlorpromazine hydrochloride, the drug auxiliary agent is ethanol, the free radical is hydroxyl free radical, and the first component is acetaldehyde. Chlorpromazine hydrochloride can generate photolysis reaction and hydroxyl radicals, and the hydroxyl radicals are captured by ethanol to generate acetaldehyde.
Further, a cascade purging and trapping device is adopted for carrying out gas-liquid separation and derivatization treatment, and the cascade purging and trapping device comprises a primary gas washing system, a secondary sample volatilizing system and a tertiary sample absorbing system which are sequentially communicated; the primary scrubbing system includes a first absorber tube containing a solution capable of removing the first component; the secondary sample volatilization system comprises a light shielding pipe for containing the illuminated sample and a heater for heating the illuminated sample; the tertiary sample absorption system includes a second absorption tube containing a derivatizing reagent of the first component. The cascade purging and trapping device can complete the steps of gas-liquid separation and derivatization, simplify the processing process of the sample, eliminate interference and reduce errors.
Further, the first absorption tube is a Bo's absorption tube, a gas flow rate controller is further arranged between the primary gas washing system and the secondary sample volatilizing system, the light shielding tube is a brown Bo's absorption tube, the second absorption tube is a U-shaped absorption tube, and the outlet end of the U-shaped absorption tube is designed by adopting a porous gasket and is provided with a ball cavity. Controlling the flow rate of the gas flowing into the brown Bosch absorber tube through a gas flow rate controller to enable the volatile first component to flow out along with the gas flow; adopt U type design, when no air current passes through, U type absorption tube bottom is stored to the absorption liquid, when blowing, the absorption liquid is blown to U type absorption tube exit end, the exit end of U type absorption tube is for adopting the design of porous gasket and be equipped with the ball die cavity, divide into more dense little air current with the atmospheric air flow in the pipe, it is not enough to promote the absorption liquid and shift up, make it stay in the gasket upper end, prevent that it from blowing out from the intraductal, the little air current that carries the first component simultaneously will blow out from the absorption liquid bottom, increase gas dwell time and area of contact in the absorption liquid simultaneously, make the first component that volatilizees fully absorbed.
Further, the colorimetric method for determining the content of the medicine in the health care product comprises the following steps of:
under the same conditions, preparing a series of standard solutions of the medicines with concentration gradients, respectively taking the standard solutions of the medicines with the same amount as the health care products, respectively adding medicine auxiliary agents into the standard solutions of the medicines, carrying out light treatment, respectively carrying out gas-liquid separation and derivatization treatment for color development, and preparing a concentration-color comparison card;
and comparing the color of the absorption liquid obtained by carrying out gas-liquid separation and derivatization treatment on the illuminated sample with a concentration-color colorimetric card, and determining the content of the medicine in the health product.
The colorimetry is used for qualitatively or semi-quantitatively determining the content of the medicine in the health care product by comparing the colors of the absorption liquid, complicated separation and detection equipment is not needed, and the method is convenient and quick.
Further, the step of determining the drug content in the health product by measuring the ultraviolet-visible absorbance value is:
under the same conditions, preparing a series of standard solutions of the medicines with concentration gradients, respectively taking standard solutions of the medicines with the same amount as the health care products, respectively adding medicine auxiliary agents into the standard solutions of the medicines, carrying out light treatment, respectively carrying out gas-liquid separation and derivatization treatment for color development, respectively measuring ultraviolet-visible absorbance values under the same specific wavelength, and drawing a standard curve of the concentration-ultraviolet-visible absorbance values to obtain a first linear regression equation;
substituting the ultraviolet-visible absorbance value of the absorption liquid of the sample subjected to gas-liquid separation and derivatization treatment into the first linear regression equation, and determining the content of the medicine in the health product.
The content of the medicine in the health product is quantitatively determined by measuring the ultraviolet-visible absorbance value of the absorption liquid at a specific wavelength, complex separation and detection equipment is not needed, the method is convenient and quick, and the result is more accurate.
For a better understanding and implementation, the present invention is described in detail below with reference to the drawings.
Drawings
FIG. 1 is a schematic diagram of a cascade purge capture apparatus of the present invention;
FIG. 2 is a graph of the photolytic mechanism of phenothiazines;
FIG. 3 is a diagram of the molecular photolysis mechanism of chlorpromazine hydrochloride;
FIG. 4 is a chromatogram of an HPLC-SPD-FL method for detecting an illuminated solution, wherein FIG. a is a fluorescent chromatogram, FIG. b is an ultraviolet chromatogram, 1 represents an illuminated TPA and HTA mixed standard solution, 2 represents an illuminated aqueous solution of chlorpromazine hydrochloride containing TPA, and 3 represents an illuminated solution of chlorpromazine hydrochloride containing TPA and 10% volume fraction ethanol;
FIG. 5 is a mass spectrum of 2-hydroxy promazine in a solution after LC-MS detection and illumination, wherein FIG. a is a mass spectrum of 2-hydroxy promazine in chlorpromazine hydrochloride solution without ethanol, and FIG. b is a mass spectrum of 2-hydroxy promazine in chlorpromazine hydrochloride solution with 10% ethanol by volume fraction;
FIG. 6 is a graph of the mass spectrum of 2-ethoxypromazine in a solution after LC-MS detection and illumination, wherein FIG. a is a graph of the mass spectrum of 2-ethoxypromazine in a chlorpromazine hydrochloride solution without ethanol, and FIG. b is a graph of the mass spectrum of 2-ethoxypromazine in a chlorpromazine hydrochloride solution with 10% ethanol by volume fraction;
fig. 7 is an ultraviolet-visible light detection diagram of chlorpromazine hydrochloride standard sample constant volume liquid, wherein fig. a is a linear regression fitting diagram, and fig. b is an ultraviolet-visible light scanning diagram;
FIG. 8 is an ultraviolet-visible light detection diagram of the constant volume liquid of the health product sample.
Detailed Description
In order to further illustrate the invention, the embodiment takes the health care product containing the illegal addition of the phenothiazine psychotropic drugs as an example, and the method for tracing and analyzing the drug content in the health care product by the auxiliary agent is described in detail. However, it will be appreciated by those skilled in the art that the specific examples are intended to be illustrative of the principles of the present invention and not to limit the invention to alternative embodiments, and that the determination of the drug content based on actual health products may be performed by those skilled in the art using the methods of the present invention as well.
Specifically, in the embodiment, a health care product containing a phenothiazine psychotropic drug chlorpromazine hydrochloride is taken as an example, namely, the health care product contains a certain amount of chlorpromazine hydrochloride, and ethanol which is a common drug solvent is adopted as a drug auxiliary agent, so that hydroxyl free radicals generated after the chlorpromazine hydrochloride is photolyzed can be captured by the ethanol to generate acetaldehyde. The phenol reagent is used for derivatization and absorption of acetaldehyde, and can be used for derivatization and color development with acetaldehyde.
In other embodiments, in addition to ethanol as a pharmaceutical adjuvant, one of the alcohol compounds such as methanol, propanol, isopropanol, and butanol can be selected as a pharmaceutical adjuvant. In addition to using a phenol reagent as the derivatizing reagent, one of acetylacetone, a schiff reagent (fuchsin sulfurous acid reagent), and AHMT (4-amino-3-hydrazino-5-mercapto-1, 2, 4-triazole) can be selected as the derivatizing reagent. According to different application scenes and requirements, proper pharmaceutical auxiliary agents and derivatization reagents are selected.
The method for tracing and analyzing the drug content in the health care product by the auxiliary agent comprises the following specific steps:
(1) Preparing a health product sample liquid and a standard sample liquid:
respectively taking a certain and equivalent amount of health care product solution and chlorpromazine hydrochloride standard solutions (2.5, 5.0, 10.0, 15.0 and 20.0 mug/mL) with different concentrations, respectively mixing the solutions with ethanol according to a ratio of 1: mixing at a volume ratio of 1 to obtain a health product sample solution and a chlorpromazine hydrochloride standard sample solution, respectively adopting 365nm wavelength ultraviolet irradiation for 15min, and preserving in dark, wherein the ultraviolet irradiation power radiation density is 882W/m 2 。
In the embodiment, after ultraviolet irradiation with 365nm wavelength is adopted for 15min, chlorpromazine hydrochloride is completely photolyzed; in other embodiments, ultraviolet light with wavelength of 200-400nm, indoor natural light and sunlight can be used as light source illumination, for example, the sunlight can be completely decomposed within 5min in summer in noon in two broad areas, and no sunlight (cloudy days) is basically decomposed by adopting indoor light for more than 2h. The illumination time is selected according to the degree of medicine photolysis, and the optimal illumination light source and illumination time can lead the medicine in the health care product to be completely photolyzed.
(2) Gas-liquid separation and derivatization treatment:
in this embodiment, a cascade purge and trap device is used for gas-liquid separation and derivatization, refer to fig. 1, which is a schematic diagram of the cascade purge and trap device of the present invention, where the cascade purge and trap device includes a primary gas washing system, a secondary sample volatilizing system and a tertiary sample absorbing system that are sequentially connected; the primary scrubbing system includes a first absorber tube containing a solution capable of removing the first component; the secondary sample volatilization system comprises a light shielding pipe for containing the sample liquid after illumination and a heater for heating the sample liquid; the tertiary sample absorption system includes a second absorption tube containing a derivatizing reagent of the first component. In this embodiment, the first absorption tube is a Bo absorption tube containing potassium dichromate solution, a gas flow rate controller is further arranged between the primary gas washing system and the secondary sample volatilizing system, the light shielding tube is a brown Bo absorption tube, the second absorption tube is a U-shaped absorption tube containing water and phenol reagents, and an outlet end of the U-shaped absorption tube is designed by adopting a porous gasket and is provided with a ball cavity.
Specifically, 1.000mL of the health product sample liquid and the chlorpromazine hydrochloride standard sample liquid which are subjected to ultraviolet irradiation in the step (1) for 15min are respectively taken and respectively placed in a brown Bo absorption tube, the flow rate of gas is controlled to be 100mL/min after air is introduced into a potassium dichromate solution, the brown Bo absorption tubes are respectively heated at constant temperature in an aqueous solution at 80 ℃, and the U-shaped absorption tubes containing 4mL of water and 0.6mL of phenol reagent are used for absorbing for 10min, so that the health product sample absorption liquid and the chlorpromazine hydrochloride standard sample absorption liquid are respectively obtained.
After air is washed by the Bo absorption tube containing potassium dichromate (removing acetaldehyde possibly existing in the air), a gas flow rate controller controls the gas flow rate, the gas is introduced into the heated brown Bo absorption tube, and the gas brings out the acetaldehyde which is a volatile component in the health-care product sample liquid after 15min of ultraviolet irradiation or the chlorpromazine hydrochloride standard sample liquid after 15min of ultraviolet irradiation, and the acetaldehyde is introduced into the U-shaped absorption tube to be absorbed by water and phenol reagents.
In this example, water and phenol reagent are used as derivatizing reagent to develop color in the U-shaped absorption tube, and acidic ferric ammonium sulfate solution is further added to develop color.
Specifically, after the absorption is finished, the health product sample absorption liquid and the chlorpromazine hydrochloride standard sample absorption liquid are respectively transferred into a 10mL glass tube, the transfer is carried out by 3 times of rinsing with 1mL of ultrapure water, shaking is carried out evenly, 200 mu L of acidic ferric ammonium sulfate solution is added after 2min, the mixture is taken out after being fully shaking and heated in a water bath kettle at 35 ℃ for 15min, and the volume of the health product sample constant volume liquid and the chlorpromazine hydrochloride standard sample constant volume liquid are obtained by the constant volume and shaking of ultrapure water.
(3) And (3) detection:
recording the color of the constant volume liquid of the health product sample obtained in the step (2), and measuring the ultraviolet-visible absorbance A of the constant volume liquid of the health product sample at 665nm wavelength. Determining the content of chlorpromazine hydrochloride in the health product by adopting a colorimetric method or measuring an ultraviolet-visible absorbance value. And (3) respectively recording the concentration of the chlorpromazine hydrochloride standard solution in the step (1) and the color of the chlorpromazine hydrochloride standard sample constant volume liquid in the corresponding step (2), making a concentration-color colorimetric card, respectively measuring the ultraviolet-visible absorbance A of the chlorpromazine hydrochloride standard sample constant volume liquid at 665nm wavelength, drawing a standard curve by taking the concentration c as the abscissa and the ultraviolet-visible absorbance A as the ordinate, and obtaining a linear regression equation of the standard curve.
Determining the content of chlorpromazine hydrochloride in the health product by adopting a colorimetric method or measuring an ultraviolet-visible absorbance value. Specifically, in this embodiment, the principle of determining the content of chlorpromazine hydrochloride in the health product is as follows:
please refer to fig. 2, which is a diagram of a photodissociation mechanism of a phenothiazine drug, wherein the phenothiazine drug is easy to undergo a photodissociation reaction under an illumination condition to generate free radicals; the free radicals react with water to form hydroxyl free radicals, and the hydroxyl free radicals are captured by ethanol serving as a pharmaceutical adjuvant to generate acetaldehyde; and then derivatizing and developing by using a phenol reagent and acetaldehyde. In this embodiment, please refer to fig. 3, which is a diagram of a mechanism of chlorpromazine hydrochloride molecule photolysis, wherein the chlorpromazine hydrochloride molecule becomes a high-excitation molecule and decomposes to generate free radicals under the condition of illumination, and a series of cascade reactions occur; the free radical reacts with water in the solvent to form a hydroxyl radical, which is captured by ethanol as a pharmaceutical adjuvant to form acetaldehyde.
Further, in order to verify that chlorpromazine hydrochloride generates hydroxyl radicals in the photolysis process, experimental verification is also performed on the photolysis mechanism process of chlorpromazine hydrochloride in the embodiment. In this example, the presence of hydroxyl radicals in chlorpromazine hydrochloride solution was demonstrated by high performance liquid chromatography-diode array-fluorescence detector (HPLC-SPD-FL) method, and further confirmed by liquid chromatography-mass spectrometry (LC-MS) method that the chlorpromazine hydrochloride molecule generated hydroxyl radicals during photolysis, and also confirmed ethoxy (C) 2 H 5 O.cndot.) free radical reaction process, specifically as follows:
terephthalic acid (TPA) is a commonly used fluorescent probe molecule for detecting hydroxyl radicals, TPA is non-fluorescent per se, but the generated hydroxyphthalic acid (HTA) after reacting with the hydroxyl radicals has fluorescence, and the product is single and stable, and has been widely used in the catalysis field to prove that the hydroxyl radicals are generated in the reaction process. Since other photolytic products of chlorpromazine hydrochloride also have fluorescence, HTA needs to be detected after separation from other fluorescent products, and thus high performance liquid chromatography-diode array-fluorescence detector (HPLC-SPD-FL) combination method with good definite ability is used to detect HTA in chlorpromazine hydrochloride.
After adding TPA into chlorpromazine hydrochloride solution, light is irradiated, and high performance liquid chromatography-diode array-fluorescence detector (HPLC-SPD-FL) combined method is used for detecting whether HTA is generated or not to prove the generation of hydroxyl free radicals. As a result, referring to fig. 4, which is a chromatogram of an illuminated solution detected by the HPLC-SPD-FL method, referring to fig. 4, which is a fluorescence chromatogram, the illuminated mixed standard solution 1 of TPA and HTA, the illuminated aqueous solution 2 of chlorpromazine hydrochloride containing TPA, and the illuminated solution 3 of chlorpromazine hydrochloride containing TPA and 10% volume fraction ethanol all have fluorescence chromatographic peak responses, that is, HTA is generated, which can prove that hydroxyl radicals are generated during the chlorpromazine hydrochloride photolysis process. Further comparing, the peak height of 3 is lower than that of 2, that is to say, the content of HTA generated by the chlorpromazine hydrochloride alcohol solution after illumination is lower than that of the chlorpromazine hydrochloride aqueous solution, because ethanol can be used as a hydroxyl radical capturing agent and can compete with TPA to capture hydroxyl radicals, thereby reducing the yield of HTA; thus, this side demonstrates that ethanol can capture hydroxyl radicals generated during chlorpromazine hydrochloride illumination, ultimately forming acetaldehyde. Referring to fig. 4, panel b, which is a uv chromatogram, the uv detector does not detect the uv response peaks of HTA of 2 and 3, which is due to the weak uv signal and strong fluorescence signal of HTA itself; TPA has only an ultraviolet absorbance signal and no fluorescence signal; making it a common reagent for proving the presence of hydroxyl radicals.
To gain insight into the mechanism of chlorpromazine hydrochloride photolysis and acetaldehyde generation upon addition of ethanol, we identified two chlorpromazine hydrochloride photolysis products associated with the free radical process using liquid chromatography-mass spectrometry (LC-MS). Please refer to fig. 5, which shows a mass spectrum of 2-hydroxy promazine in the solution after LC-MS detection and illumination, wherein fig. a shows a mass spectrum of 2-hydroxy promazine in chlorpromazine hydrochloride solution without ethanol, and fig. b shows a mass spectrum of 2-hydroxy promazine hydrochloride in chlorpromazine hydrochloride solution with 10% ethanol by volume fraction; the result shows that no matter whether ethanol auxiliary agent is added, an m/z= 301.14 molecular ion peak is detected, and the abundance ratio of m/z= 302.06 to m/z= 301.13 is close to 18.4 percent, which is completely matched with the isotope theoretical distribution ratio of 2-hydroxy promazine, so that the substance can be estimated to be the product of the chlorpromazine hydrochloride after dechlorination and being replaced by hydroxyl radicals, namely the 2-hydroxy promazine according to the isotope mass spectrometry identification method; this demonstrates from the side that free radicals are generated during chlorpromazine hydrochloride photolysis.
Referring to fig. 6, a mass spectrum of 2-ethoxypromazine in a solution after LC-MS detection and illumination is shown, wherein fig. a is a mass spectrum of 2-ethoxypromazine in a chlorpromazine hydrochloride solution without ethanol, and fig. b is a mass spectrum of 2-ethoxypromazine in a chlorpromazine hydrochloride solution with 10% ethanol by volume fraction; the results showed that m/z= 329.22 molecular ion peaks were not generated in the absence of ethanol, whereas in the presence of ethanol; m/z= 330.22 molecular ion peak to abundance ratio close to 1:5, matching with the isotope theory distribution proportion of the 2-ethoxypromazine, so that the substance can be presumed to be a product obtained by dechlorinating chlorpromazine hydrochloride and replacing the chlorpromazine hydrochloride by ethoxy, namely the 2-ethoxypromazine according to the isotope mass spectrometry identification method; in this context, however, ethoxy groups can only be derived from ethanol. Thus, it can be presumed that ethanol participates in the radical reaction process. The formation of acetaldehyde may be the reaction of hydroxyl radicals with ethanol to form ethoxy (C 2 H 5 O.radical, ethoxy (C) 2 H 5 O.cndot.) the radicals react with hydroxyl radicals to form acetaldehyde.
In the embodiment, the sample solution is obtained by mixing the health-care product solution and ethanol, ultraviolet irradiation is adopted for 15min, and chlorpromazine hydrochloride in the health-care product is completely photodecomposition to generate hydroxyl free radicals after the ultraviolet irradiation is carried out for 15min, and the hydroxyl free radicals are captured by the ethanol to generate acetaldehyde; and (3) separating acetaldehyde from the sample liquid after the ultraviolet irradiation for 15min through a cascade purging and trapping device, wherein after the aldehyde gas in the air is removed through the potassium dichromate solution, the gas flow rate is controlled by a gas flow rate controller, and the gas flow rate controller is introduced into a Brown Baoshi absorption tube which is heated by a constant-temperature water bath and contains the sample liquid after the ultraviolet irradiation for 15min, so that the acetaldehyde is separated from the solution along with the outflow of the gas, and then introduced into a derivatization reagent consisting of water and a phenol reagent in a U-shaped absorption tube to fully absorb the acetaldehyde gas flowing along with the gas.
In the embodiment, water and a phenol reagent are used as derivatization reagents, the phenol reagent absorbs acetaldehyde to be derivatized into blue oxazine compounds, and the oxazine compounds are oxidized by ferric ions in an acidic environment to form blue-green compounds for further color development.
The embodiment adopts a colorimetric method or determines the content of chlorpromazine hydrochloride in the health-care product by measuring the ultraviolet-visible absorbance value, and the method comprises the following steps:
colorimetric detection: in the range of 2.5-20.0 mug/mL of chlorpromazine hydrochloride standard solution concentration, along with the increase of the chlorpromazine hydrochloride standard solution concentration, the blue-green color of the chlorpromazine hydrochloride standard sample constant volume liquid is gradually deepened, the concentration of the chlorpromazine hydrochloride standard solution and the color of the chlorpromazine hydrochloride standard sample constant volume liquid corresponding to the concentration are recorded, and a concentration-color ratio is formed. And comparing the color of the constant volume liquid of the health product sample with the color comparison card, and qualitatively or semi-quantitatively determining the content of chlorpromazine hydrochloride in the health product.
Measuring ultraviolet-visible absorbance value method detection: please refer to fig. 7, which is a graph of ultraviolet-visible absorbance detection of a chlorpromazine hydrochloride standard sample constant volume solution, wherein fig. a is a linear regression fit graph, and fig. b is an ultraviolet-visible light scan graph; in the range of 2.5-20.0 mug/mL of chlorpromazine hydrochloride standard solution concentration, the ultraviolet-visible absorbance value of the chlorpromazine hydrochloride standard sample constant volume liquid gradually increases along with the increase of the chlorpromazine hydrochloride standard solution concentration, the linear regression equation of the standard curve is y=0.0396x+0.1062, wherein x represents the concentration of the chlorpromazine hydrochloride standard solution, y represents the ultraviolet-visible absorbance value, and the correlation coefficient R 2 =0.9890, lod=0.5 μg/mL, indicating that ultra-trace chlorpromazine hydrochloride uv-vis absorbance detection can be met. Substituting the ultraviolet light intensity detection value A of the constant volume liquid of the health product sample obtained in the step (3) into a linear regression equation y=0.0396x+0.1062 of the constant volume liquid of the chlorpromazine hydrochloride standard sample, wherein the obtained result is the chlorpromazine hydrochloride in the health product solutionIs a concentration of (3).
Specifically, referring to fig. 8, the ultraviolet scanning curve of the constant volume solution of the health product sample is consistent with chlorpromazine hydrochloride, and the initial qualitative description shows that the sample solution contains chlorpromazine hydrochloride, the absorbance a=0.612 is read at 665nm, and the result is calculated to be 12.8 mug/mL by substituting the absorbance a=0.0396x+0.1062 into a linear regression equation, namely, the concentration of chlorpromazine hydrochloride in the health product solution is 12.8 mug/mL.
The invention captures free radicals generated in the photolysis process of illegally added medicines in the health care product by utilizing the auxiliary medicines to generate volatile first components, then separates out the low-boiling-point first components by combining a gas-liquid separation technology, finally develops the first components by derivatization with a derivatization reagent, and determines the medicine content in the health care product by adopting a colorimetry or by measuring ultraviolet-visible absorbance values under specific wavelengths. Compared with the prior art, the method for analyzing the drug content in the health care product by tracing the auxiliary agent shortens the time required by sample pretreatment, greatly simplifies the detection and analysis process of the drug in the health care product, and has simple steps and high sensitivity.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that modifications and improvements can be made by those skilled in the art without departing from the spirit of the invention, and the invention is intended to encompass such modifications and improvements.
Claims (5)
1. A method for tracing and analyzing the content of medicines in a health product by using auxiliary agents is characterized by comprising the following steps: the method comprises the following steps:
sample preparation: taking a certain amount of health care products, wherein medicines in the health care products can generate photolysis reaction and generate free radicals, adding medicine auxiliary agents into the health care products to obtain samples, carrying out light treatment, wherein the medicine auxiliary agents can capture the free radicals generated by the medicines in the health care products in the photolysis process and generate a first component, the boiling point of the first component in the sample after light treatment is the lowest, and the rest is marked as a first mixture;
wherein the sample is a solution, the addition amount of the pharmaceutical auxiliary agent is at least 5% of the volume fraction of the sample solution, and the pharmaceutical auxiliary agent is an alcohol compound; the medicine is chlorpromazine hydrochloride, the free radical is a hydroxyl free radical, and the first component is a product generated after the alcohol compound captures the hydroxyl free radical;
gas-liquid separation and derivatization treatment: separating the first component from the first mixture in the illuminated sample by gas-liquid separation, absorbing the first component with a derivatizing agent to obtain an absorption solution, and developing color;
the gas-liquid separation and derivatization treatment is carried out by adopting a cascade purging and trapping device, wherein the cascade purging and trapping device comprises a primary gas washing system, a secondary sample volatilizing system and a tertiary sample absorbing system which are sequentially communicated; the primary scrubbing system includes a first absorber tube containing a solution capable of removing the first component; the secondary sample volatilization system comprises a light shielding pipe for containing the illuminated sample and a heater for heating the illuminated sample; the tertiary sample absorption system includes a second absorption tube containing a derivatizing agent for the first component;
the first absorption tube is a Bo absorption tube, a gas flow rate controller is arranged between the primary gas washing system and the secondary sample volatilizing system, the light shielding tube is a brown Bo absorption tube, the second absorption tube is a U-shaped absorption tube, and the outlet end of the U-shaped absorption tube is designed by adopting a porous gasket and is provided with a ball cavity;
and (3) detection: determining the content of the medicine in the health product by colorimetry or by measuring ultraviolet-visible absorbance values, wherein the ultraviolet-visible absorbance values are measured at specific wavelengths, and the specific wavelengths are wavelengths at absorption peaks of the absorption liquid;
wherein, the colorimetric method for determining the content of the medicine in the health care product comprises the following steps:
under the same conditions, preparing a series of standard solutions of the medicines with concentration gradients, respectively taking the standard solutions of the medicines with the same amount as the health care products, respectively adding medicine auxiliary agents into the standard solutions of the medicines, carrying out light treatment, respectively carrying out gas-liquid separation and derivatization treatment for color development, and preparing a concentration-color comparison card; comparing the color of the absorption liquid after the gas-liquid separation and derivatization treatment of the illuminated sample with a concentration-color colorimetric card to determine the content of the medicine in the health care product;
the method for determining the drug content in the health product by measuring the ultraviolet-visible absorbance value comprises the following steps:
under the same conditions, preparing a series of standard solutions of the medicines with concentration gradients, respectively taking standard solutions of the medicines with the same amount as the health care products, respectively adding medicine auxiliary agents into the standard solutions of the medicines, carrying out light treatment, respectively carrying out gas-liquid separation and derivatization treatment for color development, respectively measuring ultraviolet-visible absorbance values under the same specific wavelength, and drawing a standard curve of the concentration-ultraviolet-visible absorbance values to obtain a first linear regression equation; substituting the ultraviolet-visible absorbance value of the absorption liquid of the sample subjected to gas-liquid separation and derivatization treatment into the first linear regression equation, and determining the content of the medicine in the health product.
2. The method for adjuvant trace analysis of drug content in a health product according to claim 1, wherein: the light source for illumination is one of sunlight, indoor natural light and ultraviolet light with the wavelength of 200-400nm, and the time for illumination is more than 2 hours.
3. The method for adjuvant trace analysis of drug content in a health product according to claim 1, wherein: the derivatization reagent is one of acetylacetone, a phenol reagent, a Schiff reagent and AHMT.
4. A method for adjuvant trace analysis of drug content in a health product according to claim 3, wherein: the derivatizing reagent also includes an acidic ferric ion reagent.
5. The method for adjuvant trace analysis of drug content in a health product according to claim 1, wherein: the pharmaceutical adjuvant is ethanol, and the first component is acetaldehyde.
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