CN114166976B - 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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- CN114166976B CN114166976B CN202111495713.6A CN202111495713A CN114166976B CN 114166976 B CN114166976 B CN 114166976B CN 202111495713 A CN202111495713 A CN 202111495713A CN 114166976 B CN114166976 B CN 114166976B
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- 239000003814 drug Substances 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 45
- 229940079593 drug Drugs 0.000 title claims abstract description 33
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 26
- 230000036541 health Effects 0.000 title claims description 68
- 238000001212 derivatisation Methods 0.000 claims abstract description 32
- 238000001514 detection method Methods 0.000 claims abstract description 26
- 238000006303 photolysis reaction Methods 0.000 claims abstract description 24
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 18
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 17
- 230000015843 photosynthesis, light reaction Effects 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 65
- AKUVRZKNLXYTJX-UHFFFAOYSA-N 3-benzylazetidine Chemical group C=1C=CC=CC=1CC1CNC1 AKUVRZKNLXYTJX-UHFFFAOYSA-N 0.000 claims description 61
- 229960001657 chlorpromazine hydrochloride Drugs 0.000 claims description 61
- 239000000523 sample Substances 0.000 claims description 57
- 238000010521 absorption reaction Methods 0.000 claims description 52
- 239000007788 liquid Substances 0.000 claims description 52
- 239000000243 solution Substances 0.000 claims description 38
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- 150000003254 radicals Chemical class 0.000 claims description 26
- -1 alcohol compound Chemical class 0.000 claims description 23
- 238000005286 illumination Methods 0.000 claims description 20
- 239000012086 standard solution Substances 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 15
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 10
- 238000012417 linear regression Methods 0.000 claims description 9
- 239000000546 pharmaceutical excipient Substances 0.000 claims description 8
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 6
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- 239000006096 absorbing agent Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004811 liquid chromatography Methods 0.000 claims description 3
- 238000005201 scrubbing Methods 0.000 claims description 3
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- 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 13
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- 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
- 238000010586 diagram Methods 0.000 description 7
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-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
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- 229950000688 phenothiazine Drugs 0.000 description 6
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- 238000005516 engineering process Methods 0.000 description 5
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000006243 chemical reaction 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
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 3
- 150000001793 charged compounds Chemical class 0.000 description 3
- 238000000642 dynamic headspace extraction Methods 0.000 description 3
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 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
- 238000002835 absorbance Methods 0.000 description 1
- 239000012445 acidic reagent Substances 0.000 description 1
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- 238000006555 catalytic reaction Methods 0.000 description 1
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- 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
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 201000011243 gastrointestinal stromal tumor Diseases 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002117 illicit drug Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- 230000003340 mental effect Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 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
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- 229960001836 promazine hydrochloride Drugs 0.000 description 1
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- 230000003860 sleep quality Effects 0.000 description 1
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- 239000002904 solvent Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
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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 first component, deriving the first component from derivatizing reagent to obtain derivatization product, and high-performance liquid chromatography. 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 care product has the function of regulation, is a special food which is not used for treating diseases, and the medicine cannot be illegally added into the health care product. However, in recent years, with the increasing demand of health care products in the market, the phenomenon of forbidden addition of medicines in the 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 process of detecting the content of the illegally added medicine in the health care product, 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, and absorbing the first component with a derivatizing agent to obtain an absorption solution, wherein the derivatizing agent can be derivatized with the first component into a derivatization product;
and (3) detection: and determining the content of the medicine in the health product by adopting a high performance liquid chromatography for the absorption liquid, wherein the high performance liquid chromatography is performed with high performance liquid chromatography detection under a specific wavelength, and the specific wavelength is the wavelength at the chromatographic peak of the derivative product in 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 into a derivatization product, and adopts the high performance liquid chromatography to determine the content of the medicine in the health care product. 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, and the pharmaceutical adjuvant is added in an amount of at least 5% of the volume fraction of the sample solution. 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, and the subsequent detection can be influenced.
Further, the pharmaceutical adjuvant is an alcohol compound. 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.
Further, 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 2, 4-dinitrophenylhydrazine, acetylacetone, a phenol reagent, a schiff reagent and AHMT. And selecting a corresponding derivatization reagent according to the generated aldehyde compound, and derivatizing the derivatization reagent with the aldehyde compound to obtain a derivatization product.
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 step of determining the medicine content in the health product by the high performance liquid chromatography is as follows:
under the same conditions, preparing a series of standard solutions of the medicaments with concentration gradients, respectively taking standard solutions of the medicaments in the same amount as the health care products, respectively adding medicament auxiliary agents into the standard solutions of the medicaments, carrying out light treatment, respectively carrying out gas-liquid separation and derivatization treatment, respectively carrying out liquid chromatography detection under the same specific wavelength, and drawing a standard curve of the concentration of the standard solutions of the medicaments and the peak area of a chromatographic peak of a derivatization product to obtain a first linear regression equation;
substituting the peak area of the chromatographic peak of the derivative product obtained by high performance liquid chromatography detection of the absorption liquid into the first linear regression equation, and determining the content of the medicine in the health product.
The invention adopts liquid chromatography to determine the content of the medicine in the health care product, does not need to adopt complex sample pretreatment technology to separate the medicine from the health care product, and is suitable for detecting the illegal addition of the low-content medicine in the complex health care product of the matrix.
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 a high performance liquid chromatogram of a chlorpromazine hydrochloride standard sample constant volume solution, wherein a graph a is a DNPH-acetaldehyde peak graph, and b is a linear regression fit graph of chlorpromazine hydrochloride standard solution concentration and DNPH-acetaldehyde peak area;
FIG. 8 is a high performance liquid chromatogram of a constant volume solution of a health product sample;
FIG. 9 is a graph showing the effect of different alcohols as radical traps during photodecomposition of chlorpromazine hydrochloride.
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. 2, 4-Dinitrophenylhydrazine (DNPH) is adopted as a derivatization reagent to carry out derivatization reaction with acetaldehyde to generate a derivatization product DNPH-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 2, 4-Dinitrophenylhydrazine (DNPH) as the derivatizing agent, one of acetylacetone, a phenol reagent, 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 agent. 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:
a certain and equivalent amount of health care product solution and chlorpromazine hydrochloride standard solutions (0.1, 0.2, 0.3, 0.4, 0.5, 1.0, 1.5, 2.0, 2.5, 4.0, 6.0, 8.0 and 10.0 mug/mL) with different concentrations are respectively taken, and are respectively mixed 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 after illumination; 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 2, 4-Dinitrophenylhydrazine (DNPH), 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 obtained after the ultraviolet irradiation of the step (1) for 15min are respectively taken and respectively placed in a brown Bao's absorption tube, the flow rate of gas is controlled to be 100mL/min after air is introduced into a potassium dichromate solution, the brown Bao's absorption tube is heated at a constant temperature in an aqueous solution of 80 ℃, and the U-shaped absorption tube containing 4mL of water and 1.0mL of 2mg/mL of 2, 4-dinitrophenylhydrazine solution is used for absorbing for 10min, so that the health product sample absorption liquid and the chlorpromazine hydrochloride standard sample absorption liquid are respectively obtained; and after the absorption is finished, respectively transferring the health product sample absorption liquid and the chlorpromazine hydrochloride standard sample absorption liquid into a 10mL glass tube, rinsing and transferring with 1mL of ultrapure water for 3 times, fully shaking, heating in a water bath kettle at 60 ℃ for 15min, taking out, and fixing the volume with the ultrapure water and shaking to obtain the health product sample constant volume liquid and the chlorpromazine hydrochloride sample constant volume liquid.
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, the gas brings out the acetaldehyde which is a volatile component in a health-care product sample liquid after 15min of ultraviolet irradiation or a chlorpromazine hydrochloride standard sample liquid after 15min of ultraviolet irradiation, and the acetaldehyde is introduced into a U-shaped absorption tube to be absorbed by water and 2, 4-Dinitrophenylhydrazine (DNPH). In this example, water and 2, 4-Dinitrophenylhydrazine (DNPH) are used as derivatizing agents to generate a derivatization product DNPH-acetaldehyde in a U-shaped absorption tube.
(3) And (3) detection:
the conditions of the high performance liquid chromatography are as follows: using a column of Shim-pack GIST C18 (2.1X100 mm,3 μm), mobile phase A:0.1% trifluoroacetic acid; mobile phase B: acetonitrile, gradient elution (0-0.50 min,70.0% A;0.50-5.00min,70.0% A-20.0% A;5.00-6.00min,20.0% A-20.0% A;6.00-6.50min,20.0% A-70.0% A;6.50-9.00min,70.0% A-70.0% A), flow rate: 0.500mL/min, column temperature: 40 ℃, sample injection amount: 10. Mu.L, the detection wavelength was 355nm.
And (3) the constant volume liquid of the health product sample obtained in the step (2) enters a high performance liquid chromatograph for analysis and detection to obtain a chromatogram and the peak area of the chromatographic peak of the derived product DNPH-acetaldehyde.
And (3) respectively feeding the chlorpromazine hydrochloride standard sample constant volume liquid obtained in the step (2) into a high performance liquid chromatograph for analysis and detection to respectively obtain a chromatogram and the peak area of a derived product DNPH-acetaldehyde chromatographic peak, drawing a chlorpromazine hydrochloride standard regression curve by taking the peak area of the DNPH-acetaldehyde chromatographic peak as an ordinate and the concentration of the chlorpromazine hydrochloride standard solution as an abscissa, and obtaining a linear regression equation.
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; then the derivatization with 2, 4-Dinitrophenylhydrazine (DNPH) and acetaldehyde is employed to produce the derivatization product DNPH-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 chlorpromazine hydrochloride solution without ethanol, and FIG. b is a mass spectrum of 10% volume fractionA mass spectrum of 2-ethoxypromazine in chlorpromazine hydrochloride solution of ethanol; 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 with ethanol, and the sample solution is irradiated for 15min by ultraviolet light, and chlorpromazine hydrochloride in the health-care product is completely photodecomposition to generate hydroxyl free radicals after the ultraviolet light is irradiated for 15min, so that acetaldehyde is generated by capturing the hydroxyl free radicals by the ethanol; the acetaldehyde in the sample liquid is separated out through a cascade sweeping and capturing device, after aldehyde gas in the air is removed through potassium dichromate solution, a gas flow rate controller controls a gas flow rate, the gas flow rate controller is introduced into a Brown absorbing tube which is heated by a constant-temperature water bath and contains the sample liquid, so that the acetaldehyde is separated from the solution along with the outflow of the gas, and then the derivatization reagent which is formed by water and 2, 4-Dinitrophenylhydrazine (DNPH) in a U-shaped absorbing tube is introduced to fully absorb the acetaldehyde gas along with the outflow of the gas.
In this example, water and 2, 4-Dinitrophenylhydrazine (DNPH) are used as derivatizing agents, and the 2, 4-Dinitrophenylhydrazine (DNPH) absorbs acetaldehyde to derivatize DNPH-acetaldehyde as a derivatization product.
The embodiment adopts a high performance liquid chromatography to determine the content of chlorpromazine hydrochloride in the health care product, and specifically comprises the following steps:
referring to fig. 7, a high performance liquid chromatogram of a chlorpromazine hydrochloride standard sample constant volume solution is shown, wherein fig. a is a DNPH-acetaldehyde peak diagram, and fig. b is a linear regression fit diagram of chlorpromazine hydrochloride standard solution concentration and DNPH-acetaldehyde peak area; in chlorpromazine hydrochloride standard solution with concentration of 0-10.0 mug/mIn the L range, the peak area of DNPH-acetaldehyde chromatographic peak gradually increases with the increase of chlorpromazine hydrochloride standard solution concentration, and the linear regression equation of the standard curve is y=578517 x+6710.7, wherein x represents chlorpromazine hydrochloride standard solution concentration, y represents DNPH-acetaldehyde peak area, and the correlation coefficient R 2 =0.9990, lod=0.02 μg/mL, indicating that high performance liquid chromatography analysis of ultra trace chlorpromazine hydrochloride can be satisfied.
Referring to fig. 8, the high performance liquid chromatogram of the constant volume solution of the sample of the health product shows that the peak area of the DNPH-acetaldehyde chromatographic peak is 3709220, and the result is calculated to be 6.4 μg/mL by substituting the peak area into the linear regression equation y=578517 x+6710.7, i.e. the concentration of chlorpromazine hydrochloride in the solution of the health product is 6.4 μg/mL.
In other embodiments, in addition to ethanol, methanol, propanol, isopropanol, and butanol may also be used as radical traps for chlorpromazine hydrochloride, with the corresponding products being formaldehyde, propionaldehyde, acetone, and butyraldehyde, respectively; referring to FIG. 9, the corresponding DNPH-formaldehyde, DNPH-propionaldehyde, DNPH-acetone and DNPH-butyraldehyde signals were also detected by HPLC analysis after DNPH derivatization.
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, finally derives the first component and the derivatization reagent into a derivatization product, and adopts the high performance liquid chromatography to determine the content of the medicine in the health care product. 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 (4)
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 product, wherein medicines in the health care product can generate photolysis reaction and generate free radicals, adding a medicine auxiliary agent into the health care product to obtain a sample, carrying out light treatment, wherein the sample is a solution, the adding amount of the medicine auxiliary agent is at least 5% of the volume fraction of the sample solution, the medicine auxiliary agent can capture the free radicals generated by the medicines in the health care product 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 pharmaceutical adjuvant is an alcohol compound, and the alcohol compound is one of methanol, ethanol, propanol, isopropanol and butanol; the medicine is chlorpromazine hydrochloride; the free radical is a 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, and absorbing the first component with a derivatizing agent to obtain an absorption solution, wherein the derivatizing agent can be derivatized with the first component into a derivatization product;
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 care product by adopting a high performance liquid chromatography for the absorption liquid, wherein the high performance liquid chromatography is performed with high performance liquid chromatography detection under a specific wavelength, and the specific wavelength is the wavelength at the chromatographic peak of the derivative product in the absorption liquid;
the high performance liquid chromatography method for determining the medicine content in the health product comprises the following steps:
under the same conditions, preparing a series of standard solutions of the medicaments with concentration gradients, respectively taking standard solutions of the medicaments in the same amount as the health care products, respectively adding medicament auxiliary agents into the standard solutions of the medicaments, carrying out light treatment, respectively carrying out gas-liquid separation and derivatization treatment, respectively carrying out liquid chromatography detection under the same specific wavelength, and drawing a standard curve of the concentration of the standard solutions of the medicaments and the peak area of a chromatographic peak of a derivatization product to obtain a first linear regression equation;
substituting the peak area of the chromatographic peak of the derivative product obtained by high performance liquid chromatography detection of the absorption liquid 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 of illumination is one of sunlight, natural light and ultraviolet light with the wavelength of 200-400nm, and the time of illumination is longer than 2h.
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 2, 4-dinitrophenylhydrazine, acetylacetone, a phenol reagent, a Schiff reagent and AHMT.
4. 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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