CN102565222A - Ion chromatography-online photochemical derivatization-fluorescence analysis system for measuring carbamazepine content in tablets - Google Patents
Ion chromatography-online photochemical derivatization-fluorescence analysis system for measuring carbamazepine content in tablets Download PDFInfo
- Publication number
- CN102565222A CN102565222A CN2011104422193A CN201110442219A CN102565222A CN 102565222 A CN102565222 A CN 102565222A CN 2011104422193 A CN2011104422193 A CN 2011104422193A CN 201110442219 A CN201110442219 A CN 201110442219A CN 102565222 A CN102565222 A CN 102565222A
- Authority
- CN
- China
- Prior art keywords
- fluorescence
- online
- carbamazepine
- ion chromatography
- analysis system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to an ion chromatography-online photochemical derivatization-fluorescence detection system, in particular to an ion chromatography-online photochemical derivatization-fluorescence analysis system for measuring the carbamazepine content in tablets. The ion chromatography-online photochemical derivatization-fluorescence analysis system comprises a liquid chromatographic pump, a sample valve, an ion chromatographic column, a self-made photochemical reaction device, a power supply and a fluorescence detector. A polar organic compound or homologs thereof which have or do not have weak fluorescence intensity are separated on the ion chromatographic column, and the separated components are oxidized into hyperfluorescence substances on line in the self-made photochemical reaction device and detected and analyzed by the fluorescence detector. Signals are recorded and processed by a chromatographic work station. The ion chromatography-online photochemical derivatization-fluorescence analysis system is of a single-pump and single-flow-passage structure, adopts an online oxidization mode, is rapid and sensitive and can be used for detection and analysis on certain specific organic matters in biology and medicine.
Description
Technical field
The present invention relates to the using system that a kind of chemical apparatuses is analyzed, particularly relate to the chromatography of ions-online photochemistry that detects carbamazepine and derive-system of fluorescence analysis.
Background technology
Epilepsy has another name called " epilepsy "; Be that multiple reason causes the unusual a kind of disease of paroxysmal movement, sensation, consciousness, spirit, vegetative nerve function due to the brain neuroblastoma unit crowd paroxysmal paradoxical discharge, wherein 70%-80% is local outbreak, and drug therapy is the main method in the epilepsy therapy; Carbamazepine (Carbamazepine; CBZ) be one of partial seizures choice drug, also can effectively control polytype epileptic attack, carbamazepine has membrane stabilizing action; Also be used for prosopalgic treatment, so clinical practice is extensive.Carbamazepine listing formulation is mainly tablet; Line medicine as prevention, treatment epilepsy; Its bulk drug and preparation content determining method thereof are in that " Chinese pharmacopoeia was employed in 285nm wavelength spectrophotometry content in 2005 in the version; Impurity in that 285nm wavelength content is higher is extremely similar with the ultra-violet absorption spectrum of carbamazepine, adopts spectrophotometry content that interference is arranged to carbamazepine, can not truly reflect the actual content of carbamazepine; Present most of bibliographical information is measured the concentration of carbamazepine in Carbamazepine Tablets content and the blood plasma with the HPLC method; In recent years, the LC-MS technology is developed with corresponding instrument and has obtained certain popularization and application, but this kind method institute use instrument costs an arm and a leg; Operating cost is high, should not promote operation.For security and the validity that improves medication, need carry out carbamazepine medicine quality control accurately.
Carbamazepine does not have photoluminescent property under acid condition, through deriving, can make it become the material with hyperfluorescence character, detects with fluorescence method, and common deriving method has chemical derivatization.Chemical derivatization need consume chemical reagent, wastes time and energy.It is with the novel fluorescence analysis method of photon as derivative reagent that photochemistry is derived.Because the adding of photon can not introduced impurity in reaction system, can diluted sample yet, avoided adding chemically derived many unfavorable factors.The present invention has set up the IC-PCF method of Carbamazepine Tablets assay, and method is verified.Investigate anti-insane new drug Oxcarbazepine (Oxcarbazepine, separation case OXC) etc. with related substance carbamazepine (CBZ) similar.The result shows: this law is accurately and reliably, good reproducibility, specificity be strong, disturb less, fast, the result is accurate, is beneficial to and controls product quality better, for the detection of blood concentration new method is provided simultaneously.Up to now, do not see report with chromatography of ions-online photochemistry post-column derivation-fluorescence spectrometry carbamazepine.
Summary of the invention
The present invention is just to the weak point of prior art, provide a kind of chromatography of ions-online photochemistry derive-system of fluorescence analysis is in order to measuring carbamazepine, this system simplification the detection technique of carbamazepine, shortened analysis time.
The present invention is that a kind of chromatography of ions-online photochemistry is derived-fluorescence detecting system; The outlet of anion chromatographic exchange column is joined with self-control photochemical reactor inlet; The inlet of photochemical reactor outlet and fluorescence detector joins; The outlet of fluorescence detector is connected with the waste liquid cylinder, and fluorescence signal is connected with workstation with computing machine through signal wire.
The present invention is through ion chromatographic separation, and some polar organic matters (carbamazepine, Oxcarbazepine) that do not have or have faint fluorescence intensity can be the hyperfluorescence material by online photochemical oxidation, and need not carry out complicated off-line and online chemical oxidization method.
The material that the present invention also can be applied to not have fluorescence or faint photoluminescent property is analyzed or is improved sensitivity and improve detectability.
The present invention has following advantage and effect:
The present invention separates with the chromatography of ions, through the photochemistry post-column derivation, detects with fluorescence detector; Compare with chemically derived, saved a pump and chemical reagent, total system only needs a pump, and a single line stream is simple in structure, has simplified the detection technique of carbamazepine, has shortened analysis time.
Description of drawings
Fig. 1 derives for chromatography of ions-photochemistry-process flow diagram of system of fluorescence analysis;
Among the figure, 1-moving phase; The 2-liquid chromatography pump; The 3-sampling valve; The 4-chromatographic column; 5-uviol lamp and guard shield; The 6-teflon pipe; The 7-fluorescence detector; 8-computing machine and workstation; 9-waste liquid cylinder;
Fig. 2 is the illumination of chromatography of ions-photochemistry post-column derivation-system of fluorescence analysis and the not carbamazepine and the Oxcarbazepine fluorescence signal peak of illumination;
Among the figure, a-illumination, 1-Oxcarbazepine (20.0mgL
-1), 2-carbamazepine (20.0mgL
-1), a '-not illumination.
Embodiment
Through specific embodiment technical scheme of the present invention is further specified below:
As shown in Figure 1: moving phase 1 is carried from liquid chromatography pump 2; Analytic sample is from quantifying ring 3 quantitative sample injections; Component after anion chromatographic exchange column 4 separates is at homemade photochemical reactor 5, and 6 are oxidized to the hyperfluorescence material in the teflon pipe of braiding, and oxidation product is transported to fluorescence detector 7 by homemade photochemical reactor outlet and detects; Signal is by computing machine and workstation 8 records and processing, and the tail washings that the autofluorescence detecting device is discharged is through sewer pipe to waste liquid cylinder 9.
As shown in Figure 2: a is the chromatogram after light is derived, the 1st, and the Oxcarbazepine of 20ppm, the 2nd, the carbamazepine of 20ppm; A ' is the Oxcarbazepine of the 20ppm that do not derive through photochemistry and the chromatogram of carbamazepine.
With the ion chromatograph of U.S. Dai An company (Dionex), and Ion Pac AG11 guard column (4mm * 50mm), Ion Pac AS11 analytical column (4mm * 250mm), with 10mmolL
-1The HCL+10% acetonitrile is a moving phase, and flow rate of mobile phase is 1.0mL/min, and sample size is 25 μ L.Homemade photochemical reactor, fluorescent tube is 18w, and emission wavelength is mainly 254nm, and the pipeline of deriving is that the internal diameter of 20m braiding is the 0.5mm teflon pipe.RF-535 fluorescence detector (day island proper Tianjin company produces), excitation wavelength is 254m, emission wavelength is 478nm.Under this experiment condition, derive-system of fluorescence analysis with chromatography of ions of the present invention-online photochemistry, can be to Determination on content in the carbamazepine tablet, wherein carbamazepine detects and is limited to 0.860 μ gmL
-1
Claims (3)
1. chromatography of ions-online photochemistry is derived-fluorescence detecting system; It is characterized in that; Anion chromatographic exchange column (4) outlet is joined with self-control photochemical reactor (5) inlet; The inlet of photochemical reactor (5) outlet and fluorescence detector (7) joins, and the outlet of fluorescence detector (7) is connected with waste liquid cylinder (9), and fluorescence signal is connected with workstation (8) with computing machine through signal wire.
2. a chromatography of ions-photochemistry is derived-purposes of fluorescence detecting system; It is characterized in that; Pass through ion chromatographic separation; Some polar organic matters (carbamazepine, Oxcarbazepine) that do not have or have faint fluorescence intensity can be the hyperfluorescence material by online photochemical oxidation, and need not carry out complicated off-line and online chemical oxidization method.
3. purposes according to claim 2 is characterized in that, the material that this method also can be applied to not have fluorescence or faint photoluminescent property is analyzed or improved sensitivity and improve detectability.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104422193A CN102565222A (en) | 2011-12-26 | 2011-12-26 | Ion chromatography-online photochemical derivatization-fluorescence analysis system for measuring carbamazepine content in tablets |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104422193A CN102565222A (en) | 2011-12-26 | 2011-12-26 | Ion chromatography-online photochemical derivatization-fluorescence analysis system for measuring carbamazepine content in tablets |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102565222A true CN102565222A (en) | 2012-07-11 |
Family
ID=46411184
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104422193A Pending CN102565222A (en) | 2011-12-26 | 2011-12-26 | Ion chromatography-online photochemical derivatization-fluorescence analysis system for measuring carbamazepine content in tablets |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102565222A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565223A (en) * | 2011-12-26 | 2012-07-11 | 浙江大学 | System for detecting riboflavin in health care product through ion chromatography, on-line photochemical derivation and fluorescence analysis |
| CN114894949A (en) * | 2022-04-12 | 2022-08-12 | 北京清谱科技有限公司 | Lipid fine structure analysis process and control processing system |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565223A (en) * | 2011-12-26 | 2012-07-11 | 浙江大学 | System for detecting riboflavin in health care product through ion chromatography, on-line photochemical derivation and fluorescence analysis |
-
2011
- 2011-12-26 CN CN2011104422193A patent/CN102565222A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565223A (en) * | 2011-12-26 | 2012-07-11 | 浙江大学 | System for detecting riboflavin in health care product through ion chromatography, on-line photochemical derivation and fluorescence analysis |
Non-Patent Citations (3)
| Title |
|---|
| CHAOBIAO HUANG，ET AL: "Flow injection photochemical spectrofluorimetry for the determination of carbamazepine in pharmaceutical preparations", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 任一平等: "柱后光化学衍生荧光检测高效液相色谱法测定食品中的维生素B1", 《分析化学》 * |
| 温裕云等: "柱后光化学衍生荧光检测高效液相色谱法测定动物源性食品中7种磺胺类兽药残留", 《第四届全国环境化学学术大会论文汇编》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102565223A (en) * | 2011-12-26 | 2012-07-11 | 浙江大学 | System for detecting riboflavin in health care product through ion chromatography, on-line photochemical derivation and fluorescence analysis |
| CN114894949A (en) * | 2022-04-12 | 2022-08-12 | 北京清谱科技有限公司 | Lipid fine structure analysis process and control processing system |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| García-Galán et al. | Determination of 19 sulfonamides in environmental water samples by automated on-line solid-phase extraction-liquid chromatography–tandem mass spectrometry (SPE-LC–MS/MS) | |
| Ribeiro et al. | Environmental friendly method for urban wastewater monitoring of micropollutants defined in the Directive 2013/39/EU and Decision 2015/495/EU | |
| Li et al. | A coupled method of on-line solid phase extraction with the UHPLC‒MS/MS for detection of sulfonamides antibiotics residues in aquaculture | |
| de Souza et al. | A simple method for methylmercury, inorganic mercury and ethylmercury determination in plasma samples by high performance liquid chromatography–cold-vapor-inductively coupled plasma mass spectrometry | |
| CN102141551B (en) | Method for simultaneously measuring various drug residues in honey by utilizing liquid chromatogram tandem mass spectrum isotope dilution method | |
| Zhao et al. | Screening of neuraminidase inhibitors from traditional Chinese medicines by integrating capillary electrophoresis with immobilized enzyme microreactor | |
| CN103743826B (en) | A kind of HPLC analytical method of Azilsartan | |
| US8076652B2 (en) | Real-time, on-line analysis of haloacetic acid species and amounts thereof in drinking water supplies | |
| CN104483427A (en) | Method for separating, enriching and detecting 12 antibiotics in drinking water source | |
| Davletbaeva et al. | Flow method based on cloud point extraction for fluorometric determination of epinephrine in human urine | |
| CN109142572A (en) | A variety of drugs are synchronous in a kind of environment multimedium extracts and determination method | |
| Li et al. | Class-specific determination of fluoroquinolones based on a novel chemiluminescence system with molecularly imprinted polymers | |
| CN108732280A (en) | A kind of method of his Wei of separation detection hydrochloric acid Dacca and its optical isomer | |
| Trojanowicz | Flow-injection analysis as a tool for determination of pharmaceutical residues in aqueous environment | |
| Tsiasioti et al. | Automated fluorimetric sensor for glutathione based on zone fluidics | |
| CN103558318B (en) | The assay method of trace oxammonium hydrochloride in a kind of detection of drugs | |
| CN102565222A (en) | Ion chromatography-online photochemical derivatization-fluorescence analysis system for measuring carbamazepine content in tablets | |
| Antil et al. | UPLC method for simultaneous determination of valsartan & hydrochlorothiazide in drug products | |
| CN105738459A (en) | Method for improving blood sodium valproate detection sensitivity | |
| CN103424479B (en) | Analysis method of monensin, salinomycin and lasalocid residues | |
| CN104280473B (en) | The analytical approach of 5 hydroxymethyl furfural in a kind of Linezolid Injection | |
| Li et al. | Determination of bavachin and isobavachalcone in Fructus Psoraleae by high‐performance liquid chromatography with electrochemical detection | |
| CN102565223A (en) | System for detecting riboflavin in health care product through ion chromatography, on-line photochemical derivation and fluorescence analysis | |
| Flores et al. | Flow-through optosensor combined with photochemically induced fluorescence for simultaneous determination of binary mixtures of sulfonamides in pharmaceuticals, milk and urine | |
| CN102565208B (en) | Novel method for detecting etimicin sulfate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120711 |