CN110361485A - Oxcarbazepine monitor drug concentration kit and its detection method in a kind of blood - Google Patents

Oxcarbazepine monitor drug concentration kit and its detection method in a kind of blood Download PDF

Info

Publication number
CN110361485A
CN110361485A CN201910671617.9A CN201910671617A CN110361485A CN 110361485 A CN110361485 A CN 110361485A CN 201910671617 A CN201910671617 A CN 201910671617A CN 110361485 A CN110361485 A CN 110361485A
Authority
CN
China
Prior art keywords
content
oxcarbazepine
concentration
sample
methanol
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.)
Withdrawn
Application number
CN201910671617.9A
Other languages
Chinese (zh)
Inventor
石功名
何伶秀
孙丹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou Aidimai Medical Technology Co Ltd
Original Assignee
Suzhou Aidimai Medical Technology Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Suzhou Aidimai Medical Technology Co Ltd filed Critical Suzhou Aidimai Medical Technology Co Ltd
Priority to CN201910671617.9A priority Critical patent/CN110361485A/en
Publication of CN110361485A publication Critical patent/CN110361485A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/34Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/86Signal analysis
    • G01N30/8624Detection of slopes or peaks; baseline correction
    • G01N30/8631Peaks

Abstract

The present invention relates to medical detection fields, more particularly to Oxcarbazepine and its metabolite Therapeutic Drug Monitoring kit in a kind of blood based on multidimensional on-line solid phase extraction liquid-phase chromatographic analysis technological development, the method that accurate quantitative analysis detection is more specifically carried out to Oxcarbazepine in blood and its metabolite drug concentration using on-line solid phase extraction and multidimensional liquid-phase chromatographic analysis technology.Kit includes calibration object reagent, quality-control product reagent, treatment fluid, extract liquor, cleaning solution, eluent.Therapeutic Drug Monitoring kit of the invention, blood sample only need centrifugal treating, and it is small to repeat detection variability, Stability and veracity is high, testing cost is low, and every methodology index can meet the needs of Oxcarbazepine and its metabolite Therapeutic Drug Monitoring in blood, easy to spread.

Description

Oxcarbazepine monitor drug concentration kit and its detection method in a kind of blood
Technical field
The present invention relates to medical detection fields, more particularly to one kind to be based on multidimensional on-line solid phase extraction liquid-phase chromatographic analysis Oxcarbazepine and its metabolite Therapeutic Drug Monitoring kit in the blood of technological development, more specifically using online solid Mutually extraction and multidimensional liquid-phase chromatographic analysis technology carry out accurate quantitative analysis to Oxcarbazepine in blood and its metabolite drug concentration The method of monitoring.
Background technique
The anticonvulsant action of Oxcarbazepine and its metabolite is mainly the Voltage-gated Sodium Channels for having blocked brain, To block the propagation of the epilepsy electrical activity of epileptogenic focus.The effective blood drug concentration of Oxcarbazepine and its metabolite is 10-35mg/ L, as blood concentration > 35mg/L, toxic side effect enhancing.Adverse reaction is common out of strength, dizzy, headache etc., accidental stomach and intestine function Energy obstacle, flush, blood count decline etc..Since Oxcarbazepine and its metabolite therapeutic window are relatively narrow, it is metabolized in vivo There are biggish individual differences for process, so being adjustment dosage to the detection of its blood drug concentration, reduce adverse reaction Important references are of great significance in clinical application.Oxcarbazepine and its metabolite therapeutic agent detect common at present Method has: ultraviolet spectrophotometry, high performance liquid chromatography, Liquid Chromatography-Mass Spectrometry, surpasses and faces high performance thin layer chromatography Boundary's chromatograph-mass spectrometer coupling method etc..In numerous methods, liquid chromatography is measure Oxcarbazepine and its metabolite most quasi- True method.Previous methods are there are complex pretreatment, qualitative, quantitative is not accurate enough, at high cost, analysis time is long or to experiment people The problems such as member's technical requirements are high.
Summary of the invention
An object of the present invention is in view of the deficiencies of the prior art, to provide a kind of based on multidimensional on-line solid phase extraction liquid phase Oxcarbazepine and its metabolite Therapeutic Drug Monitoring kit in the blood of chromatographic technique exploitation, it is difficult to understand in blood to meet The needs of oxcarbazepine and its metabolite Therapeutic Drug Monitoring.
It is a further object of the present invention to provide utilize kit monitoring Oxcarbazepine and its metabolite blood Chinese medicine The method of object concentration.
The present invention is that technical solution used by solving its technical problem is:
Oxcarbazepine and its metabolite Therapeutic Drug Monitoring kit in a kind of blood, it is characterised in that: the reagent Box includes calibration object reagent, quality-control product reagent, treatment fluid, extract liquor, cleaning solution, eluent.
Further, the calibration object reagent is containing Oxcarbazepine and its metabolite freeze-dried powder, stabilizer and plastotype agent Animal blood serum, the concentration range of the Oxcarbazepine and its metabolite freeze-dried powder in animal blood serum be 1.5~55mg/L, The concentration of the stabilizer is 10~30g/L, and the concentration of the plastotype agent is 10~30g/L;
Further, the quality-control product reagent is containing Oxcarbazepine and its metabolite freeze-dried powder, stabilizer and plastotype agent Animal blood serum, the concentration range of the Oxcarbazepine and its metabolite freeze-dried powder in animal blood serum be 1.5~55mg/L, The concentration of the stabilizer is 10~30g/L, and the concentration of the plastotype agent is 10~30g/L;
Preferably, the concentration of the stabilizer is 15~25g/L, and the concentration of the plastotype agent is 15~25g/L;
Further, the sample treatment solution is one or more of acetate buffer solution, acetonitrile and methanol Mixture aqueous solution, the content of ammonium acetate is 0.1 ‰~0.3 ‰ in the acetate buffer solution.The methanol contains Amount is 5%~15%, and the content of the acetonitrile is 5%~15%.
Further, the extract liquor includes extract liquor H1 and extract liquor H2;
Further, the extract liquor H1 is one or more of acetate buffer solution, acetonitrile and methanol The aqueous solution of mixture, the acetate buffer solution content are 0.1 ‰~0.3 ‰, the content of the methanol is 3%~ 10%, the content of the acetonitrile is 2%~8%.
Further, the extract liquor H2 is one or more of acetate buffer solution, acetonitrile and methanol The aqueous solution of mixture, the content of ammonium acetate is 0.05 ‰~0.15 ‰ in the acetate buffer solution.The methanol contains Amount is 30%~50%, and the content of the acetonitrile is 40%~70%.
Further, the cleaning solution is the aqueous solution of methanol or acetonitrile or two kinds of mixtures, the content of the methanol It is 0%~40%, the content of the isopropanol is 0%~20%, and the content of the acetonitrile is 0%~50%.
Further, the eluent includes eluent A, eluent B and eluent C;
Further, the eluent A is the mixed of one or more of acetate buffer solution, acetonitrile and methanol The aqueous solution of object is closed, the content of ammonium acetate is 0.05 ‰~0.15 ‰ in the acetate buffer solution, the content of the methanol It is 0%~15%, the content of the acetonitrile is 70%~90%;
Further, the mixing of one or more of the eluent B acetate buffer solution, acetonitrile and methanol The aqueous solution of object, the content of ammonium acetate is 0.1 ‰~0.3 ‰ in the acetate buffer solution, and the content of the methanol is 0% ~10%, the content of the acetonitrile is 5%~15%;The pH of the eluent B is 3~5;
Further, the mixing of one or more of the eluent C acetate buffer solution, acetonitrile and methanol The aqueous solution of object, the content of ammonium acetate is 0.1 ‰~0.3 ‰ in the acetate buffer solution, and the content of the methanol is 0% ~10%, the content of the acetonitrile is 5%~15%;The pH of the eluent B is 6~8.
The acetate buffer solution includes the mixture of one or two of acetic acid, ammonium acetate, ammonium hydroxide or more.
Further, the stabilizer is bovine serum albumin(BSA) (BSA);The plastotype agent mannitol and sucrose are a kind of Or two kinds of mixture, the ratio of the mixture of the mannitol and sucrose is 1:2~5.
Further, the detection method of the kit includes the following steps: that blood sample takes supernatant after being centrifuged Sample introduction, compensation is combined before and after carrying out in-line purification, enrichment, desorption and column by on-line solid phase extraction column, then passes through Vavle switching side Target analytes in blood sample are sent into analytical column and are separated by formula, finally by UV detector or diode array The analysis detections such as detector or mass detector, are calculated using calibration curve method, and drug is dense in final acquisition blood sample Angle value.
Calculation formula is as follows: linear regression equation: y=ax+b, and wherein a is slope, and b is intercept, and y is actual measurement peak face Product, x are mark concentration, and sample results calculate: the Oxcarbazepine of sample and its metabolite peak area are substituted into standard curve side Journey calculates Oxcarbazepine and its Metabolites Concentration in sample;
Specific step is as follows:
(1) 1~4mL of sample to be tested is taken, 10min is centrifuged in the case where centrifugal speed is 3000~5000rpm, supernatant is taken to obtain Serum or blood plasma;
(2) above-mentioned serum or blood plasma are taken, 1.0ml is pipetted and is added in sample bottle, be put into autosampler sample introduction 100ul into Row liquid chromatogram quantitative detection;
Chromatographic condition: extraction column: SLCZ column (30 × 4.6mm, 10 μm of partial sizes);Analytical column: C18 column (250 × 4.6mm, 5 μ M partial size);Mobile phase: extract liquor H1, extract liquor H2, eluent A, eluent B and eluent C;Column temperature: 35 DEG C;Sample volume: 100 μL;Wavelength: 239nm.
(3) drug concentration in sample is calculated according to above-mentioned formula.
The present invention has the advantages that
1, using multidimensional on-line solid phase extraction liquid-phase chromatographic analysis technology to Oxcarbazepine in blood and its metabolite Drug concentration carries out accurate quantitative analysis detection, and testing result is Oxcarbazepine and its metabolite proto-drug concentration, and energy is more acurrate The relationship illustrated before drug concentration-effect treatment-adverse reaction three;
2, blood sample is reduced brought by pre-treatment merely through centrifugal treating using blood plasma or serum direct injected Error and personnel's operating error improve the accuracy, repeatability and the rate of recovery of quantitative result, greatly shorten detection time, make Detection process is easy quickly, and experimental cost reduces, and more conducively detects in clinical treatment to the drug concentration of patient's body.
3, kit provided by the invention is commented by the drug concentration of Oxcarbazepine and its metabolite in detection blood Estimate the clinical drug effect of Oxcarbazepine and its metabolite.I.e. the present invention also provides the kits in assessment anti-fungal infection medicine Application in object clinical efficacy.
Detailed description of the invention
Fig. 1 is Oxcarbazepine and its metabolite chromatogram in Quality Control sample in embodiment;
Fig. 2 is Oxcarbazepine representative standard curve figure in embodiment
Fig. 3 is Oxcarbazepine metabolite representative standard curve figure in embodiment;
Fig. 4 is Oxcarbazepine and its metabolite chromatogram in serum sample in embodiment.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below Diagram and specific embodiment are closed, the present invention is further explained.
One, the preparation of Oxcarbazepine and its metabolite Therapeutic Drug Monitoring kit:
Standard curve reagent: wherein Oxcarbazepine and its metabolite are with the animal blood containing 2% stabilizer and 2% moulding agent It is configured to a series of concentration, respectively 1.5mg/L, 3.0mg/L, 6.0mg/L, 14.0mg/L, 27.0mg/L, 55.0mg/L clearly, Every bottle of packing 1.0ml.The above component is lyophilized to be saved in measurement bottom of bottle.Quality-control product reagent: wherein Oxcarbazepine and its metabolism produce Object is configured to high, normal, basic three concentration with the animal blood serum containing 2% stabilizer and 2% moulding agent, respectively 5.0mg/L, 25.0mg/L, 45.0mg/L, every bottle of packing 1.0ml.The above component is lyophilized to be saved in measurement bottom of bottle.
Sample treatment solution: precision weighs 0.12g ammonium acetate, sets in 1000mL volumetric flask, adds distilled water 700ml to dissolve, adds Acetic acid adjusts pH value 5.0, then plus acetonitrile 100ml and methanol 100ml, then plus distilled water is diluted to scale to get dispensing, patch Label label, completes operation.
Extract liquor H1: precision weighs 0.12g ammonium acetate, sets in 1000mL volumetric flask, and distilled water 700ml is added to dissolve, then plus Acetonitrile 50mL, then plus distilled water is diluted to scale to get packing, labeling label completes operation.
Extract liquor H2: precision weighs 0.12g ammonium acetate, sets in 1000mL volumetric flask, and distilled water 100ml is added to dissolve, then plus Acetonitrile 800ml, then plus distilled water is diluted to scale to get packing, labeling label completes operation.
Cleaning solution: precision weighs methanol 200ml and acetonitrile 350ml, sets in 1000mL volumetric flask, and distilled water is added to be diluted to quarter Degree is to get packing, labeling label completes operation.
Eluent A: precision weighs 0.12g ammonium acetate, sets in 1000mL volumetric flask, adds distilled water 250ml to dissolve, then plus second Nitrile 700mL, then plus distilled water is diluted to scale to get packing, labeling label completes operation.
Eluent B: precision weighs 0.12g ammonium acetate, sets in 1000mL volumetric flask, adds distilled water 700ml to dissolve, adds acetic acid PH value is adjusted to 3.5, then plus acetonitrile 100ml, then plus distilled water is diluted to scale to get packing, labeling label completes behaviour Make.
Eluent C: precision weighs 0.12g ammonium acetate, sets in 1000mL volumetric flask, adds distilled water 700ml to dissolve, adds 10% Ammonium hydroxide adjusts pH value to 7.0, then plus acetonitrile 50ml, then plus distilled water is diluted to scale to get packing, labeling label is completed Operation.
Two, the detecting step using above-mentioned monitoring reagent box is as follows:
1, it is applicable in instrument
Fully automatic therapy drug test analysis system (SLC), high performance liquid chromatograph (HPLC), liquid chromatography-tandem matter Spectrometer (LC-MS/MS).
2, sample requirement
Venous whole sample is acquired, is placed in anticoagulant tube, 2~8 DEG C of refrigerators is placed in immediately and seals standby survey up for safekeeping.
3, the method for inspection
Sample pretreatment:
Sample treatment solution is taken, 0.5ml is quantitatively pipetted and is added in sample reagent bottle;Sample to be tested at least 4mL is taken, is being centrifuged Speed is to be centrifuged 10min under 4000rpm, pipettes supernatant 1.0ml and is added in sample bottle, and vortex mixes, and is put into autosampler Middle sample introduction, and carry out liquid chromatogram quantitative detection;
Chromatographic condition:
On-line extraction column: SLCZ column (30 × 4.6mm, 10 μm of partial sizes);
On-line analysis column: C18 column (250 × 4.6mm, 5 μm of partial sizes);
Mobile phase: extract liquor H1, extract liquor H2, eluent A, eluent B and eluent C;
Column temperature: 35 DEG C;Sample volume: 100 μ L;Wavelength: 239nm.
1 condition of gradient elution of table
Measuring method:
After taking calibration object, quality-control product, sample to be tested to carry out Sample pretreatment, 100 μ L of supernatant sample introduction is taken to carry out chromatography fixed Amount analysis, records chromatographic peak area.
Quality Control requirement:
Every 1 analysis 1 standard curve of this retinue of lot sample (6 each 1 of various concentration value calibration product samples) and 6 Quality Control samples This (each 2 of high, medium and low concentration).Quality-control product sample measures result error should be less than 10%, at most allow 1/3 quality-control product sample This result is more than above-mentioned limit, but there can be no in same concentration quality-control product sample.As quality-control product sample measures result is not inconsistent Above-mentioned requirements are closed, then the analysis batch sample tests cancel, and detect again.
4, result calculates
As shown in Figs 1-4,
Specification Curve of Increasing:
With the calibration object concentration (1.5,3.0,6.0,14.0,27.0,55.0mg/L) of 6 different mark concentration for abscissa (x), using the actual measurement peak area of 6 calibration object samples as ordinate (y), standard curve is drawn.
The fitting of calibration curve equation:
With the actual measurement peak area (y) of 6 calibration object samples to mark concentration (x) using weighting (1/x2) least square method into Row linear regression.Oxcarbazepine linear regression equation: Y=0.7761X-0.3353, wherein 0.7761 is slope ,- 0.3353 is intercept, and calculates related coefficient (r), and r should be not less than 0.9900.R is 0.9999;The fitting of Oxcarbazepine metabolite Equation of linear regression: Y=0.3699X+0.0420, wherein 0.3699 is slope, 0.0420 is intercept, and calculates related coefficient (r), r should be not less than 0.9900.R is 0.9999.
The calculating of the rate of recovery:
The Oxcarbazepine of quality-control product sample measures and its metabolite peak area are substituted into above-mentioned standard curvilinear equation, calculated The Oxcarbazepine and its metabolite of quality-control product sample measure concentration.The calculation formula of the quality-control product sample rate of recovery are as follows: the rate of recovery (%)=measurement concentration/mark concentration × 100, the rate of recovery (%) should be in 100 ± 15% ranges.The Oxcarbazepine rate of recovery: 92.7%;The Oxcarbazepine metabolite rate of recovery: 95.3%.Sample results calculate:
The Oxcarbazepine of sample and its metabolite peak area are substituted into calibration curve equation, calculate the Oxcarbazepine of sample And its metabolite drug concentration.Oxcarbazepine is calculated and its metabolite drug concentration is 2.94ug/mL; 3.51ug/mL。
It summarizes, under the process conditions, the calibration curve coefficient correlation and quality-control product of Oxcarbazepine and its metabolite are returned Yield meets regulation, it is ensured that the accuracy of this method institute sample result.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent defines.

Claims (10)

1. Oxcarbazepine monitor drug concentration kit in a kind of blood, it is characterised in that: the kit includes calibration object examination Agent, quality-control product reagent, treatment fluid, extract liquor, cleaning solution, eluent.
2. kit according to claim 1, it is characterised in that: the calibration object reagent is containing Oxcarbazepine and its metabolism The animal blood serum of product freeze-dried powder, stabilizer and plastotype agent, the Oxcarbazepine and its metabolite freeze-dried powder are in animal blood serum In concentration range be 1.5~55mg/L, concentration gradient be 1.5~55mg/L;The concentration of the stabilizer is 10~30g/L, The concentration of the plastotype agent is 10~30g/L;
The quality-control product reagent is the animal blood serum containing Oxcarbazepine and its metabolite freeze-dried powder, stabilizer and plastotype agent, institute Stating the concentration range of Oxcarbazepine and its metabolite freeze-dried powder in animal blood serum is 1.5~55mg/L, the stabilizer Concentration is 10~30g/L, and the concentration of the plastotype agent is 10~30g/L.
3. kit according to claim 1, it is characterised in that: the concentration of the stabilizer is 15~25g/L, the modeling The concentration of type agent is 15~25g/L.
4. kit according to claim 1, it is characterised in that: the sample treatment solution is acetate buffer solution, second The aqueous solution of the mixture of one or more of nitrile and methanol, the content of ammonium acetate is in the acetate buffer solution 0.1 ‰~0.3 ‰, the content of the methanol is 5%~15%, and the content of the acetonitrile is 5%~15%.
5. kit according to claim 1, it is characterised in that: the extract liquor includes extract liquor H1 and extract liquor H2;
The extract liquor H1 is the water-soluble of the mixture of one or more of acetate buffer solution, acetonitrile and methanol Liquid, the content of ammonium acetate is 0.1 ‰~0.3 ‰ in the acetate buffer solution, and the content of the methanol is 3%~10%, The content of the acetonitrile is 2%~8%.
The extract liquor H2 is the water-soluble of the mixture of one or more of acetate buffer solution, acetonitrile and methanol Liquid, the content of ammonium acetate is 0.05 ‰~0.15 ‰ in the acetate buffer solution, the content of the methanol is 30%~ 50%, the content of the acetonitrile is 40%~70%.
6. kit according to claim 1, it is characterised in that: the cleaning solution is methanol or acetonitrile or two kinds of mixing The aqueous solution of object.
7. kit according to claim 1, it is characterised in that: the eluent include eluent A, eluent B and Eluent C;
The eluent A is the aqueous solution of the mixture of one or more of acetate buffer solution, acetonitrile and methanol, The content of ammonium acetate is 0.05 ‰~0.15 ‰ in the acetate buffer solution, and the content of the methanol is 0%~15%, institute The content for stating acetonitrile is 70%~90%;
The aqueous solution of the mixture of one or more of the eluent B acetate buffer solution, acetonitrile and methanol, institute The content for stating ammonium acetate in acetate buffer solution is 0.1 ‰~0.3 ‰, and the content of the methanol is 0%~10%, the second The content of nitrile is 5%~15%;The pH of the eluent B is 3~5;
The aqueous solution of the mixture of one or more of the eluent C acetate buffer solution, acetonitrile and methanol, institute The content for stating ammonium acetate in acetate buffer solution is 0.1 ‰~0.3 ‰, and the content of the methanol is 0%~10%, the second The content of nitrile is 5%~15%;The pH of the eluent B is 6~8.
8. according to kit described in claim 4~7 any one, it is characterised in that: the acetate buffer solution includes vinegar The mixture of the one or two of acid, ammonium acetate, ammonium hydroxide or more.
9. kit according to claim 2 or 3, it is characterised in that: the stabilizer is bovine serum albumin(BSA) (BSA);The ratio of the mixture of the mixture of the plastotype agent mannitol and sucrose one or two, the mannitol and sucrose Example is 1:2~5.
10. a kind of detection method of kit described in claim 1, include the following steps: that blood sample takes after being centrifuged on Clear liquid sample introduction, compensation is combined before and after carrying out in-line purification, enrichment, desorption and column by on-line solid phase extraction column, then is cut by valve Changing mode will separate in target analytes feeding analytical column in blood sample, finally by UV detector or diode The analysis detections such as array detector or mass detector, are calculated using calibration curve method, final to obtain blood sample Chinese medicine Object concentration value;
Calculation formula is as follows: linear regression equation: y=ax+b, and wherein a is slope, and b is intercept, and y is actual measurement peak area, x To indicate concentration, sample results are calculated: the Oxcarbazepine of sample and its metabolite peak area are substituted into calibration curve equation, meter Calculate the Oxcarbazepine and its Metabolites Concentration in sample;
Specific step is as follows:
(1) 1~4mL of sample to be tested is taken, 10min is centrifuged in the case where centrifugal speed is 3000~5000rpm, supernatant is taken to obtain serum Or blood plasma;
(2) above-mentioned serum or blood plasma are taken, 1.0ml is pipetted and is added in sample bottle, sample introduction 100ul in autosampler is put into and carries out liquid The detection of phase chromatogram quantification;
(3) drug concentration in sample is calculated according to above-mentioned formula.
CN201910671617.9A 2019-07-24 2019-07-24 Oxcarbazepine monitor drug concentration kit and its detection method in a kind of blood Withdrawn CN110361485A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910671617.9A CN110361485A (en) 2019-07-24 2019-07-24 Oxcarbazepine monitor drug concentration kit and its detection method in a kind of blood

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910671617.9A CN110361485A (en) 2019-07-24 2019-07-24 Oxcarbazepine monitor drug concentration kit and its detection method in a kind of blood

Publications (1)

Publication Number Publication Date
CN110361485A true CN110361485A (en) 2019-10-22

Family

ID=68220937

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910671617.9A Withdrawn CN110361485A (en) 2019-07-24 2019-07-24 Oxcarbazepine monitor drug concentration kit and its detection method in a kind of blood

Country Status (1)

Country Link
CN (1) CN110361485A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110763800A (en) * 2019-11-12 2020-02-07 北京和合医学诊断技术股份有限公司 Method for detecting oxcarbazepine and 10, 11-dihydro-10-hydroxycarbazepine in blood
CN114671809A (en) * 2020-12-25 2022-06-28 苏州博源医疗科技有限公司 Oxcarbazepine derivative, immunogen, anti-oxcarbazepine specific antibody, preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110763800A (en) * 2019-11-12 2020-02-07 北京和合医学诊断技术股份有限公司 Method for detecting oxcarbazepine and 10, 11-dihydro-10-hydroxycarbazepine in blood
CN114671809A (en) * 2020-12-25 2022-06-28 苏州博源医疗科技有限公司 Oxcarbazepine derivative, immunogen, anti-oxcarbazepine specific antibody, preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN111175394B (en) Method for detecting plasma catecholamine and metabolite thereof by liquid chromatography-tandem mass spectrometry
Liu et al. Global characterization of neutral saccharides in crude and processed Radix Rehmanniae by hydrophilic interaction liquid chromatography tandem electrospray ionization time-of-flight mass spectrometry
Keevil Does the presence of 3-epi-25OHD3 affect the routine measurement of vitamin D using liquid chromatography tandem mass spectrometry?
Riggin et al. Liquid chromatographic method for monitoring therapeutic concentrations of L-dopa and dopamine in serum.
Alam et al. Measurement of homocysteine: a historical perspective
CN109030658B (en) Method for detecting fructo-oligosaccharide and raffinose in infant milk powder
CN102141552A (en) High-sensitivity whole blood tacrolimus quantitative assay kit and preparation method thereof
CN110361485A (en) Oxcarbazepine monitor drug concentration kit and its detection method in a kind of blood
Breaud et al. A rapid and reliable method for the quantitation of tricyclic antidepressants in serum using HPLC-MS/MS
CN109633181A (en) The detection kit of metanephrine and normetanephrine in a kind of blood plasma
CN106959345A (en) A kind of full Isotopic Internal Standard mass spectrum quantitative approach of neurotransmitter metabolite
DeFelice et al. Rapid LC-MS/MS quantification of cancer related acetylated polyamines in human biofluids
CN111458417B (en) Method and kit for combined detection of multiple antibiotics in sample to be detected
CN110361488A (en) Lamotrigine monitor drug concentration kit and its detection method in a kind of blood
CN110361482A (en) Linezolid monitor drug concentration kit and its detection method in a kind of blood
CN110361481A (en) Vancomycin monitor drug concentration kit and its detection method in a kind of blood
CN110361484A (en) Amiodarone monitor drug concentration kit and its detection method in a kind of blood
CN110045037A (en) A kind of kit and detection method detecting nilotinib drug concentration in dry blood cake
CN105891368A (en) Method for detecting acetyl choline content in peripheral blood mononuclear cells
CN110361489A (en) Amitriptyline monitor drug concentration kit and its detection method in a kind of blood
CN110361486A (en) Aripiprazole drug substance concentration monitor kit and its detection method in a kind of blood
CN113125600B (en) Method for simultaneously determining concentration of 3 vitamin B12 in serum
CN114264765B (en) Analytical method for determining related substances in glimepiride intermediate by utilizing HPLC
Nishida et al. Miniaturized sample preparation method for determination of amphetamines in urine
CN114397379A (en) Method for determining concentration of ornidazole in blood plasma by liquid chromatography-mass spectrometry

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20191022