CN107991420A - The liquid phase chromatography analytical method of carbamazepine content in a kind of detection blood - Google Patents
The liquid phase chromatography analytical method of carbamazepine content in a kind of detection blood Download PDFInfo
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- 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
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Abstract
The method of Karma western drug concentration is that standard solution is demarcated using liquid chromatography analysis equipment and UV detector in present invention detection blood,It is y=a*x+b that fitting, which obtains calibration curve equation,,Take blood sample to be measured,In the blood to be detected after treatment,Equally sample to be measured is detected using liquid chromatography analysis equipment and UV detector,Obtain blood y values to be measured,Blood y to be measured is substituted into calibration curve equation,Object relative concentration x in blood sample to be measured is obtained by calculation,Internal standard compound working solution concentration is known,Thus the Karma western drug concentration in blood to be detected is calculated in the sample,Internal standard method is combined by the present invention with high performance liquid chromatography,It is quantitative accurate,Quickly,High specificity,With higher separating degree and sensitivity,Reliable experimental data is provided for the therapeutic drug monitoring of clinically carbamazepine,The doctor that is more convenient for provides accurate carbamazepine dosage regimen for patient in time.
Description
Technical field
The present invention relates in the clinical therapeutic drug monitoring technical field of antipsychotics, more particularly to a kind of detection blood
The method of antiepileptic Carbamazepine.
Background technology
Carbamazepine (Carbamazepine, CBZ), molecular formula C15H12N2O, its chemical constitution are 5H- dibenzo [b, f]
Azatropylidene -5- formamides, concrete structure are as shown in Figure 1.CBZ is usually used in seizure resistant, be simple partial seizures especially
It is the choice drug of Complicated cases, it is also effective in cure to big breaking-out, limitation breaking-out and mixed type epilepsy.In addition, separately have
Clinical mental illness research points out that it can be used for treatment schizophrenia and bipolar disorder etc..The medicine effective concentration is 4-
12mg/L, has the characteristics that safe range is small, internal metabolism individual difference is big, toxicity is stronger, and its curative effect and adverse reaction with
Blood drug concentration is closely related, it is necessary to adjust dosage regimen according to blood concentration, therefore is necessary to carry out it clinical blood medicine
Concentration monitor.
At present, the common methods of Determination of Concentration of Carbamazepine measure have：Ultraviolet spectrophotometry, fluorescence polarization immunoassay,
High performance liquid chromatography, gas chromatography-mass spectrometry, Liquid Chromatography-Mass Spectrometry etc..In numerous methods, liquid phase
Chromatography is the prefered method of measure carbamazepine.Previous methods there are complex pretreatment, disturbing factor is more, analysis time is long,
The problem of sensitivity is not high, qualitative, quantitative is not accurate enough.
The content of the invention
For above-mentioned technical problem, it is an object of the present invention to provide a kind of side for detecting carbamazepine medicine concentration in blood
Method, this method is accurate, quick, high specificity, has higher separating degree.
The present invention uses following technical scheme：
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：It comprises the following steps：
(1) calibration of standard solution
First by the 10 μ L of standard working solution of at least three kinds various concentrations respectively with 10 μ L internal standards working solutions and by 1: 1 volume
The 80 μ L redissolution liquid of proportion methanol and water composition is mixed and made at least three kinds of standard solution, above-mentioned standard solution and is in rotating speed respectively
It is vortexed under 1200-2000rpm after mixing 30s-1min, it is molten to above-mentioned standard using liquid chromatography analysis equipment and UV detector
Liquid is detected, and Karma west and the internal standard chromatogram of above-mentioned at least three kinds standard solution is drawn, in above-mentioned Karma west and internal standard color
Standard target thing peak area and internal standard compound peak area are respectively obtained in spectrogram, with above-mentioned at least three standard targets thing peak area with
Ordinate y of the ratio of internal standard compound peak area as canonical plotting is dense with above-mentioned standard working solution concentration and internal standard working solution
Ratio, that is, relative concentration of degree is the abscissa x as canonical plotting, and gained at least three groups of data are detected by more than into line
Property return, to obtain calibration curve equation be y=a*x+b for fitting, and draws weight coefficient a and b；The standard working solution is card
The western solution of horse, the internal standard working solution are cyheptamide solution；
(a) preparation of standard working solution：
It is accurate to weigh the western standard items 15mg of Karma and be placed in 10ml volumetric flasks, with the methanol solution that water content is 0%-25% into
Row dissolving, and constant volume obtains standard reserving solution A in 10ml, standard reserving solution A is molten with the methanol that water content is 30%-60%
The dilution of liquid is diluted, and configures each standard work in the scope containing 5.00mg/L-400.0mg/L Karmas west respectively
Liquid, and preserved under the conditions of -80 DEG C；
(b) preparation of internal standard working solution：
Accurately weighing cyheptamide standard items 10mg is placed in 10mL volumetric flasks, is that 0%-25% methanol dissolves with water content,
And constant volume obtains standard reserving solution B, by the dilution of the standard reserving solution B methanol solutions for being 30%-60% with water content in 10mL
Liquid is diluted, and is obtained concentration and is the internal standard working solution of 300mg/L, and is preserved under the conditions of -20 DEG C；
(2) centrifugation of blood is detected
Blood to be detected at least 5ml is taken, 10min is centrifuged in the case where centrifugal speed is 3500rpm, takes supernatant to obtain serum or blood
Slurry, it is spare to before analyzing that above-mentioned serum or blood plasma are placed in the lower preservation of -20 DEG C of freezings；
(3) sample to be tested is handled
(c) pipette internal standard working solution described in 10 μ L steps (b) with liquid-transfering gun and in 1.5ml centrifuge tubes, then add 100
Serum or blood plasma described in μ L step (2), be vortexed concussion mixing 20s-1min under the rotating speed of 1200-2000rpm；
(d) ethyl acetate that 800uL is pipetted with liquid-transfering gun is added in the centrifuge tube of step (c), 1200-2000rpm's
Be vortexed concussion mixing 4-6min under rotating speed, then the high speed centrifugation 4-6min under the rotating speed of 10000-15000rpm, obtains supernatant；
(e) take step (d) supernatant 600uL to be put into another 1.5ml centrifuge tube, use N at normal temperatures2Slowly drying；
(f) being made of 1: 1 volume ratio methanol with water for 100 μ L is added into the centrifuge tube of the above-mentioned drying of step (e)
100 μ L redissolve liquid, then under 1200-2000rpm rotating speeds be vortexed mix 30s-1min, obtain sample to be tested；
(4) detection of sample to be tested
It is detected, is drawn using liquid chromatography analysis equipment and the UV detector sample to be measured to above-mentioned steps (f)
The Karma west of above-mentioned sample to be measured and internal standard chromatogram, object peak to be measured is obtained in above-mentioned Karma west and internal standard chromatogram
Area and internal standard compound peak area, above-mentioned steps (one) are substituted into by the ratio y of object peak area to be measured and internal standard compound peak area
In calibration curve equation, object relative concentration x in detected sample is obtained by calculation, internal standard compound working solution concentration is known
, the Karma western drug concentration in blood to be detected is thus calculated in the sample；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：The above-mentioned standard working solution is dense
Degree refers to the concentration in contained Karma west in standard working solution, and internal standard working solution concentration refers to contained cyheptamide in internal standard working solution
Concentration；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：Seven kinds are used in step (1)
The standard working solution of various concentrations；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：The mark of seven kinds of various concentrations
Quasi- working solution be respectively containing 5.00,10.00,20.00,40.00,80.00,160.00, the Karma west of 320.00mg/L concentration
Solution；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：In step (a) and (b), standard
Storing solution A and standard internal standard storing solution B is dissolved with methanol to be prepared, standard working solution and internal standard working solution using water content as
The dilution of 50% methanol solution is diluted；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：The UV detector is
VANQISH detectors, its Detection wavelength are 318nm, and pot strainer is 1290 Infinity inline of Agilent
filter；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：Stating high performance liquid chromatograph is made
Chromatographic column is the Extend-C18 of ZORBAX companies；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：The high performance liquid chromatograph is set
The column temperature put is 25 DEG C；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：The high performance liquid chromatograph institute
The use of mobile phase is methanol-water, the ratio of methanol and water is 45: 55, and the sample size of high performance liquid chromatograph is 10 μ L, uses ladder
Spend elution program, flow velocity 0.45ml/min, analysis time 5min；
The method of Karma western drug concentration in a kind of detection blood of the present invention, wherein：The water content is volume of aqueous
Amount.
Beneficial effect of the present invention：
The method of Carbamazepine in detection blood of the present invention, internal standard method is mutually tied with high performance liquid chromatography
Close, quantitative accurate, quick, high specificity, has higher separating degree and sensitivity, for the blood concentration of clinically carbamazepine
Monitoring provides reliable experimental data, and the doctor that is more convenient for provides accurate carbamazepine dosage regimen in time for patient.
Brief description of the drawings
Fig. 1 is carbamazepine chemical structural formula
Fig. 2 is carbamazepine and its internal standard chromatogram in embodiment Plays solution；Wherein, CBZ：Carbamazepine；CBZ-
IS：Cyheptamide；
Fig. 3 be embodiment in mark-on blood disappear or plasma sample in carbamazepine and its internal standard chromatogram；Wherein, CBZ：Karma
Xiping；CBZ-IS：Cyheptamide；
Below in conjunction with specific embodiments and the drawings, the invention will be further described.
Embodiment
A kind of method for detecting Karma western drug concentration in blood of the present invention comprises the following steps：
(1) calibration of standard solution
First by the 10 μ L of standard working solution of seven kinds of various concentrations respectively with 10 μ L internal standards working solutions and by 1: 1 volume ratio
80 μ L of methanol and water composition redissolve liquid and are mixed and made into seven kinds of standard solution, and above-mentioned standard solution is respectively 2000rpm in rotating speed
It is lower to be vortexed after mixing 30s, above-mentioned standard solution is detected using liquid chromatography analysis equipment and UV detector, is drawn
Karma west and the internal standard chromatogram of seven kinds of standard solution are stated, standard target is respectively obtained in above-mentioned Karma west and internal standard chromatogram
Thing peak area and internal standard compound peak area, standard is used as using the ratio of above-mentioned seven kinds of standard target thing peak areas and internal standard compound peak area
The ordinate y of curve map, is marked using ratio, that is, relative concentration of above-mentioned standard working solution concentration and internal standard working solution concentration to be used as
The abscissa x of directrix curve figure, seven groups of data of detection gained carry out linear regression by more than, and it is y that fitting, which obtains calibration curve equation,
=a*x+b, and draw weight coefficient a and b；The standard working solution is the western solution of Karma, and standard working solution concentration index is accurate
The concentration in contained Karma west in working solution；The internal standard working solution is cyheptamide solution, and internal standard working solution concentration refers to internal standard
The concentration of contained cyheptamide in working solution；
(a) preparation of standard working solution：
Accurately weighing the western standard items 15mg of Karma is placed in 10ml volumetric flasks, is dissolved with methanol, and constant volume is obtained in 10ml
To standard reserving solution A, standard reserving solution A is diluted with the dilution for the methanol solution that water content is 50%, is respectively configured
Go out the concentration containing Karma west for 5.00,10.00,20.00,40.00,80.00,160.00, the solution of 320.00mg/L, and
Preserved under the conditions of -80 DEG C；
(b) preparation of internal standard working solution：
It is accurate to weigh cyheptamide standard items 10mg and be placed in 10mL volumetric flasks, dissolved with methanol, and constant volume is in 10mL,
Standard reserving solution B is obtained, standard reserving solution B is diluted with the dilution for the methanol solution that water content is 50%, is obtained dense
The internal standard working solution for 300mg/L is spent, and is preserved under the conditions of -20 DEG C；
(2) centrifugation of blood is detected
Blood to be detected at least 5ml is taken, 10min is centrifuged in the case where centrifugal speed is 3500rpm, takes supernatant to obtain serum or blood
Slurry, it is spare to before analyzing that above-mentioned serum or blood plasma are placed in the lower preservation of -20 DEG C of freezings；
(3) sample to be tested is handled
(c) pipette internal standard working solution described in 10 μ L steps (b) with liquid-transfering gun and in 1.5ml centrifuge tubes, then add 100
Serum or blood plasma described in μ L step (2), be vortexed concussion mixing 30s under the rotating speed of 1500rpm；
(d) ethyl acetate that 800uL is pipetted with liquid-transfering gun is added in the centrifuge tube of step (c), under the rotating speed of 1500rpm
Be vortexed concussion mixing 5min, then the high speed centrifugation 5min under the rotating speed of 12000rpm, obtains supernatant；
(e) take step (d) supernatant 600uL to be put into another 1.5ml centrifuge tube, use N at normal temperatures2Slowly drying；
(f) being made of 1: 1 volume ratio methanol with water for 100 μ L is added into the centrifuge tube of the above-mentioned drying of step (e)
Redissolution liquid, then under 1500rpm rotating speeds be vortexed mix 30s, obtain sample to be tested；
(4) detection of sample to be tested
It is detected, is drawn using liquid chromatography analysis equipment and the UV detector sample to be measured to above-mentioned steps (f)
The Karma west of above-mentioned sample to be measured and internal standard chromatogram, object peak to be measured is obtained in above-mentioned Karma west and internal standard chromatogram
Area and internal standard compound peak area, above-mentioned steps (one) are substituted into by the ratio y of object peak area to be measured and internal standard compound peak area
In calibration curve equation, object relative concentration x in detected sample is obtained by calculation, internal standard compound working solution concentration is known
, the Karma western drug concentration in blood to be detected is thus calculated in the sample.
UV detector is VANQISH detectors, its Detection wavelength is 318nm, and pot strainer is Agilent 1290
Infinity inline filter.Chromatographic column used in high performance liquid chromatograph is the Extend-C18 of ZORBAX companies,
The column temperature that high performance liquid chromatograph is set is 25 DEG C；It is methanol-water that the high performance liquid chromatograph, which uses mobile phase, methanol with
The ratio of water is 45: 55, and the sample size of high performance liquid chromatograph is 10 μ L, uses gradient elution program, flow velocity 0.45ml/
Min, analysis time 5min.
If without specified otherwise, the water content is volumetric(al) moisture content in this application.
Technical method demonstration is as follows in the present embodiment：
First, the linear relationship and quantitative limit of this method
By the carbamazepine standard working solution of each concentration of 10 μ L of above-mentioned preparation, 10 μ L internal standard working solutions, whirlpool are added
Rotation mix, and add 80 μ L dilutions (methanol: water=1: 1), be vortexed mix after sample introduction, by the present embodiment determination condition concentration by
It is low to high to be measured, mapped with quantitative chromatographic peak area-concentration, obtain standard curve, the results showed that carbamazepine it is linear
Scope and quantitative limit are as follows：
(1) test limit (LOD)：0.07mg/L.
(2) quantitative limit (LOQ)：0.21mg/L.
(3) range of linearity：
Carbamazepine is linear good in the range of 0.5mg/L to 32.0mg/L, coefficient R2＞ 0.995.
2nd, the rate of recovery and precision of this method
Taking carbamazepine standard working solution to be configured to, high, medium and low 3 kinds of concentration carries out sample recovery rate experiment and precision is real
Test, be measured by the present embodiment method, replicate analysis measure 3 batches, its rate of recovery and precision are respectively such as table 1 below.Its
Average recovery rate in the range of 3 basic, normal, high pitch-based spheres is 93.36%~96.69%, and relative standard deviation is
0.46%~6.12%, it the results are shown in Table 1.
1 carbamazepine recovery of standard addition of table and precision
| Mark-on amount | 1.0mg/L | 4.0mg/L | 16.0mg/L |
| Average recovery rate | 93.94% | 96.69% | 93.36% |
| Precision RSD | 0.46% | 1.56% | 6.12% |
Summary checking test, the test limit of the present embodiment, all technical such as the rate of recovery and precision meet
It is required that carbamazepine medicine concentration in method detection blood, reappearance is good, and analysis time is short, and sample recovery rate is carried
Height, so as to improve the accuracy of testing result.
Carbamazepine and its interior target chromatogram are shown in Fig. 3 in serum or plasma sample, in standard solution carbamazepine and its
Interior target chromatogram is shown in Fig. 2, and the retention time of carbamazepine and cyheptamide is respectively 1.96min and 3.36min, by Fig. 2 and
Fig. 3 understands the present embodiment method using cyheptamide as internal standard so that the identification of target compound is more accurate, analysis time is short,
Disturb small, Internal standard curve method has high accuracy.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
The various modifications and improvement that case is made, should all fall into the protection domain that claims of the present invention determines.
Claims (10)
- A kind of 1. method for detecting Karma western drug concentration in blood, it is characterised in that：It comprises the following steps：(1) calibration of standard solutionFirst by the 10 μ L of standard working solution of at least three kinds various concentrations respectively with 10 μ L internal standards working solutions and by 1: 1 volume ratio The 80 μ L redissolution liquid of methanol and water composition is mixed and made at least three kinds of standard solution, above-mentioned standard solution and is in rotating speed respectively It is vortexed under 1200-2000rpm after mixing 30s-1min, it is molten to above-mentioned standard using liquid chromatography analysis equipment and UV detector Liquid is detected, and Karma west and the internal standard chromatogram of above-mentioned at least three kinds standard solution is drawn, in above-mentioned Karma west and internal standard color Standard target thing peak area and internal standard compound peak area are respectively obtained in spectrogram, with above-mentioned at least three standard targets thing peak area with Ordinate y of the ratio of internal standard compound peak area as canonical plotting is dense with above-mentioned standard working solution concentration and internal standard working solution Ratio, that is, relative concentration of degree is the abscissa x as canonical plotting, and gained at least three groups of data are detected by more than into line Property return, to obtain calibration curve equation be y=a*x+b for fitting, and draws weight coefficient a and b；The standard working solution is card The western solution of horse, the internal standard working solution are cyheptamide solution；(a) preparation of standard working solution：Accurately weighing the western standard items 15mg of Karma is placed in 10ml volumetric flasks, and the methanol solution for being 0%-25% with water content carries out molten Solution, and constant volume obtains standard reserving solution A, the methanol solution for being 30%-60% with water content by standard reserving solution A in 10ml Dilution is diluted, and configures each standard working solution in the scope containing 5.00mg/L-400.0mg/L Karmas west respectively, And preserved under the conditions of -80 DEG C；(b) preparation of internal standard working solution：Accurately weighing cyheptamide standard items 10mg is placed in 10mL volumetric flasks, is that 0%-25% methanol dissolves with water content, and fixed Be dissolved in 10mL, obtain standard reserving solution B, by the dilution of the standard reserving solution B methanol solutions for being 30%-60% with water content into Row dilution, obtains concentration and is the internal standard working solution of 300mg/L, and is preserved under the conditions of -20 DEG C；(2) centrifugation of blood is detectedBlood to be detected at least 5ml is taken, 10min is centrifuged in the case where centrifugal speed is 3500rpm, takes supernatant to obtain serum or blood plasma, It is spare to before analyzing that above-mentioned serum or blood plasma are placed in the lower preservation of -20 DEG C of freezings；(3) sample to be tested is handled(c) internal standard working solution described in 10 μ L steps (b) is pipetted in 1.5ml centrifuge tubes with liquid-transfering gun, then add 100 μ L steps Suddenly serum or blood plasma described in (two), be vortexed concussion mixing 20s-1min under the rotating speed of 1200-2000rpm；(d) ethyl acetate that 800uL is pipetted with liquid-transfering gun is added in the centrifuge tube of step (c), in the rotating speed of 1200-2000rpm The lower concussion mixing 4-6min that is vortexed, then the high speed centrifugation 4-6min under the rotating speed of 10000-15000rpm, obtain supernatant；(e) take step (d) supernatant 600uL to be put into another 1.5ml centrifuge tube, use N at normal temperatures2Slowly drying；(f) being answered by 1: 1 volume ratio methanol with what water formed for 100 μ L is added into the centrifuge tube of the above-mentioned drying of step (e) Solution, is then vortexed under 1200-2000rpm rotating speeds and mixes 30s-1min, obtain sample to be tested；(4) detection of sample to be testedIt is detected, is drawn above-mentioned using liquid chromatography analysis equipment and the UV detector sample to be measured to above-mentioned steps (f) The Karma west of sample to be measured and internal standard chromatogram, object peak area to be measured is obtained in above-mentioned Karma west and internal standard chromatogram With internal standard compound peak area, the ratio y of object peak area to be measured and internal standard compound peak area is substituted into the standards of above-mentioned steps (one) In curvilinear equation, be obtained by calculation object relative concentration x in detected sample, internal standard compound working solution concentration be it is known, Thus the Karma western drug concentration in blood to be detected is calculated in the sample.
- 2. the method for Karma western drug concentration in blood is detected as claimed in claim 1, it is characterised in that：The above-mentioned standard The concentration in contained Karma west in the quasi- working solution of working solution concentration index, internal standard working solution concentration refer to contained in internal standard working solution The concentration of cyheptamide.
- 3. the method for Karma western drug concentration in blood is detected as claimed in claim 2, it is characterised in that：In step (1) Use the standard working solution of seven kinds of various concentrations.
- 4. the method for Karma western drug concentration in blood is detected as claimed in claim 3, it is characterised in that：Seven kinds of differences The standard working solution of concentration be respectively containing 5.00,10.00,20.00,40.00,80.00,160.00,320.00mg/L concentration The western solution of Karma.
- 5. the method for Karma western drug concentration in blood is detected as claimed in claim 4, it is characterised in that：In step (a) and (b) in, standard reserving solution A and standard internal standard storing solution B are dissolved with methanol to be prepared, standard working solution and internal standard working solution with Water content is that the dilution of 50% methanol solution is diluted.
- 6. the method for Karma western drug concentration in blood is detected as claimed in claim 5, it is characterised in that：The ultraviolet detection Device is VANQISH detectors, its Detection wavelength is 318nm, and pot strainer is Agilent 1290Infinity inline filter。
- 7. the method for Karma western drug concentration in blood is detected as claimed in claim 5, it is characterised in that：The efficient liquid phase Chromatographic column used in chromatograph is the Extend-C18 of ZORBAX companies.
- 8. the method for Karma western drug concentration in blood is detected as claimed in claim 5, it is characterised in that：The efficient liquid phase The column temperature that chromatograph is set is 25 DEG C.
- 9. the method for Karma western drug concentration in blood is detected as claimed in claim 5, it is characterised in that：The efficient liquid phase It is methanol-water that chromatograph, which uses mobile phase, and the ratio of methanol and water is 45：55, the sample size of high performance liquid chromatograph is 10 μ L, uses gradient elution program, flow velocity 0.45ml/min, analysis time 5min.
- 10. the method for Karma western drug concentration in the detection blood as described in one of claim 5 to 9, it is characterised in that：It is described Water content is volumetric(al) moisture content.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109541107A (en) * | 2018-11-30 | 2019-03-29 | 徐州佳生医药科技有限公司 | A kind of method that LC-MS measures Carbamazepine in blood plasma |
| CN109884235A (en) * | 2019-02-28 | 2019-06-14 | 上海药明康德新药开发有限公司 | The efficient liquid phase detection method of carbamazepine |
| CN112034078A (en) * | 2020-09-21 | 2020-12-04 | 北京和合医学诊断技术股份有限公司 | Method for detecting carbamazepine |
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