CN109884235A - The efficient liquid phase detection method of carbamazepine - Google Patents
The efficient liquid phase detection method of carbamazepine Download PDFInfo
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Abstract
The present invention discloses a kind of efficient liquid phase detection method of carbamazepine, it uses reverse phase C18 chromatographic column, DAD detector, mobile phase A is the mixed solution of formic acid-ammonium acetate aqueous solution and acetonitrile, and Mobile phase B is the mixed solution of formic acid-ammonium acetate acetonitrile solution and water, using gradient elution.Using method 3~5ul of sample introduction of the invention, carbamazepine and its related substance can be effectively detected, and separating degree R can be steady up to 1.5 or more, HPLC spectrum baseline, does not drift about；This method detection time is short, only needs 3min that efficient liquid phase detection process can be completed, and this method substantially reduces sample consumption, improves detection efficiency, is suitble to high flux screening；Solvent can be saved, cost is reduced；Method of the invention is used for the assay of carbamazepine, has good linear relationship, reproducibility is high, meaningful in terms of bulk pharmaceutical chemicals, quality of the pharmaceutical preparations research and pharmacokinetics.
Description
Technical field
The present invention relates to Pharmaceutical Analysis technical fields, and in particular to a kind of efficient liquid phase detection method of carbamazepine.
Background technique
Carbamazepine (Carbamazepine) is a kind of anti-epileptic, class of setting the mind at rest drug, sends out big breaking-out, limitation
Make and mixed epilepsy is also effective in cure.It is mainly used for treating epilepsy, anxiety disorder and trigeminal neuralgia.Carbamazepine has very
More side effects, including: the allergic reaction of energy threat to life, it is toxic to trigeminal neuralgia, it may cause skin and internal organs
Grievous injury, therefore during treatment the blood substance level of patient is monitored extremely important.
Currently, there is the common method of toll bar Xiping blood concentration in detection blood plasma: ultraviolet spectrophotometry, fluorescence polarization are exempted from
Epidemic disease method, high performance liquid chromatography, gas chromatography-mass spectrometry, Liquid Chromatography-Mass Spectrometry, in these methods, liquid phase color
Spectrometry is the prefered method in toll bar Xiping.Previous detection method there are complex pretreatment, disturbing factor is more, analysis time is long, clever
The problem that sensitivity is not high, qualitative, quantitative is not accurate enough.
Chinese Pharmacopoeia version in 2015, describes the detection method of the related substance of carbamazepine, chromatographic condition are as follows: with color
Spectral condition and system suitability nitrile propyl silane bonded silica gel are filler, with methanol-tetrahydrofuran-water (120:30:
850) (0.02% formic acid is added for mobile phase；0.05% triethylamine), Detection wavelength 230nm, 20uL sample introduction.In addition, existing skill
Art has reported the content assaying method of carbamazepine, uses nitrile propyl silane bonded silica gel also as the chromatographic column of filler, flows
Dynamic phase A is 50mmol/L ammonium dihydrogen phosphate, and Mobile phase B uses acetonitrile, gradient elution time 65min, sample introduction 50uL,
215nm detection.Inventor is in this way measured carbamazepine content and its impurity, and discovery HPLC map elutes base line
There is drift, integral inaccuracy, the accuracy and accuracy being used for when quantitative analysis be not high, and detection needs 65min or more, consumes
Duration.
Summary of the invention
A kind of the technical problem to be solved by the invention is to provide detection times short, good separating effect, accuracy and accurate
Spend the efficient liquid phase detection method of higher carbamazepine.
In order to solve the above technical problems, the efficient liquid phase detection method of carbamazepine provided by the invention, wherein
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is that the mixing of formic acid-ammonium acetate aqueous solution and acetonitrile is molten
Liquid, formic acid volumetric concentration is 0.01~0.03% in aqueous solution, and acetic acid ammonium concentration is 0.5~1.5mM in aqueous solution, aqueous solution with
The volume ratio of acetonitrile is 100~95:0~5；Mobile phase B is the mixed solution of formic acid-ammonium acetate acetonitrile solution and water, acetonitrile
Formic acid volumetric concentration is 0.01~0.03% in solution, and acetic acid ammonium concentration is 0.5~1.5mM in acetonitrile solution, acetonitrile solution with
The volume ratio of water is 100~95:0~5；
Using gradient elution, gradient elution program is carried out by following procedure: 0~0.01min, Mobile phase B keep volume hundred
Divide than being 20%；0.01~2.10min, Mobile phase B percent by volume are incremented to 90% by 20%；2.10~2.11min, flowing
Phase B percentage by volume is decremented to 20% by 90%；2.11~3.00min, it is 20% that Mobile phase B, which keeps percentage by volume,.
In a preferred embodiment, mobile phase A is that the volume fraction of formic acid-ammonium acetate aqueous solution and acetonitrile is
The mixed solution of 95:5, Mobile phase B are that the volume fraction of formic acid-ammonium acetate acetonitrile solution and water is the mixed solution of 95:5.
In a preferred embodiment, in mobile phase A, formic acid volumetric concentration is 0.025% in aqueous solution；Mobile phase B
In, formic acid volumetric concentration is 0.025% in acetonitrile solution.
In a preferred embodiment, in mobile phase A, acetic acid ammonium concentration is 1mM in aqueous solution；In Mobile phase B, acetonitrile
Acetic acid ammonium concentration is 1mM in solution.
In a preferred embodiment, column's length 100mM.
In a preferred embodiment, flow velocity is 1.0~2.0ml/min, more preferably 1.4ml/min.
In a preferred embodiment, Detection wavelength is 280~285nm, more preferably 284nm.
In a preferred embodiment, column temperature control is at 35~40 DEG C, and more preferably 40 DEG C.
In a preferred embodiment, sample volume is 2~8 μ l, more preferably 3~5 μ l.
The present invention also provides a kind of efficient liquid phase methods for measuring carbamazepine content, comprising the following steps:
(1) preparation of reference substance solution and test solution: precision weighs appropriate carbamazepine reference substance, uses dimethylene
Sulfoxide dissolves and constant volume is at multiple reference substance solutions with a certain concentration gradient；Precision weighs appropriate carbamazepine test sample,
With the dissolution of dimethylene sulfoxide and constant volume obtains test solution；
(2) chromatographic condition:
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is the mixing of formic acid-ammonium acetate aqueous solution and acetonitrile
Solution, formic acid volumetric concentration is 0.025% in aqueous solution, and acetic acid ammonium concentration is 1mM, the volume of aqueous solution and acetonitrile in aqueous solution
Than for 95:5；Mobile phase B is the mixed solution of formic acid-ammonium acetate acetonitrile solution and water, formic acid volumetric concentration in acetonitrile solution
It is 0.025%, acetic acid ammonium concentration is 1mM in acetonitrile solution, and the volume ratio of acetonitrile solution and water is 95:5；
Using gradient elution, gradient elution program is carried out by following procedure: 0~0.01min, Mobile phase B keep volume hundred
Divide than being 20%；0.01~2.10min, Mobile phase B percent by volume are incremented to 90% by 20%；2.10~2.11min, flowing
Phase B percentage by volume is decremented to 20% by 90%；2.11~3.00min, it is 20% that Mobile phase B, which keeps percentage by volume,；
(3) measuring method:
The multiple reference substance solution and test solution are pressed into described (2) chromatographic condition successively sample introduction, record chromatography
Figure, prepares linear related work curve according to the spectrum data of multiple reference substance solutions and concentration data, substitutes into test sample
Spectrum data calculates and obtains test solution concentration, according to the title of obtained test solution concentration and carbamazepine test sample
Taken amount calculates carbamazepine content, completes the measurement of carbamazepine content.
In a preferred embodiment, the concentration of reference substance solution is followed successively by 6.25,12.5,25,50,100,200 μ g/
Ml, flow velocity 1.4ml/min.Detection wavelength is 284nm, and column temperature is 40 DEG C, and sample volume is 3~5 μ l.
The efficient liquid phase detection method of carbamazepine provided by the invention it is a technical advantage that:
1. method of the invention can effectively detect carbamazepine and its related substance, and separating degree R can up to 1.5 with
On.
2. method measurement HPLC spectrum baseline of the invention is steady, do not drift about.
3. method detection time of the invention is short, only need 3min that efficient liquid phase detection process can be completed, this method is significantly
Detection efficiency is improved, high flux screening is suitble to.
4. method of the invention can save solvent, cost is reduced, safe operation is simple, handles convenient and efficient.
5. method of the invention is used for the assay of carbamazepine, there is good linear relationship, reproducibility is high, in original
Expect that medicine, quality of the pharmaceutical preparations research and related pharmacokinetics quantitative study etc. have important research value.
Detailed description of the invention
Fig. 1 is the HPLC map using method measurement carbamazepine test sample of the invention.
Fig. 2 is the HPLC map one that the embodiment of the present invention 1 measures carbamazepine test sample.
Fig. 3 is the HPLC map two that the embodiment of the present invention 1 measures carbamazepine test sample.
Fig. 4 is the HPLC map three that the embodiment of the present invention 1 measures carbamazepine test sample.
Fig. 5 is the HPLC map four that the embodiment of the present invention 1 measures carbamazepine test sample.
Fig. 6 is the carbamazepine working curve drawn using method of the invention.
Specific embodiment
Present inventor gropes to have obtained a kind of the efficient of carbamazepine by extensive research and a large amount of experiment
Liquid phase detection method, this method provides can efficiently separate carbamazepine and its flow visualizing in relation to substance and gradient are washed
De- program, will can be difficult in the prior art the carbamazepine efficiently separated and its related substance realizes good separating effect,
Separating degree R is up to 1.5 or more.
The efficient liquid phase detection method for the carbamazepine that inventor uses is:
Chromatographic column uses reverse phase C18 chromatographic column, such as using octadecylsilane chemically bonded silica as the Waters of filler
XBridge chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A be formic acid-ammonium acetate aqueous solution/acetonitrile (100~
95/0~5；V/v mixed solution), formic acid volumetric concentration is 0.01~0.03% in aqueous solution, acetic acid ammonium concentration in aqueous solution
For 0.5~1.5mM；Mobile phase B is formic acid-ammonium acetate acetonitrile solution/water (100~95/0~5；V/v mixed solution),
Formic acid volumetric concentration is 0.01~0.03% in acetonitrile solution, and acetic acid ammonium concentration is 0.5~1.5mM in acetonitrile solution；
Using gradient elution, mobile phase A+Mobile phase B=100%, gradient elution program is carried out by following procedure: 0~
0.01min, it is 20% that Mobile phase B, which keeps percent by volume,；0.01~2.10min, Mobile phase B percent by volume are incremented by by 20%
To 90%；2.10~2.11min, Mobile phase B percentage by volume are decremented to 20% by 90%；2.11~3.00min, Mobile phase B
Keeping percentage by volume is 20%.
In a preferred embodiment of the invention, mobile phase A is the volume of formic acid-ammonium acetate aqueous solution and acetonitrile
Score is the mixed solution of 95:5, and Mobile phase B is volume fraction the mixing for 95:5 of formic acid-ammonium acetate acetonitrile solution and water
Close solution.
In a preferred embodiment of the invention, in mobile phase A, formic acid volumetric concentration is 0.025% in aqueous solution；Stream
In dynamic phase B, formic acid volumetric concentration is 0.025% in acetonitrile solution.
In a preferred embodiment of the invention, in mobile phase A, acetic acid ammonium concentration is 1mM in aqueous solution；Mobile phase B
In, acetic acid ammonium concentration is 1mM in acetonitrile solution.
In a preferred embodiment of the invention, column's length 100mM.
In a preferred embodiment of the invention, flow velocity is 1.0~2.0ml/min, more preferably 1.4ml/min.
In a preferred embodiment of the invention, Detection wavelength is 280~285nm, more preferably 284nm.
In a preferred embodiment of the invention, column temperature is controlled at 35~40 DEG C, and more preferably 40 DEG C.
In a preferred embodiment of the invention, sample volume is 2~8 μ l, more preferably 3~5 μ l.
Clear, complete description is carried out to technical solution of the present invention below in conjunction with specific embodiment, it is clear that described
Embodiment be a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without making creative work, belongs to guarantor of the present invention
The range of shield.
Experiment condition in the embodiment of the present invention is as follows:
Instrument: high performance liquid chromatograph (LC-20A)
Chromatographic column: Waters XBridge C18 chromatographic column, column length 100mm；
Test solution: precision weighs carbamazepine test sample 10mg, is placed in 10ml volumetric flask, uses dmso solution
And constant volume, obtain test solution；
Flow velocity: 1.4ml/min；
Detection wavelength: 284nm；
Column temperature: 40 DEG C；
Mobile phase: mobile phase A+Mobile phase B=100%；
Gradient elution: 0~0.01min, it is 20% that Mobile phase B, which keeps percent by volume,；0.01~2.10min, Mobile phase B
Percent by volume is incremented to 90% by 20%；2.10~2.11min, Mobile phase B percentage by volume are decremented to 20% by 90%；
2.11~3.00min, it is 20% that Mobile phase B, which keeps percentage by volume,；
Embodiment 1
Mobile phase A is formic acid-ammonium acetate aqueous solution/acetonitrile (95/5；V/v mixed solution), formic acid body in aqueous solution
Product concentration is 0.025%, and acetic acid ammonium concentration is 1mM in aqueous solution；Mobile phase B is formic acid-ammonium acetate acetonitrile solution/water
(95/5；V/v mixed solution), formic acid volumetric concentration is 0.025% in acetonitrile solution, and acetic acid ammonium concentration is in acetonitrile solution
1mM。
Pass through four sample introductions under the method, HPLC map is as shown in Figure 2-5, and baseline is steady, and reproducible, 3min can be complete
Portion's appearance, carbamazepine retention time are 2.043~2.045min, and process impurity retention time is 0.750~0.847, and point
1.5 are all larger than from degree, theoretical cam curve 21509.
Embodiment 2
Mobile phase A is formic acid-ammonium acetate aqueous solution/acetonitrile (95/5；V/v mixed solution), formic acid body in aqueous solution
Product concentration is 0.01%, and acetic acid ammonium concentration is 0.5mM in aqueous solution；Mobile phase B is formic acid-ammonium acetate acetonitrile solution/water
(95/5；V/v mixed solution), formic acid volumetric concentration is 0.01% in acetonitrile solution, and acetic acid ammonium concentration is in acetonitrile solution
0.5mM。
Baseline is steady under the method, and carbamazepine retention time is 2.045min or so, and separating degree is 13.505.
Embodiment 3
Mobile phase A is formic acid-ammonium acetate aqueous solution/acetonitrile (95/5；V/v mixed solution), formic acid body in aqueous solution
Product concentration is 0.03%, and acetic acid ammonium concentration is 1.5mM in aqueous solution；Mobile phase B is formic acid-ammonium acetate acetonitrile solution/water
(95/5；V/v mixed solution), formic acid volumetric concentration is 0.03% in acetonitrile solution, and acetic acid ammonium concentration is in acetonitrile solution
1.5mM。
Baseline is steady under the method, and carbamazepine retention time is 2.044min or so, and separating degree is 13.443.
Embodiment 4
Mobile phase A is formic acid-ammonium acetate aqueous solution/acetonitrile (95/5；V/v mixed solution), formic acid body in aqueous solution
Product concentration is 0.025%, and acetic acid ammonium concentration is 1mM in aqueous solution；Mobile phase B is formic acid-ammonium acetate acetonitrile solution, and acetonitrile is molten
Formic acid volumetric concentration is 0.025% in liquid, and acetic acid ammonium concentration is 1mM in acetonitrile solution.
Baseline is steady under the method, and carbamazepine retention time is 2.043min or so, and separating degree is 13.801.
Embodiment 5
Mobile phase A is formic acid-ammonium acetate aqueous solution, and formic acid volumetric concentration is 0.025% in aqueous solution, second in aqueous solution
Sour ammonium concentration is 1mM；Mobile phase B is formic acid-ammonium acetate acetonitrile solution, and formic acid volumetric concentration is 0.025% in acetonitrile solution,
Acetic acid ammonium concentration is 1mM in acetonitrile solution.
Baseline is steady under the method, and carbamazepine retention time is 2.043min or so, and separating degree is 13.892.
Embodiment 6
Mobile phase A is formic acid-ammonium acetate aqueous solution, and formic acid volumetric concentration is 0.025% in aqueous solution, second in aqueous solution
Sour ammonium concentration is 1mM；Mobile phase B is formic acid-ammonium acetate acetonitrile solution, and formic acid volumetric concentration is 0.025% in acetonitrile solution,
Acetic acid ammonium concentration is 1mM in acetonitrile solution.
Mobile phase: mobile phase A+Mobile phase B=100%；
The gradient elution of the present embodiment adjusts are as follows: 0~0.01min, it is 10% that Mobile phase B, which keeps percent by volume,；0.01
~2.10min, Mobile phase B percent by volume are incremented to 80% by 10%；2.10~2.11min, Mobile phase B percentage by volume by
80% is decremented to 10%；2.11~3.00min, it is 10% that Mobile phase B, which keeps percentage by volume,；
Occur that baseline is unstable, separating degree is too long less than 1, retention time under the method.
Based on above-mentioned detection method, inventor also provides a kind of efficient liquid phase method for measuring carbamazepine content, presses
Following steps carry out:
(1) preparation of reference substance solution and test solution: precision weighs carbamazepine reference substance, molten with dimethyl sulfoxide
It solves and constant volume obtains the stock solution of 1mg/ml, it is accurate to draw 50 μ l stock solutions, constant volume is successively diluted with dimethyl sulfoxide to be obtained
6.25, the reference substance solution of 12.5,25,50,100,200ug/ml；Precision weighs carbamazepine test sample, uses dimethyl sulfoxide
It dissolves and constant volume obtains test solution；
(2) chromatographic condition:
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is formic acid-ammonium acetate aqueous solution/acetonitrile (95/5；v/
V) mixed solution, formic acid volumetric concentration is 0.025% in aqueous solution, and acetic acid ammonium concentration is 1mM in aqueous solution；Mobile phase B is
Formic acid-ammonium acetate acetonitrile solution/water (95/5；V/v mixed solution), formic acid volumetric concentration is in acetonitrile solution
0.025%, acetic acid ammonium concentration is 1mM in acetonitrile solution；
Using gradient elution, gradient elution program is carried out by following procedure: 0~0.01min, Mobile phase B keep volume hundred
Divide than being 20%；0.01~2.10min, Mobile phase B percent by volume are incremented to 90% by 20%；2.10~2.11min, flowing
Phase B percentage by volume is decremented to 20% by 90%；2.11~3.00min, it is 20% that Mobile phase B, which keeps percentage by volume,；
(3) measuring method:
6 reference substance solutions and test solution are pressed into the chromatographic condition successively sample introduction, record chromatogram, according to
The carbamazepine peak area and concentration data of 6 reference substance solutions prepare linear related work curve (as shown in Figure 6), the work
Curve linear relationship is good, r >=0.9999；It substitutes into the carbamazepine calculated by peak area of test sample and show that test solution is dense
Extension rate when the test solution concentration and sample introduction of degree, the test solution concentration of comparative measurements and constant volume, calculates
The content of carbamazepine out.
The efficient liquid phase detection method of carbamazepine of the invention can effectively detect carbamazepine and its related substance,
And separating degree R can be up to 1.5 or more, and detection method in the prior art is difficult to realize having for carbamazepine and its related substance
Effect separation；The HPLC of detection method of the invention composes baseline stability, does not drift about；Method detection time of the invention is short, only
Need 3min that efficient liquid phase detection process can be completed, and detection method in the prior art then needs at least 65min or more ability
Detection is completed, this method substantially increases detection efficiency, is suitble to high flux screening；Method of the invention can be rapidly completed analysis and
Solvent is saved, cost is reduced, safe operation is simple, handles convenient and efficient；Method of the invention is for carbamazepine containing measurement
It is fixed, there is good linear relationship, r >=0.9999, reproducibility is high, in bulk pharmaceutical chemicals, quality of the pharmaceutical preparations research and related pharmacokinetics
Quantitative study etc. is worth with important research.
In conclusion the various embodiments described above are only presently preferred embodiments of the present invention, it is not of the invention to limit
Protection scope, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be all included in
In protection scope of the present invention.
Claims (12)
1. a kind of efficient liquid phase detection method of carbamazepine, which is characterized in that
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is the mixed solution of formic acid-ammonium acetate aqueous solution and acetonitrile,
Formic acid volumetric concentration is 0.01~0.03% in aqueous solution, and acetic acid ammonium concentration is 0.5~1.5mM, aqueous solution and second in aqueous solution
The volume ratio of nitrile is 100~95:0~5；Mobile phase B is the mixed solution of formic acid-ammonium acetate acetonitrile solution and water, and acetonitrile is molten
Formic acid volumetric concentration is 0.01~0.03% in liquid, and acetic acid ammonium concentration is 0.5~1.5mM, acetonitrile solution and water in acetonitrile solution
Volume ratio be (100~95): (0~5)；
Using gradient elution, gradient elution program is carried out by following procedure: 0~0.01min, Mobile phase B keep percent by volume
It is 20%；0.01~2.10min, Mobile phase B percent by volume are incremented to 90% by 20%；2.10~2.11min, Mobile phase B
Percentage by volume is decremented to 20% by 90%；2.11~3.00min, it is 20% that Mobile phase B, which keeps percentage by volume,.
2. the method as described in claim 1, which is characterized in that the mobile phase A is formic acid-ammonium acetate aqueous solution and second
The volume fraction of nitrile is the mixed solution of 95:5, and the Mobile phase B is the volume point of formic acid-ammonium acetate acetonitrile solution and water
Number is the mixed solution of 95:5.
3. method according to claim 2, which is characterized in that in the mobile phase A, formic acid volumetric concentration is in aqueous solution
0.025%；In the Mobile phase B, formic acid volumetric concentration is 0.025% in acetonitrile solution.
4. method as claimed in claim 3, which is characterized in that in the mobile phase A, acetic acid ammonium concentration is 1mM in aqueous solution；
In the Mobile phase B, acetic acid ammonium concentration is 1mM in acetonitrile solution.
5. the method as described in claim 1, which is characterized in that column's length 100mM.
6. the method as described in claim 1, which is characterized in that flow velocity is 1.0~2.0ml/min.
7. the method as described in claim 1, which is characterized in that Detection wavelength is 280~285nm.
8. the method as described in claim 1, which is characterized in that column temperature is controlled at 35~40 DEG C.
9. the method as described in claim 1, which is characterized in that sample volume is 2~8 μ L.
10. a kind of efficient liquid phase method for measuring carbamazepine content characterized by comprising
(1) preparation of reference substance solution and test solution: precision weighs appropriate carbamazepine reference substance, with dimethylene sulfoxide
It dissolves and constant volume is at multiple reference substance solutions with a certain concentration gradient；Precision weighs appropriate carbamazepine test sample, with two
Simultaneously constant volume obtains test solution for sulfoxide dissolution；
(2) chromatographic condition:
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is the mixed solution of formic acid-ammonium acetate aqueous solution and acetonitrile,
Formic acid volumetric concentration is 0.025% in aqueous solution, and acetic acid ammonium concentration is 1mM in aqueous solution, and the volume ratio of aqueous solution and acetonitrile is
95:5；Mobile phase B is the mixed solution of formic acid-ammonium acetate acetonitrile solution and water, and formic acid volumetric concentration is in acetonitrile solution
0.025%, acetic acid ammonium concentration is 1mM in acetonitrile solution, and the volume ratio of acetonitrile solution and water is 95:5；
Using gradient elution, gradient elution program is carried out by following procedure: 0~0.01min, Mobile phase B keep percent by volume
It is 20%；0.01~2.10min, Mobile phase B percent by volume are incremented to 90% by 20%；2.10~2.11min, Mobile phase B
Percentage by volume is decremented to 20% by 90%；2.11~3.00min, it is 20% that Mobile phase B, which keeps percentage by volume,；
(3) measuring method:
The multiple reference substance solution and test solution are pressed into described (2) chromatographic condition successively sample introduction, record chromatogram, root
Linear related work curve is prepared according to the spectrum data and concentration data of multiple reference substance solutions, substitutes into the map number of test sample
According to calculating and obtaining test solution concentration, carbamazepine content is calculated in conjunction with the meter that weighs of carbamazepine test sample.
11. method as claimed in claim 10, which is characterized in that the concentration of the reference substance solution is followed successively by 6.25,12.5,
25、50、100、200μg/ml。
12. method as claimed in claim 10, which is characterized in that flow velocity is 1.4ml/min in chromatographic condition, and Detection wavelength is
284nm, column temperature are 40 DEG C, and sample volume is 3~5 μ L.
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| CN115166095A (en) * | 2022-07-20 | 2022-10-11 | 江苏省食品药品监督检验研究院 | Method for detecting related substances of egg yolk lecithin |
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