CN117368385A - Content detection method of tadalafil tablets - Google Patents
Content detection method of tadalafil tablets Download PDFInfo
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- CN117368385A CN117368385A CN202311447112.7A CN202311447112A CN117368385A CN 117368385 A CN117368385 A CN 117368385A CN 202311447112 A CN202311447112 A CN 202311447112A CN 117368385 A CN117368385 A CN 117368385A
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- IEHKWSGCTWLXFU-IIBYNOLFSA-N tadalafil Chemical compound C1=C2OCOC2=CC([C@@H]2C3=C([C]4C=CC=CC4=N3)C[C@H]3N2C(=O)CN(C3=O)C)=C1 IEHKWSGCTWLXFU-IIBYNOLFSA-N 0.000 title claims abstract description 81
- 229960000835 tadalafil Drugs 0.000 title claims abstract description 81
- 238000001514 detection method Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 8
- 238000010829 isocratic elution Methods 0.000 claims abstract description 7
- 239000012445 acidic reagent Substances 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000000741 silica gel Substances 0.000 claims abstract description 5
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 5
- 239000000945 filler Substances 0.000 claims abstract description 3
- FPLYNRPOIZEADP-UHFFFAOYSA-N octylsilane Chemical group CCCCCCCC[SiH3] FPLYNRPOIZEADP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 53
- 239000002904 solvent Substances 0.000 claims description 45
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 42
- 239000013558 reference substance Substances 0.000 claims description 26
- 239000000523 sample Substances 0.000 claims description 20
- 239000012488 sample solution Substances 0.000 claims description 19
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical group OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 16
- 238000011208 chromatographic data Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010812 external standard method Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 239000012085 test solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZOOGRGPOEVQQDX-KHLHZJAASA-N cyclic guanosine monophosphate Chemical compound C([C@H]1O2)O[P@](O)(=O)O[C@@H]1[C@H](O)[C@H]2N1C(N=C(NC2=O)N)=C2N=C1 ZOOGRGPOEVQQDX-KHLHZJAASA-N 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000012088 reference solution Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- DYLIWHYUXAJDOJ-OWOJBTEDSA-N (e)-4-(6-aminopurin-9-yl)but-2-en-1-ol Chemical compound NC1=NC=NC2=C1N=CN2C\C=C\CO DYLIWHYUXAJDOJ-OWOJBTEDSA-N 0.000 description 1
- -1 1, 3-benzodioxol-5-yl Chemical group 0.000 description 1
- 101100296726 Caenorhabditis elegans pde-5 gene Proteins 0.000 description 1
- 101100189582 Dictyostelium discoideum pdeD gene Proteins 0.000 description 1
- 101150098694 PDE5A gene Proteins 0.000 description 1
- 102000011016 Type 5 Cyclic Nucleotide Phosphodiesterases Human genes 0.000 description 1
- 108010037581 Type 5 Cyclic Nucleotide Phosphodiesterases Proteins 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 102100029175 cGMP-specific 3',5'-cyclic phosphodiesterase Human genes 0.000 description 1
- 210000005226 corpus cavernosum Anatomy 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000013037 reversible inhibitor Substances 0.000 description 1
- 210000002460 smooth muscle Anatomy 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The application discloses a content detection method of tadalafil tablets, which adopts high performance liquid chromatography to detect the content of the tadalafil tablets and comprises the following chromatographic conditions: the octyl silane bonded silica gel is used as a filler, and a mobile phase is composed of water, an acid reagent and an organic solvent and is subjected to isocratic elution; the method is used for solving the technical problems that in the content detection process of tadalafil tablets in the prior art, the content and impurity isomers are difficult to distinguish, the detection difficulty is increased, the detection result is inaccurate, the time consumption is long, the related detection content cannot be obtained, and the detection sensitivity is low.
Description
Technical Field
The application relates to the technical field of tadalafil tablet detection, in particular to a method for detecting the content of tadalafil tablets.
Background
Tadalafil tablet comprises Tadalafil as main ingredient, and has chemical name of (6R, 12 aR) -6- (1, 3-benzodioxol-5-yl) -2-methyl-2, 3,6,7, 12, 12 a-hexahydropyrazino [1 ', 2' -1,6] -pyrido [3,4-b ] indole-1, 4-dione, and molecular formula of C22H19N3O4, relative molecular weight of 389.41, and is selective reversible inhibitor of cyclic guanosine monophosphate (cGMP) specific phosphodiesterase 5 (PDE 5), and local stimulation causes local release of nitric oxide, PDE5 is inhibited by Tadalafil, so that cGMP level in corpora cavernosa is increased, smooth muscle is relaxed, blood flows into penile tissue, and erection is generated.
At present, in the detection method for the tadalafil tablet content in the prior art, the content and the impurity isomer are difficult to distinguish, the detection difficulty is increased, the detection result is inaccurate, the time consumption is long, the related detection content cannot be obtained, and the detection sensitivity is low.
Disclosure of Invention
The embodiment of the application provides a content detection method of tadalafil tablets, which is used for solving the technical problems that in the content detection process of tadalafil tablets in the prior art, the content and impurity isomers are difficult to distinguish, the detection difficulty is increased, the detection result is inaccurate, the time consumption is long, the related detection content cannot be obtained evidence, and the detection sensitivity is low.
In view of this, the present application provides a method for detecting the content of tadalafil tablets, which adopts high performance liquid chromatography to detect the content of tadalafil tablets, comprising the following chromatographic conditions: the octyl silane bonded silica gel is used as a filler, and the mobile phase is composed of water, an acid reagent and an organic solvent and is subjected to isocratic elution.
Optionally, the acid reagent is trifluoroacetic acid, and the organic solvent is acetonitrile.
Optionally, the detection wavelength is 284-286 nm.
Optionally, the flow rate of the high performance liquid chromatography is 1.4-1.6 ml/min.
Optionally, the column temperature of the high performance liquid chromatography is 38-42 ℃.
Optionally, the mobile phase includes a mobile phase a and a mobile phase B, the mobile phase a is a 0.1% trifluoroacetic acid aqueous solution, the mobile phase B is an acetonitrile solution, and the volume ratio of the mobile phase a to the mobile phase B is (60-50): (40-50).
Alternatively, the sample volume is 20. Mu.l.
Optionally, the octyl bonded silica gel column is a Venusil ASB TiC8 column or a ZORBAX SB-C8 column.
Optionally, the method comprises the following detection steps:
s1, detecting a blank solvent, namely a blank Bai Rongji chromatogram;
s2, detecting the reference substance solution to obtain a chromatogram of the reference substance solution;
s3, detecting the sample solution to obtain a chromatogram of the sample solution;
s4, calculating the peak area according to the chromatographic data of the reference substance solution chromatogram and the chromatographic data of the sample solution chromatogram by an external standard method, and further calculating the content of tadalafil tablets in the sample.
Optionally, preparation of a blank solvent is included: mixing water and acetonitrile according to the volume ratio of 1:1 to prepare a blank solvent;
preparing a reference substance solution: taking about 10mg of tadalafil reference substance, precisely weighing, placing into a 100ml measuring flask, adding a blank solvent, performing ultrasonic treatment to dissolve, cooling to room temperature, adding the blank solvent to dilute to a scale, and shaking uniformly;
preparation of test solution: taking 10 pieces of the product, precisely weighing, grinding, precisely weighing a proper amount of fine powder, placing into a 100ml measuring flask, adding a blank solvent, performing ultrasonic treatment to dissolve, cooling to room temperature, diluting to a scale with the blank solvent, shaking uniformly, filtering, and taking subsequent filtrate.
From the above technical solutions, the embodiments of the present application have the following advantages:
the method can accurately detect the content of the tadalafil tablets, has high sensitivity and good separation degree, calculates the peak area according to an external standard method by using chromatographic data of a reference substance solution chromatogram and a test substance solution chromatogram, and further calculates the content of the tadalafil tablets in the test substance.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed for describing the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a chromatogram of a test solution of the present invention;
FIG. 2 is a chromatogram of a control solution of the present invention;
FIG. 3 is a chromatogram of a blank solvent of the present invention;
FIG. 4 is a chromatogram of a blank co-liquid of the present invention;
FIG. 5 is a chromatogram of a mixed solution of the present invention
FIG. 6 is a chromatogram of a solution suitable for use in the system of the present invention.
Detailed Description
In order to make the present invention better understood by those skilled in the art, the following description will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention is described in further detail below with reference to the examples and figures 1 to 6:
a content detection method of tadalafil tablets adopts high performance liquid chromatography to detect the content of tadalafil tablets, comprising the following chromatographic conditions:
chromatographic column: a ZORBAX SB-C8 column or a Venusil ASB TiC8 column;
mobile phase: the volume ratio of the mobile phase A to the mobile phase B is (60-50): (40-50);
sample injection volume: 20 μl;
detection wavelength: 284-286 nm;
column temperature: 38-42 ℃;
flow rate: 1.4 to 1.6ml/min;
performing isocratic elution;
the preparation operation of the solution comprises the following steps:
preparation of blank solvent: mixing water and acetonitrile according to the volume ratio of 1:1 to prepare a blank solvent;
preparing a reference substance solution: taking about 10mg of tadalafil reference substance, precisely weighing, placing into a 100ml measuring flask, adding a blank solvent, performing ultrasonic treatment to dissolve, cooling to room temperature, adding the solvent to dilute to a scale, and shaking uniformly;
preparation of test solution: taking 10 pieces of the product, precisely weighing, grinding, precisely weighing a proper amount of fine powder (about equivalent to 10mg of tadalafil), placing into a 100ml measuring flask, adding a blank solvent, performing ultrasonic treatment to dissolve, cooling to room temperature, diluting to a scale with the blank solvent, shaking uniformly, filtering, and taking a subsequent filtrate.
The detection operation steps are as follows:
s1, detecting a blank solvent, namely a blank Bai Rongji chromatogram; the blank solvent is mainly acetonitrile water solution, and acetonitrile water solution is used as the blank solvent for detection, so that the interference of the acetonitrile water solution can be eliminated, and better chromatogram data can be obtained;
s2, detecting the reference substance solution to obtain a chromatogram of the reference substance solution; the tadalafil reference substance solution is used for detection, and the content of the detection substance can be clearly compared with a standard chromatogram used as a reference;
s3, detecting the sample solution to obtain a chromatogram of the sample solution; the substances to be detected in the sample and the content of the substances can be clearly detected and contrasted by eliminating the interference of the blank solvent and using the tadalafil reference substance solution as a reference standard chromatogram;
s4, calculating the peak area according to the chromatographic data of the reference substance solution chromatogram and the chromatographic data of the sample solution chromatogram by an external standard method, and further calculating the content of tadalafil tablets in the sample.
The content of tadalafil tablets in the sample is further calculated by calculating the peak area according to an external standard method through the chromatographic data of the control solution chromatogram and the sample solution chromatogram, so that the interference of other substances is avoided, the feeding amount of tadalafil can be accurately controlled in the tadalafil tablet production process, and the practical significance of the tadalafil tablet content measurement is realized.
Example 1
The specific test procedure of this example 1 is as follows:
1. chromatographic conditions: high performance liquid chromatograph, ultraviolet detector, chromatographic column: ZORBAX SB-C8, 4.6X105 mm,5 μm;
an aqueous solution of trifluoroacetic acid with the weight percentage of 0.1 percent is adopted as a mobile phase A; acetonitrile is adopted as a mobile phase B for isocratic elution, and the volume ratio of the mobile phase A to the mobile phase B is 55:45; flow rate: 1.5mL/min; detection wavelength: 285nm; column temperature: 40 ℃; sample injection volume: 20. Mu.L;
the preparation operation of the solution comprises the following steps:
preparation of blank solvent: mixing water and acetonitrile according to the volume ratio of 1:1 to prepare a blank solvent;
preparing a reference substance solution: taking about 10mg of tadalafil reference substance, precisely weighing, placing into a 100ml measuring flask, adding a blank solvent, performing ultrasonic treatment to dissolve, cooling to room temperature, adding the blank solvent to dilute to a scale, and shaking uniformly;
preparation of test solution: taking 10 pieces of the product, precisely weighing, grinding, precisely weighing a proper amount of fine powder (about equivalent to 10mg of tadalafil), placing into a 100ml measuring flask, adding a blank solvent, performing ultrasonic treatment to dissolve, cooling to room temperature, diluting to a scale with the blank solvent, shaking uniformly, filtering, and taking a subsequent filtrate.
The detection operation steps are as follows:
s1, detecting a blank solvent, namely a blank Bai Rongji chromatogram; the blank solvent is mainly acetonitrile water solution, and acetonitrile water solution is used as the blank solvent for detection, so that the interference of the acetonitrile water solution can be eliminated, and better chromatogram data can be obtained
S2, detecting the reference substance solution to obtain a chromatogram of the reference substance solution; the tadalafil reference substance solution is used for detection, and the content of the detection substance can be clearly compared with a standard chromatogram used as a reference;
s3, detecting the sample solution to obtain a chromatogram of the sample solution; the substances to be detected in the sample and the content of the substances can be clearly detected and contrasted by eliminating the interference of the blank solvent and using the tadalafil reference substance solution as a reference standard chromatogram;
s4, calculating the content of tadalafil tablets in the test sample according to the chromatographic data of the control solution chromatogram and the test sample solution chromatogram.
Detection result: referring to fig. 1 to 3, the obtained tadalafil has stable spectrum base line, symmetrical peak shape, good peak shape, high sensitivity and good separation degree, and the content of tadalafil tablets in a sample is further calculated according to the peak area by an external standard method through the chromatographic data of a control substance solution chromatogram and a sample solution chromatogram, so that the interference of other substances is avoided, the feeding amount of tadalafil can be accurately controlled in the production process of the tadalafil tablets, and the practical significance of the measurement of the tadalafil tablet content is realized.
Example 2
Method verification
(1) Specificity test and System applicability test
Acceptable standards: the blank solvent and blank auxiliary materials do not interfere with the measurement of the sample; under each breaking test condition, the main component peak and each degradation product can be well separated.
Solution preparation operation:
preparing a blank solvent from acetonitrile-water (1:1);
preparing a blank auxiliary material, placing a proper amount of the blank auxiliary material (equivalent to the amount of 2 tadalafil tablets) into a 100ml volumetric flask, ultrasonically dissolving and diluting to scale by using a blank solvent, shaking uniformly, filtering, and taking a continuous filtrate as a blank auxiliary material solution;
preparing a mixed solution of tadalafil 0.1mg/ml and impurities 1.5 ug/ml;
preparing a control solution by precisely taking 10mg of tadalafil control, placing the 10mg into a 100ml volumetric flask, and adding acetonitrile-water (1:1) blank solvent;
preparing a sample solution, namely precisely weighing a proper amount of fine powder (about equivalent to 10mg of tadalafil), placing the sample solution into a 100ml measuring flask, adding a blank solvent, ultrasonically dissolving, releasing to a scale, shaking uniformly, and filtering;
the system applicability solution was prepared to be 0.25mg/ml of tadalafil solution 50ml, 0.5ml of 5mol/l sodium hydroxide solution was added, and the mixture was allowed to stand for 30 minutes, followed by adjusting the pH to 7.0 with trifluoroacetic acid.
Detection operation:
according to the preparation method of the solution, on-machine test is carried out, and test results are recorded, wherein the specific test results are shown in table 1.
TABLE 1
The results show that:
as can be seen from table 1 and fig. 1 to 6, the blank solvent and the blank auxiliary material do not interfere with the measurement; the separation degree of the main peak and the adjacent impurity peak in the mixed solution is 3.07, which accords with the regulations; the retention time of the main peak of the sample solution is consistent with that of the main peak of the reference solution; in the system applicability solution, the separation degree of the trans isomer and the main peak is more than 3, and the tailing factor of the main peak is less than 1.5. The test result meets the requirements.
(2) Linearity test
Acceptable standards: the correlation coefficient (R) of the regression line must not be less than 0.998.
Detection operation:
taking a proper amount of tadalafil reference substance, precisely weighing, and adding solvent acetonitrile: dissolving with water (1:1) and diluting to obtain solution containing tadalafil 0.5mg per 1ml as mother liquor; the mother solution is precisely measured and diluted with solvent to prepare solutions containing 70 mug, 80 mug, 100 mug, 120 mug and 130 mug of tadalafil in each 1ml, and the solutions are uniformly shaken to be used as series standard solutions. According to chromatographic conditions, 20 μl of the sample is precisely measured, the sample is injected into a liquid chromatograph, a chromatogram is recorded, the concentration C (μg/ml) is taken as an abscissa, the peak area A is taken as an ordinate, linear regression is performed, a regression equation and a correlation coefficient are calculated, and the result is shown in Table 2.
TABLE 2
The results show that:
as is clear from Table 2, tadalafil has a good linear relationship in the range of 69.15ug/ml to 128.42ug/ml (70% -130%).
(3) Durability test
Acceptable standards: the relative standard deviation of the content data under each condition should be not more than 2%.
Detection operation:
taking a proper amount of tadalafil reference substance, precisely weighing, and adding solvent acetonitrile: dissolving with water (1:1) and diluting to obtain a solution containing tadalafil 0.1mg per 1ml as reference solution; weighing 10 pieces of the product, grinding into fine powder, precisely taking a proper amount of fine powder (equivalent to 10mg of tadalafil), placing into a 100ml volumetric flask, and adding solvent acetonitrile: proper amount of water (1:1) is dissolved by ultrasonic, and the subsequent filtrate is taken as a sample solution. The results of calculating the sample content according to the external standard method are shown in Table 3.
TABLE 3 Table 3
The results show that:
the test results show that the blank solvent does not interfere with the measurement by changing the wavelength (285+/-2 nm), the column temperature (40 ℃ +/-5 ℃), the flow rate (1.5+/-0.1 ml/min), the proportion of the mobile phase (+ -2) and the proportion of trifluoroacetic acid (+ -0.02%; the average content of tadalafil is 101.79%, the RSD is 0.97%, and the method has good durability.
Example 3
Example 3 corresponds to the specific detection procedure of example 1, except that the column of example 3 differs from the column of example 1.
Chromatographic column: venusil ASB TiC8, 4.6X105 mm,5 μm;
the remaining chromatographic conditions were identical to those of example 1.
The results show that: under the condition of the invention, the obtained tadalafil has stable spectrum base line, symmetrical peak shape and good peak shape, and the content of the tadalafil component in the sample to be tested is accurately measured, so that the content of the tadalafil in the tadalafil tablet is calculated, the interference of other substances is avoided, the feeding amount of the tadalafil can be accurately controlled in the tadalafil tablet production process, and the practical significance of the tadalafil tablet content measurement is realized.
Example 4
Chromatographic conditions:
high performance liquid chromatograph, ultraviolet detector, chromatographic column: ZORBAX SB-C8, 4.6X105 mm,5 μm;
an aqueous solution of trifluoroacetic acid with the weight percentage of 0.1 percent is adopted as a mobile phase A; acetonitrile is adopted as a mobile phase B for isocratic elution, and the volume ratio of the mobile phase A to the mobile phase B is 60:40; flow rate: 1.40mL/min; detection wavelength: 284nm; column temperature: 38 ℃; sample injection volume: 20. Mu.L;
the detection operation process comprises the following steps: same as in example 1
The results show that: under the condition of the invention, the obtained tadalafil has stable spectrum base line, symmetrical peak shape and good peak shape.
Example 5
Chromatographic conditions:
high performance liquid chromatograph, ultraviolet detector, chromatographic column: ZORBAX SB-C8, 4.6X105 mm,5 μm;
an aqueous solution of trifluoroacetic acid with the weight percentage of 0.1 percent is adopted as a mobile phase A; acetonitrile is adopted as a mobile phase B for isocratic elution, and the volume ratio of the mobile phase A to the mobile phase B is 50:50; flow rate: 1.60mL/min; detection wavelength: 286nm; column temperature: 42 ℃; sample injection volume: 20. Mu.L;
the detection operation process comprises the following steps: same as in example 1
The results show that: under the condition of the invention, the obtained tadalafil has stable spectrum base line, symmetrical peak shape and good peak shape.
The detection and display results of examples 3 to 5 show that the spectrum baseline of tadalafil obtained by detecting the tadalafil tablet content by the method is stable and symmetrical in peak shape, good in peak shape, high in sensitivity and good in separation degree, and the content of tadalafil tablets in a sample is further calculated according to the external standard method and calculated according to the peak area by using the chromatographic data of the reference solution chromatogram and the sample solution chromatogram, so that the interference of other substances is avoided, the feeding amount of tadalafil can be accurately controlled in the tadalafil tablet production process, and the practical significance of tadalafil tablet content measurement is realized.
The above embodiments are merely for illustrating the technical solution of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (10)
1. The method for detecting the content of the tadalafil tablet is characterized by adopting a high performance liquid chromatography to detect the content of the tadalafil tablet, and comprises the following chromatographic conditions: the octyl silane bonded silica gel is used as a filler, and the mobile phase is composed of water, an acid reagent and an organic solvent and is subjected to isocratic elution.
2. The method for detecting the content of tadalafil tablets according to claim 1, wherein the acid reagent is trifluoroacetic acid and the organic solvent is acetonitrile.
3. The method for detecting the content of tadalafil tablets according to claim 1, wherein the detection wavelength is 284-286 nm.
4. The method for detecting the content of tadalafil tablets according to claim 1, wherein the flow rate of the high performance liquid chromatography is 1.4-1.6 ml/min.
5. The method for detecting the content of tadalafil tablets according to claim 1, wherein the column temperature of the high performance liquid chromatography is 38-42 ℃.
6. The method for detecting the content of tadalafil tablets according to claim 1, wherein the mobile phase comprises a mobile phase a and a mobile phase B, wherein the mobile phase a is a 0.1% trifluoroacetic acid aqueous solution, the mobile phase B is an acetonitrile solution, and the volume ratio of the mobile phase a to the mobile phase B is (60-50): (40-50).
7. The method for detecting the content of tadalafil tablets according to claim 1, wherein the sample injection volume is 20 μl.
8. The method for detecting the content of tadalafil tablets according to claim 1, wherein the octyl-bonded silica gel column is a ZORBAX SB-C8 chromatographic column or a Venusil ASB TiC8 chromatographic column.
9. The method for detecting the content of tadalafil tablets according to claim 1, comprising the following detection steps:
s1, detecting a blank solvent, namely a blank Bai Rongji chromatogram;
s2, detecting the reference substance solution to obtain a chromatogram of the reference substance solution;
s3, detecting the sample solution to obtain a chromatogram of the sample solution;
s4, calculating the peak area according to the chromatographic data of the reference substance solution chromatogram and the chromatographic data of the sample solution chromatogram by an external standard method, and further calculating the content of tadalafil tablets in the sample.
10. The method for detecting the content of tadalafil tablets according to claim 9, comprising the steps of: mixing water and acetonitrile according to the volume ratio of 1:1 to prepare a blank solvent;
preparing a reference substance solution: taking about 10mg of tadalafil reference substance, precisely weighing, placing into a 100ml measuring flask, adding a blank solvent, performing ultrasonic treatment to dissolve, cooling to room temperature, adding the blank solvent to dilute to a scale, and shaking uniformly;
preparation of test solution: taking 10 pieces of the product, precisely weighing, grinding, precisely weighing a proper amount of fine powder, placing into a 100ml measuring flask, adding a blank solvent, performing ultrasonic treatment to dissolve, cooling to room temperature, diluting to a scale with the blank solvent, shaking uniformly, filtering, and taking subsequent filtrate.
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