CN111398475A - Method for analyzing composition of hydroxychloroquine sulfate preparation by using high performance liquid chromatography - Google Patents
Method for analyzing composition of hydroxychloroquine sulfate preparation by using high performance liquid chromatography Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 49
- ZAVJTSLIGAGALR-UHFFFAOYSA-N 2-(2,2,2-trifluoroacetyl)cyclooctan-1-one Chemical group FC(F)(F)C(=O)C1CCCCCCC1=O ZAVJTSLIGAGALR-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229960002927 hydroxychloroquine sulfate Drugs 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004128 high performance liquid chromatography Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 49
- 239000013558 reference substance Substances 0.000 claims abstract description 48
- 239000011259 mixed solution Substances 0.000 claims abstract description 32
- 238000007865 diluting Methods 0.000 claims abstract description 26
- 239000003085 diluting agent Substances 0.000 claims abstract description 14
- 239000012488 sample solution Substances 0.000 claims abstract description 14
- 238000005303 weighing Methods 0.000 claims abstract description 14
- 238000012360 testing method Methods 0.000 claims abstract description 12
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 230000035945 sensitivity Effects 0.000 claims abstract description 7
- 229960004171 hydroxychloroquine Drugs 0.000 claims abstract description 5
- XXSMGPRMXLTPCZ-UHFFFAOYSA-N hydroxychloroquine Chemical compound ClC1=CC=C2C(NC(C)CCCN(CCO)CC)=CC=NC2=C1 XXSMGPRMXLTPCZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 7
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 6
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 6
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims description 6
- 239000000523 sample Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 238000009472 formulation Methods 0.000 claims 2
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 6
- 229940079593 drug Drugs 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 210000002966 serum Anatomy 0.000 abstract description 2
- YWGMPTKTEYDHST-UHFFFAOYSA-M sodium;heptane-1-sulfonate;methanol Chemical compound [Na+].OC.CCCCCCCS([O-])(=O)=O YWGMPTKTEYDHST-UHFFFAOYSA-M 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- FQYRLEXKXQRZDH-UHFFFAOYSA-N 4-aminoquinoline Chemical compound C1=CC=C2C(N)=CC=NC2=C1 FQYRLEXKXQRZDH-UHFFFAOYSA-N 0.000 description 2
- 208000006926 Discoid Lupus Erythematosus Diseases 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 208000004921 cutaneous lupus erythematosus Diseases 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000036470 plasma concentration Effects 0.000 description 2
- 201000000596 systemic lupus erythematosus Diseases 0.000 description 2
- WHTVZRBIWZFKQO-AWEZNQCLSA-N (S)-chloroquine Chemical compound ClC1=CC=C2C(N[C@@H](C)CCCN(CC)CC)=CC=NC2=C1 WHTVZRBIWZFKQO-AWEZNQCLSA-N 0.000 description 1
- 208000003456 Juvenile Arthritis Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960003677 chloroquine Drugs 0.000 description 1
- WHTVZRBIWZFKQO-UHFFFAOYSA-N chloroquine Natural products ClC1=CC=C2C(NC(C)CCCN(CC)CC)=CC=NC2=C1 WHTVZRBIWZFKQO-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001647 drug administration Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 206010039073 rheumatoid arthritis Diseases 0.000 description 1
- 206010040882 skin lesion Diseases 0.000 description 1
- 231100000444 skin lesion Toxicity 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
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- 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
-
- 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
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- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/36—Control of physical parameters of the fluid carrier in high pressure liquid systems
-
- 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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a method for analyzing the composition of a hydroxychloroquine sulfate preparation by using a high performance liquid chromatography, which comprises the following steps: step a: selecting 50mg of hydroxychloroquine sulfate reference substance, and precisely weighing; step b: precisely measuring the mixed solution in the step a of 1.0ml,2.0ml,3.0ml,4.0ml,5.0ml,6.0ml and 7.0ml and placing the mixed solution in a 10ml volumetric flask for later use; step c: carrying out chromatographic analysis by using a chromatographic column to obtain a regression equation of the concentration C and the peak area A; step d: b, removing a proper amount of the mixture in the step a, precisely weighing, adding a diluent to dissolve the mixture, and quantitatively diluting the mixture to prepare a solution containing 0.5mg of the diluent in each 1ml of the mixture to obtain a sample solution; precisely measuring the sample solution, adding mobile phase, diluting to obtain solution containing 0.05g of control solution per 1ml, precisely measuring 0.2ml of control solution, injecting into liquid chromatograph, and adjusting instrument sensitivity for testing. The method for analyzing the composition of the hydroxychloroquine sulfate preparation by the high performance liquid chromatography is simple and convenient to operate, sensitive, high in accuracy, suitable for monitoring the serum drug concentration of the clinical hydroxychloroquine and high in specificity.
Description
Technical Field
The invention relates to a method for analyzing the composition of a hydroxychloroquine sulfate preparation by using a high performance liquid chromatography, belonging to the technical field of medicines.
Background
Hydroxychloroquine sulfate, which is clinically used for rheumatoid arthritis, juvenile chronic arthritis, discoid and systemic lupus erythematosus and skin lesions caused or aggravated by sunlight, has similar pharmacological action, pharmacokinetics and in vivo metabolic processes as chloroquine. After oral administration, hydroxychloroquine is rapidly and almost completely absorbed. In one study, the mean peak plasma concentration was in the range of 53-208ng/ml with a mean level of 105ng/ml following administration of a single dose of hydroxychloroquine of 400mg to healthy volunteers. The mean time to peak plasma concentration was 1.83 hours. The mean plasma elimination half-life varies according to time after administration as follows: the plasma peak concentrations were 5.9 hours, 26.1 hours and 299 hours respectively at-10 hours, 10-48 hours and 48-504 hours. The parent compounds and metabolites are widely distributed throughout the body and elimination occurs primarily through the urine. In one study, 3% of the administration dosage can be observed in 24 hours, the hydroxychloroquine sulfate tablet is a new 4 aminoquinoline medicament developed in recent years, and the main component is hydroxychloroquine sulfate which is used for treating discoid lupus erythematosus and systemic lupus erythematosus. The content determination method specified in the national drug administration drug Standard [330(289)99(1) is repeated extraction of chloroform, and after evaporation and concentration of an extracting solution, non-aqueous alkali amount method determination.
Disclosure of Invention
The invention aims to provide a method for analyzing the composition of a hydroxychloroquine sulfate preparation by using a high performance liquid chromatography, and aims to solve the problems that the existing content determination method proposed in the background art is repeated chloroform extraction, and the non-aqueous alkali content determination method is carried out after an extracting solution is evaporated and concentrated, and the method is complicated and time-consuming, has high solvent toxicity, and needs special attention to labor protection during operation.
In order to achieve the purpose, the invention provides the following technical scheme: a method for analyzing the composition of hydroxychloroquine sulfate preparation by high performance liquid chromatography comprises the following steps:
step a: selecting 50mg of hydroxychloroquine sulfate as a reference substance, precisely weighing, placing the reference substance in a volumetric flask with the volume of 50ml, dissolving the reference substance by using a mobile phase, diluting the reference substance to a scale, and fully shaking the reference substance for later use;
step b: precisely measuring the mixed solution in the step a of 1.0ml,2.0ml,3.0ml,4.0ml,5.0ml,6.0ml and 7.0ml, placing the mixed solution in a 10ml volumetric flask, dissolving the mixed solution by using the mobile phase and diluting the mixed solution to a scale, and then fully and uniformly shaking the mixed solution for later use;
step c: carrying out chromatographic analysis by using a chromatographic column to obtain a regression equation of the concentration C and the peak area A;
step d: b, removing a proper amount of the mixture in the step a, precisely weighing, adding a diluent to dissolve the mixture, and quantitatively diluting the mixture to prepare a solution containing 0.5mg of the diluent in each 1ml of the mixture to obtain a sample solution; precisely measuring the sample solution, adding mobile phase, diluting to obtain solution containing 0.05g of control solution per 1ml, precisely measuring 0.2ml of control solution, injecting into liquid chromatograph, and adjusting instrument sensitivity for testing.
Preferably, in the step a, the content of the hydroxychloroquine sulfate reference substance is 99.9%, and the reference substance is dried to constant weight under the condition of 105 ℃.
Preferably, the chromatographic column is a shim-packvp-ODS column, and the mobile phase is 0.05 mol. L-1Potassium dihydrogen phosphate and 0.05mol L-1Sodium heptanesulfonate methanol solution.
Preferably, the regression equation in the step C is that C is-9.30 × 10-3+2.6×10-8A, r is 0.9999, linear range 8 × 10-2-5.6×10-1mg·ml-1。
Preferably, the detection wavelength in step c is 245-350nm, and the flow rate is 2.0 ml/min.
Preferably, the mobile phase of the chromatographic column in the step c is acetonitrile 0.2 mol-L-1And potassium dihydrogen phosphate, the sample amount is 150-.
Preferably, the control solution and the test solution in step d are measured for 1, 2, 4, 8 and 16 hours respectively.
Compared with the prior art, the invention has the following beneficial effects: the method for analyzing the composition of the hydroxychloroquine sulfate preparation by the high performance liquid chromatography is simple and convenient to operate, sensitive, high in accuracy, suitable for monitoring the concentration of clinical hydroxychloroquine serum drugs, high in specificity, capable of being suitable for quality control of the drugs on a large scale, capable of fully separating impurities and free of influencing the accuracy of the detection method recorded in the application.
Detailed Description
In order to make the technical solutions of the present invention more clear and definite for those skilled in the art, the present invention is further described in detail with reference to the following examples, but the embodiments of the present invention are not limited thereto.
The method for analyzing the composition of the hydroxychloroquine sulfate preparation by using the high performance liquid chromatography provided by the embodiment comprises the following specific steps:
step a: selecting 50mg of hydroxychloroquine sulfate as a reference substance, precisely weighing, placing the reference substance in a volumetric flask with the volume of 50ml, dissolving the reference substance by using a mobile phase, diluting the reference substance to a scale, and fully shaking the reference substance for later use;
step b: precisely measuring the mixed solution in the step a of 1.0ml,2.0ml,3.0ml,4.0ml,5.0ml,6.0ml and 7.0ml, placing the mixed solution in a 10ml volumetric flask, dissolving the mixed solution by using the mobile phase and diluting the mixed solution to a scale, and then fully and uniformly shaking the mixed solution for later use;
step c: carrying out chromatographic analysis by using a chromatographic column to obtain a regression equation of the concentration C and the peak area A;
step d: b, removing a proper amount of the mixture in the step a, precisely weighing, adding a diluent to dissolve the mixture, and quantitatively diluting the mixture to prepare a solution containing 0.5mg of the diluent in each 1ml of the mixture to obtain a sample solution; precisely measuring the sample solution, adding mobile phase, diluting to obtain solution containing 0.05g of control solution per 1ml, precisely measuring 0.2ml of control solution, injecting into liquid chromatograph, and adjusting instrument sensitivity for testing.
And (b) in the step a, the content of the hydroxychloroquine sulfate reference substance is 99.9%, and the reference substance is dried to constant weight at 105 ℃.
The chromatographic column is a shim-packvp-ODS column, and the mobile phase is 0.05 mol. L-1Potassium dihydrogen phosphate and 0.05mol L-1Sodium heptanesulfonate methanol solution.
In the step C, the regression equation is that C is-9.30 × 10-3+2.6×10-8A, r is 0.9999, linear range 8 × 10-2-5.6×10-1mg·ml-1。
In step c, the detection wavelength is 245nm, and the flow rate is 2.0 ml/min.
Step (ii) ofThe mobile phase of the chromatographic column in the step c is acetonitrile 0.2 mol. L-1And potassium dihydrogen phosphate, in a sample amount of 150. mu. L.
In the step d, the reference substance solution and the test substance solution are respectively measured for 1, 2, 4, 8 and 16 hours.
In this example, a method for analyzing the composition of hydroxychloroquine sulfate preparation by high performance liquid chromatography is as follows:
step a: selecting 50mg of hydroxychloroquine sulfate as a reference substance, precisely weighing, placing the reference substance in a volumetric flask with the volume of 50ml, dissolving the reference substance by using a mobile phase, diluting the reference substance to a scale, and fully shaking the reference substance for later use;
step b: precisely measuring the mixed solution in the step a of 1.0ml,2.0ml,3.0ml,4.0ml,5.0ml,6.0ml and 7.0ml, placing the mixed solution in a 10ml volumetric flask, dissolving the mixed solution by using the mobile phase and diluting the mixed solution to a scale, and then fully and uniformly shaking the mixed solution for later use;
step c: carrying out chromatographic analysis by using a chromatographic column to obtain a regression equation of the concentration C and the peak area A;
step d: b, removing a proper amount of the mixture in the step a, precisely weighing, adding a diluent to dissolve the mixture, and quantitatively diluting the mixture to prepare a solution containing 0.5mg of the diluent in each 1ml of the mixture to obtain a sample solution; precisely measuring the sample solution, adding mobile phase, diluting to obtain solution containing 0.05g of control solution per 1ml, precisely measuring 0.2ml of control solution, injecting into liquid chromatograph, and adjusting instrument sensitivity for testing.
And (b) in the step a, the content of the hydroxychloroquine sulfate reference substance is 99.9%, and the reference substance is dried to constant weight at 105 ℃.
The chromatographic column is a shim-packvp-ODS column, and the mobile phase is 0.05 mol. L-1Potassium dihydrogen phosphate and 0.05mol L-1Sodium heptanesulfonate methanol solution.
In the step C, the regression equation is that C is-9.30 × 10-3+2.6×10-8A, r is 0.9999, linear range 8 × 10-2-5.6×10-1mg·ml-1。
In step c, the detection wavelength is 350nm, and the flow rate is 2.0 ml/min.
The mobile phase of the chromatographic column in the step c is acetonitrile 0.2 mol. L-1And potassium dihydrogen phosphate, in a sample amount of 200. mu. L.
In the step d, the reference substance solution and the test substance solution are respectively measured for 1, 2, 4, 8 and 16 hours.
In this example, a method for analyzing the composition of hydroxychloroquine sulfate preparation by high performance liquid chromatography is as follows:
step a: selecting 50mg of hydroxychloroquine sulfate as a reference substance, precisely weighing, placing the reference substance in a volumetric flask with the volume of 50ml, dissolving the reference substance by using a mobile phase, diluting the reference substance to a scale, and fully shaking the reference substance for later use;
step b: precisely measuring the mixed solution in the step a of 1.0ml,2.0ml,3.0ml,4.0ml,5.0ml,6.0ml and 7.0ml, placing the mixed solution in a 10ml volumetric flask, dissolving the mixed solution by using the mobile phase and diluting the mixed solution to a scale, and then fully and uniformly shaking the mixed solution for later use;
step c: carrying out chromatographic analysis by using a chromatographic column to obtain a regression equation of the concentration C and the peak area A;
step d: b, removing a proper amount of the mixture in the step a, precisely weighing, adding a diluent to dissolve the mixture, and quantitatively diluting the mixture to prepare a solution containing 0.5mg of the diluent in each 1ml of the mixture to obtain a sample solution; precisely measuring the sample solution, adding mobile phase, diluting to obtain solution containing 0.05g of control solution per 1ml, precisely measuring 0.2ml of control solution, injecting into liquid chromatograph, and adjusting instrument sensitivity for testing.
And (b) in the step a, the content of the hydroxychloroquine sulfate reference substance is 99.9%, and the reference substance is dried to constant weight at 105 ℃.
The chromatographic column is a shim-packvp-ODS column, and the mobile phase is 0.05 mol. L-1Potassium dihydrogen phosphate and 0.05mol L-1Sodium heptanesulfonate methanol solution.
In the step C, the regression equation is that C is-9.30 × 10-3+2.6×10-8A, r is 0.9999, linear range 8 × 10-2-5.6×10-1mg·ml-1。
In step c, the detection wavelength is 300nm, and the flow rate is 2.0 ml/min.
The mobile phase of the chromatographic column in the step c is acetonitrile 0.2 mol. L-1And potassium dihydrogen phosphate, in a sample amount of 180. mu. L.
In the step d, the reference substance solution and the test substance solution are respectively measured for 1, 2, 4, 8 and 16 hours.
In this example, a method for analyzing the composition of hydroxychloroquine sulfate preparation by high performance liquid chromatography is as follows:
step a: selecting 50mg of hydroxychloroquine sulfate as a reference substance, precisely weighing, placing the reference substance in a volumetric flask with the volume of 50ml, dissolving the reference substance by using a mobile phase, diluting the reference substance to a scale, and fully shaking the reference substance for later use;
step b: precisely measuring the mixed solution in the step a of 1.0ml,2.0ml,3.0ml,4.0ml,5.0ml,6.0ml and 7.0ml, placing the mixed solution in a 10ml volumetric flask, dissolving the mixed solution by using the mobile phase and diluting the mixed solution to a scale, and then fully and uniformly shaking the mixed solution for later use;
step c: carrying out chromatographic analysis by using a chromatographic column to obtain a regression equation of the concentration C and the peak area A;
step d: b, removing a proper amount of the mixture in the step a, precisely weighing, adding a diluent to dissolve the mixture, and quantitatively diluting the mixture to prepare a solution containing 0.5mg of the diluent in each 1ml of the mixture to obtain a sample solution; precisely measuring the sample solution, adding mobile phase, diluting to obtain solution containing 0.05g of control solution per 1ml, precisely measuring 0.2ml of control solution, injecting into liquid chromatograph, and adjusting instrument sensitivity for testing.
And (b) in the step a, the content of the hydroxychloroquine sulfate reference substance is 99.9%, and the reference substance is dried to constant weight at 105 ℃.
The chromatographic column is a shim-packvp-ODS column, and the mobile phase is 0.05 mol. L-1Potassium dihydrogen phosphate and 0.05mol L-1Sodium heptanesulfonate methanol solution.
In the step C, the regression equation is that C is-9.30 × 10-3+2.6×10-8A, r is 0.9999, linear range 8 × 10-2-5.6×10-1mg·ml-1。
In step c, the detection wavelength is 245-350nm, and the flow rate is 2.0 ml/min.
The mobile phase of the chromatographic column in the step c is acetonitrile 0.2 mol. L-1And potassium dihydrogen phosphate, the sample amount is 150-.
In the step d, the reference substance solution and the test substance solution are respectively measured for 1, 2, 4, 8 and 16 hours.
The above description is only for the purpose of illustrating the present invention and is not intended to limit the scope of the present invention, and any person skilled in the art can substitute or change the technical solution of the present invention and its conception within the scope of the present invention.
Claims (7)
1. A method for analyzing the composition of hydroxychloroquine sulfate preparation by high performance liquid chromatography is characterized by comprising the following steps:
step a: selecting 50mg of hydroxychloroquine sulfate as a reference substance, precisely weighing, placing the reference substance in a volumetric flask with the volume of 50ml, dissolving the reference substance by using a mobile phase, diluting the reference substance to a scale, and fully shaking the reference substance for later use;
step b: precisely measuring the mixed solution in the step a of 1.0ml,2.0ml,3.0ml,4.0ml,5.0ml,6.0ml and 7.0ml, placing the mixed solution in a 10ml volumetric flask, dissolving the mixed solution by using the mobile phase and diluting the mixed solution to a scale, and then fully and uniformly shaking the mixed solution for later use;
step c: carrying out chromatographic analysis by using a chromatographic column to obtain a regression equation of the concentration C and the peak area A;
step d: b, removing a proper amount of the mixture in the step a, precisely weighing, adding a diluent to dissolve the mixture, and quantitatively diluting the mixture to prepare a solution containing 0.5mg of the diluent in each 1ml of the mixture to obtain a sample solution; precisely measuring the sample solution, adding mobile phase, diluting to obtain solution containing 0.05g of control solution per 1ml, precisely measuring 0.2ml of control solution, injecting into liquid chromatograph, and adjusting instrument sensitivity for testing.
2. The method for analyzing the composition of hydroxychloroquine sulfate formulation by high performance liquid chromatography as claimed in claim 1, wherein said step of: and (b) in the step a, the content of the hydroxychloroquine sulfate reference substance is 99.9%, and the reference substance is dried to constant weight at 105 ℃.
3. The method for analyzing the composition of hydroxychloroquine sulfate as claimed in claim 1, wherein said chromatographic column is a shim-pack vp-ODS column, and the mobile phase is 0.05 mol-L-1Potassium dihydrogen phosphate and 0.05mol L-1Heptane sulfonic acid sodium saltMethanol solution.
4. The method for analyzing the composition of hydroxychloroquine sulfate by high performance liquid chromatography as claimed in claim 1, wherein said regression equation in step C is C-9.30 × 10-3+2.6×10-8A, r is 0.9999, linear range 8 × 10-2-5.6×10-1mg·ml-1。
5. The method for analyzing the composition of hydroxychloroquine sulfate formulation by high performance liquid chromatography as claimed in claim 1, wherein said step of: the detection wavelength in the step c is 245-350nm, and the flow rate is 2.0 ml/min.
6. The method for separating the composition of hydroxychloroquine preparation by high performance liquid chromatography as claimed in claim 1, wherein said mobile phase of said column in step c is acetonitrile 0.2 mol-L-1And potassium dihydrogen phosphate, the sample amount is 150-.
7. The method for analyzing the composition of hydroxychloroquine sulfate preparation by high performance liquid chromatography as claimed in claim 1, wherein: and d, respectively measuring the reference substance solution and the test substance solution in the step d for 1, 2, 4, 8 and 16 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112129874A (en) * | 2020-09-24 | 2020-12-25 | 江西国药有限责任公司 | Method for detecting content of hydroxychloroquine sulfate |
| CN114720574A (en) * | 2020-12-22 | 2022-07-08 | 远大医药（中国）有限公司 | Method for detecting content of hydroxychloroquine sulfate in hydroxychloroquine sulfate tablet |
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| CN114720574A (en) * | 2020-12-22 | 2022-07-08 | 远大医药（中国）有限公司 | Method for detecting content of hydroxychloroquine sulfate in hydroxychloroquine sulfate tablet |
| CN115629145A (en) * | 2022-12-07 | 2023-01-20 | 北京和合医学诊断技术股份有限公司 | Method for simultaneously detecting content of 7 anti-new coronavirus medicines |
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