CN113624702A - Dissolution curve determination method of rabeprazole sodium enteric-coated tablets - Google Patents
Dissolution curve determination method of rabeprazole sodium enteric-coated tablets Download PDFInfo
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- CN113624702A CN113624702A CN202110947922.3A CN202110947922A CN113624702A CN 113624702 A CN113624702 A CN 113624702A CN 202110947922 A CN202110947922 A CN 202110947922A CN 113624702 A CN113624702 A CN 113624702A
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- ZGDLVKWIZHHWIR-UHFFFAOYSA-N 4-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl]morpholine Chemical compound O1C(C)(C)C(C)(C)OB1C1=CC=C(N2CCOCC2)N=C1 ZGDLVKWIZHHWIR-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229960001778 rabeprazole sodium Drugs 0.000 title claims abstract description 85
- 238000004090 dissolution Methods 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 55
- 239000002662 enteric coated tablet Substances 0.000 title claims abstract description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 192
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 164
- 239000000243 solution Substances 0.000 claims abstract description 89
- 239000012738 dissolution medium Substances 0.000 claims abstract description 62
- 239000012085 test solution Substances 0.000 claims abstract description 38
- 239000013558 reference substance Substances 0.000 claims abstract description 32
- 239000008055 phosphate buffer solution Substances 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 22
- 239000012088 reference solution Substances 0.000 claims abstract description 16
- 239000012528 membrane Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000005259 measurement Methods 0.000 claims abstract description 12
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims abstract description 12
- 238000002835 absorbance Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 26
- 238000012360 testing method Methods 0.000 claims description 25
- 238000007865 diluting Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 239000012488 sample solution Substances 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 9
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 3
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 3
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 3
- 235000011009 potassium phosphates Nutrition 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 235000011008 sodium phosphates Nutrition 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 31
- 239000002253 acid Substances 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 6
- 230000002452 interceptive effect Effects 0.000 abstract description 4
- 239000002244 precipitate Substances 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 238000005374 membrane filtration Methods 0.000 abstract description 2
- 239000000825 pharmaceutical preparation Substances 0.000 abstract description 2
- 239000002609 medium Substances 0.000 description 15
- 238000011084 recovery Methods 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 12
- 239000003814 drug Substances 0.000 description 8
- 230000002378 acidificating effect Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000012216 screening Methods 0.000 description 7
- 239000002671 adjuvant Substances 0.000 description 6
- 238000002211 ultraviolet spectrum Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 229920003132 hydroxypropyl methylcellulose phthalate Polymers 0.000 description 4
- 229940031704 hydroxypropyl methylcellulose phthalate Drugs 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000002775 capsule Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 2
- 229930195725 Mannitol Natural products 0.000 description 2
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 description 2
- 239000007857 degradation product Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007922 dissolution test Methods 0.000 description 2
- 239000002552 dosage form Substances 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 210000001035 gastrointestinal tract Anatomy 0.000 description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 235000012245 magnesium oxide Nutrition 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000000594 mannitol Substances 0.000 description 2
- 235000010355 mannitol Nutrition 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000008363 phosphate buffer Substances 0.000 description 2
- 229960004157 rabeprazole Drugs 0.000 description 2
- YREYEVIYCVEVJK-UHFFFAOYSA-N rabeprazole Chemical compound COCCCOC1=CC=NC(CS(=O)C=2NC3=CC=CC=C3N=2)=C1C YREYEVIYCVEVJK-UHFFFAOYSA-N 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000001069 triethyl citrate Substances 0.000 description 2
- 235000013769 triethyl citrate Nutrition 0.000 description 2
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000009506 drug dissolution testing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012055 enteric layer Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- 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)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a dissolution curve determination method of rabeprazole sodium enteric-coated tablets, belonging to the technical field of analysis and detection of pharmaceutical preparations. The determination method of the invention takes phosphate buffer solution as dissolution medium, hydrochloric acid and methanol are added in the preparation of the test solution, the solutions are respectively taken at different time points, and the solution is filtered by a filter membrane to remove the interference of auxiliary materials and is taken as the test solution; dissolving rabeprazole sodium reference substance in methanol, and adding hydrochloric acid and phosphate buffer solution to constant volume to obtain reference substance solution; and (4) measuring absorbance by adopting an ultraviolet-visible spectrophotometry and calculating. According to the invention, the acid and the methanol are added into the test solution, and the precipitated precipitate is removed by using a filter membrane filtration mode, so that the interfering auxiliary materials in the rabeprazole sodium enteric-coated tablets can be effectively removed, and the solvent compositions of the test solution and the reference solution can be consistent, thereby ensuring the accuracy of the dissolution measurement result, being simple and rapid to operate, and being suitable for the dissolution curve measurement with large sample amount.
Description
Technical Field
The invention relates to the technical field of analysis and detection of pharmaceutical preparations, in particular to a method for determining a dissolution curve of rabeprazole sodium enteric-coated tablets.
Background
The raw material medicine of the rabeprazole sodium enteric-coated capsule is very easy to degrade in an acidic dissolution medium, degradation products are complex, effective detection is difficult by using an HPLC method, the raw material medicine and the degradation products thereof have ultraviolet absorption, and effective detection can be performed by adopting an ultraviolet-visible spectrophotometry. At present, the literature reports that the rabeprazole sodium enteric-coated preparation is directly dissolved in a dissolving medium with the pH value of 6.8 by using an ultraviolet-visible spectrophotometry, and the measuring wavelength is 282 nm. However, the method is only suitable for the condition that the auxiliary materials are not interfered, and if the auxiliary materials are interfered at the wavelength, the accuracy of the result cannot be guaranteed.
The rabeprazole sodium enteric-coated preparation is originally researched by the Japanese Weidai company, is rabeprazole sodium enteric-coated tablets, and has the dosage form of enteric-coated tablets, and according to the requirement of the imitation drugs, the difference of dissolution curves of a self-made preparation and a reference preparation needs to be compared in a plurality of dissolution media. The establishment of an accurate and reliable determination method of the dissolution curve in the acidic dissolution medium of the rabeprazole sodium enteric-coated tablets is a precondition for the comparative study of the dissolution curve. The auxiliary materials of the rabeprazole sodium enteric-coated tablet mainly comprise mannitol, magnesium oxide, ethyl cellulose, hydroxypropyl cellulose, triethyl citrate and hydroxypropyl methylcellulose phthalate, and are greatly different from rabeprazole sodium enteric-coated capsules. The hydroxypropyl methyl cellulose phthalate is a common enteric material in rabeprazole sodium enteric preparations, has strong ultraviolet absorption, and can seriously interfere with the determination result of an ultraviolet-visible spectrophotometry. The document Development and identification of dissolution testing in acidic media for rabeprazole and the Chinese patent CN105021559A all adopt the steps of adding acid to precipitate, centrifuging to remove hydroxypropyl methyl cellulose phthalate, taking the supernatant as a sample solution so as to eliminate the interference of enteric materials, and then adopting an ultraviolet-visible spectrophotometry to carry out measurement. The method can remove the interference of enteric materials, but can only be suitable for a specific prescription process and a specific dosage form, and cannot be directly applied to rabeprazole sodium enteric-coated tablets. And the solvent components of the test solution and the reference solution are different, so that the measurement result is inaccurate. On the other hand, the operation of removing the precipitate by centrifugation after adding acid to separate out the precipitate is inconvenient and low in efficiency: according to the general oral solid preparation dissolution curve determination and comparison guide principle issued by the national drug evaluation center, 12 tablets are determined in 1 batch of dissolution curves, if counted according to 6 time points, 72 test sample solutions need to be processed, and according to the centrifugation method in the patent, the centrifugation of 1 batch can be expected to be completed within 4 hours.
Therefore, it is necessary to develop an elution profile measuring method that can effectively remove the interfering excipients in rabeprazole sodium enteric-coated tablets, and can ensure the accuracy of elution measurement results by making the solvent compositions of the test solution and the reference solution consistent.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the method for measuring the dissolution curve of the rabeprazole sodium enteric-coated tablet, the method can effectively remove the interfering auxiliary materials in the enteric-coated tablet, and simultaneously, the solvent compositions of the test solution and the reference solution are consistent, so that the accuracy of the dissolution measurement result can be ensured, the operation is simple and convenient, and the detection efficiency is high.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a dissolution curve determination method of rabeprazole sodium enteric-coated tablets comprises the following steps:
s1, pretreatment of the test piece: taking 0.1mol/L hydrochloric acid solution as a dissolution medium, rotating at 50r/min, operating according to the method when the temperature of the dissolution medium reaches 37.0 +/-0.5 ℃, and taking out a test piece after 90-150 min;
s2, preparation of a test solution: taking a phosphate buffer solution with the pH of 6.0-6.8 as a dissolution medium, rotating at the speed of 50r/min, taking a pretreated test piece when the temperature of the dissolution medium reaches 37.0 +/-0.5 ℃, and continuing to operate according to the method; in a sampling tube, the ratio of hydrochloric acid: pre-adding 1mol/L hydrochloric acid solution and methanol according to the volume ratio of 1: 0.9-1, and respectively adding the hydrochloric acid solution: taking the dissolution liquid according to the volume ratio of 1: 8-8.1, placing the dissolution liquid in a sampling test tube, uniformly mixing, placing for 15-45 min, and filtering with a filter membrane to obtain a test solution;
s3, preparation of control solutions: precisely weighing a rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a measuring flask, dissolving and diluting the rabeprazole sodium reference substance by using methanol to scale, and shaking up; precisely measuring a proper amount of a placing bottle according to the mass ratio of methanol: 0.9-1% of hydrochloric acid: 1mol/L hydrochloric acid solution is added according to the volume ratio of 1, the mixture is diluted to scale by using a dissolution medium of phosphate buffer solution with the pH value of 6.0-6.8, the mixture is shaken up and stands for 0.5-1 h at room temperature to be used as a reference solution;
s4, measurement: and taking a proper amount of the reference substance solution and the test solution, respectively measuring the absorbance at the wavelength of 297-299 nm by an ultraviolet-visible spectrophotometry, and calculating.
In a preferred embodiment of the present invention, when the pH of the phosphate buffer solution as the dissolution medium in step S2 is 6.0, the volume ratio of hydrochloric acid to methanol in step S2 is 1:0.9, and after 20, 30, 40, 50, 60, 70, 80, and 90min, the following solutions are prepared: taking the dissolution liquid according to the volume ratio of 1:8.1, uniformly mixing the dissolution liquid with a pre-added 1mol/L hydrochloric acid solution and methanol, standing for 30min, and filtering by using a filter membrane to obtain a test solution.
Further, the volume ratio of methanol to hydrochloric acid in step S3 is 0.9: 1, diluting to scale with dissolution medium of phosphate buffer solution with pH of 6.0, shaking up, and standing at room temperature for 0.5 h.
Further, the detection wavelength of step S4 is 299 nm.
In a preferred embodiment of the present invention, when the pH of the phosphate buffer solution as the dissolution medium in step S2 is 6.8, the volume ratio of hydrochloric acid to methanol in step S2 is 1:1, and after 20, 25, 30, 35, 40, and 50min, the following solutions of hydrochloric acid are mixed: taking the dissolution liquid according to the volume ratio of 1:8, uniformly mixing the dissolution liquid with a pre-added 1mol/L hydrochloric acid solution and methanol, standing for 30min, and filtering by using a filter membrane to obtain a test solution.
Further, in step S3, the volume ratio of methanol to hydrochloric acid is 1:1, diluted to the scale with the dissolution medium of phosphate buffer solution with pH of 6.8, shaken well, and left to stand at room temperature for 1 h.
Further, the detection wavelength of step S4 is 297 nm.
As a preferred embodiment of the present invention, the phosphate of the phosphate buffer in steps S2 and S3 is selected from one of sodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, potassium phosphate, dipotassium hydrogen phosphate, and potassium dihydrogen phosphate; the pH regulator for regulating the pH value of the phosphate buffer solution is sodium hydroxide or potassium hydroxide.
Compared with the prior art, the invention has the beneficial effects that:
(1) the auxiliary materials of the rabeprazole sodium enteric-coated tablet mainly comprise mannitol, magnesium oxide, ethyl cellulose, hydroxypropyl cellulose, triethyl citrate and hydroxypropyl methylcellulose phthalate, and are greatly different from rabeprazole sodium enteric-coated capsules.
(2) The determination method provided by the invention is simple and rapid to operate, only needs less than 30min for one batch of samples, is suitable for determination of dissolution curves with large sample amount, and effectively solves the problems of complex operation and low efficiency in a centrifugal mode in the prior art.
(3) According to the invention, by optimizing the amount of acid and methanol and the ultraviolet measurement wavelength, the measurement method is not influenced by the release speed of the rabeprazole sodium enteric-coated tablet in an acidic medium and the degradation degree of the released raw material medicine, and has high accuracy, reliability and repeatability. Therefore, the method for determining the dissolution curve established by the invention can provide guidance for the research of the preparation prescription process required by the imitation drug declaration.
Drawings
FIG. 1 is a superimposed view of ultraviolet spectra of a test solution in a pH6.0 dissolution medium of example 1 at different times of 0-180 min;
FIG. 2 is a superimposed view of UV spectra of 0, 60 and 120min of a control solution in dissolution medium with pH6.0 of example 1;
FIG. 3 is a superimposed view of the ultraviolet spectra of the blank auxiliary material solution in the dissolution medium with pH6.0, the reference solution and the test solution at different times in example 1;
FIG. 4 is a superimposed view of ultraviolet spectra of the test solution in the dissolution medium with pH6.8 in example 2 at different times of 0-180 min;
FIG. 5 is a superimposed view of UV spectra of 0, 60 and 150min of a control solution in dissolution medium with pH6.8 in example 2;
FIG. 6 is a superimposed view of the ultraviolet spectra of the blank auxiliary material solution of the dissolution medium with pH of 6.8, the reference solution and the sample solution at different times in example 2.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
A dissolution curve determination method of rabeprazole sodium enteric-coated tablets comprises the following steps:
s1, pretreatment of the test piece: taking 0.1mol/L hydrochloric acid solution as a dissolution medium, rotating at 50r/min, operating according to the method when the temperature of the dissolution medium reaches 37.0 +/-0.5 ℃, and taking out a test piece after 90-150 min; the test pieces do not have the phenomena of color change, cracks or disintegration;
s2, preparation of a test solution: taking a phosphate buffer solution with the pH of 6.0-6.8 as a dissolution medium, rotating at the speed of 50r/min, taking a pretreated test piece when the temperature of the dissolution medium reaches 37.0 +/-0.5 ℃, and continuing to operate according to the method; in a sampling tube, the ratio of hydrochloric acid: pre-adding 1mol/L hydrochloric acid solution and methanol according to the volume ratio of 1: 0.9-1, and respectively adding the hydrochloric acid solution: taking the dissolution liquid according to the volume ratio of 1: 8-8.1, placing the dissolution liquid in a sampling test tube, uniformly mixing, standing for 0.5-1 h, and filtering with a filter membrane to obtain a test solution;
s3, preparation of control solutions: precisely weighing a rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a measuring flask, dissolving and diluting the rabeprazole sodium reference substance by using methanol to scale, and shaking up; precisely measuring a proper amount of the solution in a measuring flask, and measuring the mass ratio of the solution: 0.9-1% of hydrochloric acid: 1mol/L hydrochloric acid solution is added according to the volume ratio of 1, the mixture is diluted to scale by using a dissolution medium of phosphate buffer solution with the pH value of 6.0-6.8, the mixture is shaken up and stands for 0.5-1 h at room temperature to be used as a reference solution;
s4, measurement: and taking a proper amount of the reference substance solution and the test solution, respectively measuring the absorbance at the wavelength of 297-299 nm by an ultraviolet-visible spectrophotometry, and calculating.
When the pH of the phosphate buffer solution of the dissolution medium in step S2 is 6.0, the volume ratio of hydrochloric acid to methanol in step S2 is 1:0.9, and after 20, 30, 40, 50, 60, 70, 80, and 90min, the following solutions of hydrochloric acid are added: taking the dissolution liquid according to the volume ratio of 1:8.1, uniformly mixing the dissolution liquid with a pre-added 1mol/L hydrochloric acid solution and methanol, standing for 30min, and filtering by using a filter membrane to obtain a test solution. In step S3, the volume ratio of the dissolution liquid to the hydrochloric acid is 0.9: 1, diluting to scale with dissolution medium of phosphate buffer solution with pH of 6.0, shaking up, and standing at room temperature for 0.5 h. The detection wavelength of step S4 is 299 nm.
When the pH of the phosphate buffer solution of the dissolution medium in the step S2 is 6.8, the volume ratio of hydrochloric acid to methanol in the step S2 is 1:1, and after 20, 25, 30, 35, 40 and 50min, the following solutions of hydrochloric acid are added: taking the dissolution liquid according to the volume ratio of 1:8, uniformly mixing the dissolution liquid with a pre-added 1mol/L hydrochloric acid solution and methanol, standing for 30min, and filtering by using a filter membrane to obtain a test solution. And step S3, diluting the dissolution liquid and the hydrochloric acid at a volume ratio of 1:1 with a dissolution medium of a phosphate buffer solution with pH of 6.8 to scale, shaking up, and standing for 1h at room temperature. The detection wavelength of step S4 was 297 nm.
The phosphate of the phosphate buffer in the above steps S2 and S3 is selected from one of sodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, potassium phosphate, dipotassium hydrogen phosphate, and potassium dihydrogen phosphate; the pH regulator for regulating the pH value of the phosphate buffer solution is sodium hydroxide or potassium hydroxide.
The raw material medicine of the rabeprazole sodium enteric-coated tablet is easy to degrade in an acidic dissolution medium and complex to degrade, the acid and the methanol are added into the test solution, and the precipitated precipitate is removed by using a filter membrane filtration method, so that the auxiliary materials which interfere with the rabeprazole sodium enteric-coated tablet can be effectively removed, the solvent composition of the test solution and the reference solution can be consistent, and the accuracy of the dissolution determination result can be ensured.
Determination of methanol and hydrochloric acid adding amount and detection wavelength
To further determine the amounts of hydrochloric acid and methanol added and the wavelength of detection, the inventors conducted the following screening tests:
1. screening the test solution with pH6.0 medium for hydrochloric acid and methanol, and screening by measuring wavelength
Preparation of control solutions
Precisely weighing about 18mg of rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a 100ml measuring flask, dissolving and diluting the rabeprazole sodium reference substance to a scale mark by using methanol, and shaking up the solution. Precisely measure 4.5ml, put into a 50ml measuring flask, add 5ml of 1mol/L hydrochloric acid solution, dilute to the scale with pH6.0 medium, shake up, as a control solution.
Weighing 20mg of rabeprazole sodium and 145mg of blank auxiliary materials, placing the rabeprazole sodium and the blank auxiliary materials in a dissolution cup, adding 1000ml of dissolution medium with the pH value of 6.0 at 37 ℃, rapidly stirring for 1min to dissolve the rabeprazole sodium and the blank auxiliary materials, setting the rotation speed to be 50rpm, measuring the dissolution rate and the release rate according to the determination method, starting an experiment, precisely measuring 8.1ml of dissolution liquid in 0, 30, 60, 90, 120, 150 and 180min respectively, immediately mixing the dissolution liquid with the preset solutions, standing the mixture for 30min at room temperature, filtering the mixture by using a 0.45 mu m filter membrane, and taking the filtrate as a sample solution.
(1) Screening the amount of methanol: 1ml of hydrochloric acid and 0.8ml of methanol, 1ml of hydrochloric acid and 0.9ml of methanol, and 1ml of hydrochloric acid and 1ml of methanol;
(2) screening the amount of hydrochloric acid: 0.8ml of hydrochloric acid and 0.9ml of methanol, 1ml of hydrochloric acid and 0.9ml of methanol, and 1.2ml of hydrochloric acid and 0.9ml of methanol;
the solutions (1) and (2) were measured at 299nm, and the results are shown in Table 1 as "recovery rates of different methanol amounts" and "recovery rates of different hydrochloric acid amounts". The test solutions mixed with 1ml of hydrochloric acid and 0.9ml of methanol were measured at wavelengths of 297nm and 299nm, respectively, and the results are shown in "different-wavelength recovery" in Table 1.
TABLE 1 comparison of recovery (%) for different volumes of hydrochloric acid, methanol and different wavelengths
The results in Table 1 show that the recovery rate at different time points is closest to 100% and the accuracy is the best when 0.9ml of methanol, 1ml of hydrochloric acid and 299nm of detection wavelength are added.
2. Screening the test solution with pH6.8 medium for hydrochloric acid and methanol, and screening by measuring wavelength
Preparation of control solutions
Precisely weighing about 16mg of rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a 100ml measuring flask, dissolving and diluting the rabeprazole sodium reference substance to a scale mark by using methanol, and shaking up the solution. Precisely measure 5ml, place in a 50ml measuring flask, add 5ml of 1mol/L hydrochloric acid solution, dilute to the scale with pH6.8 medium, shake up, as a control solution.
Weighing 20mg of rabeprazole sodium and 145mg of blank auxiliary materials, placing the rabeprazole sodium and the blank auxiliary materials in a dissolution cup, adding 1000ml of dissolution medium with the pH value of 6.8 at 37 ℃, rapidly stirring for 1min to dissolve the rabeprazole sodium and the blank auxiliary materials, setting the rotation speed to be 50rpm, precisely measuring a proper amount of dissolution liquid in 0min, 30min, 60min, 90min, 120min and 180min respectively, immediately mixing the dissolution liquid with the preset solution, standing the solution at room temperature for 30min, filtering the solution by using a 0.45 mu m filter membrane, and taking the filtrate as a sample solution. The volume of the extract sampled and the amounts of hydrochloric acid and methanol were as follows:
(1) 7.9ml of eluent, 1.2ml of hydrochloric acid and 0.88ml of methanol;
(2) 9ml of eluent, 1.2ml of hydrochloric acid and 0ml of methanol;
(3) the eluate (8 ml), hydrochloric acid (1 ml) and methanol (1 ml).
The above solutions (1), (2) and (3) were measured at a wavelength of 297nm, and the results are shown in "sample solution + hydrochloric acid + methanol (ml)" in Table 2. The results of measurements of the solution (2) at wavelengths of 297nm, 298nm and 299nm are shown in "recovery (%) at different detection wavelengths" in Table 2.
TABLE 2 comparison of recovery (%) for different volumes of hydrochloric acid, methanol and different wavelengths
The results in Table 2 show that the recovery rate at each time point is closest to 100% in the mixed treatment of 8ml of the sample solution, 1ml of methanol and 1ml of hydrochloric acid. At the same time, at this ratio, the recovery rate at the wavelength of 297nm is closest to 100%, and the fluctuation range of the recovery rate at each time point is minimized, so that 297nm was selected as the detection wavelength of the sample solution in the medium at ph 6.8.
Therefore, the determination method is not influenced by the release speed of the rabeprazole sodium enteric-coated tablet in an acidic medium and the degradation degree of the released raw material medicine by optimizing the amount of the added acid and the added methanol and the ultraviolet determination wavelength, and has high accuracy, reliability and repeatability.
The enteric layer of the rabeprazole sodium enteric-coated tablet begins to dissolve at the pH value of more than 5.5, and is mainly released and absorbed in the intestinal tract with the pH value of 6.0 to 6.8 by combining the pH environment of the gastrointestinal tract of a human body, so that the dissolution curve of a dissolution medium with the pH value of 6.0 and 6.8 can be related to in vivo absorption. The invention will be further illustrated by the following example of a pH6.8 dissolution medium of pH 6.0.
Example 1
A method for determining the dissolution curve of rabeprazole sodium enteric-coated tablets in a dissolution medium with pH6.0 comprises the following steps:
s1 preparation of test solution
Weighing 20mg of rabeprazole sodium and 145mg of blank auxiliary materials, placing the rabeprazole sodium and the blank auxiliary materials in a dissolution cup, adding 1000ml of dissolution medium with the pH value of 6.0 at 37 ℃, rapidly stirring for 1min to dissolve the rabeprazole sodium, setting the rotation speed to be 50rpm, precisely measuring 8.1ml of dissolution liquid in 0, 30, 60, 90, 120, 150 and 180min respectively, immediately mixing the dissolution liquid with 1ml of preset 1mol/L hydrochloric acid solution and 0.9ml of methanol uniformly, standing for 30min at room temperature, filtering by using a 0.45 mu m filter membrane, and taking filtrate as a test solution.
S2 preparation of control solution
Precisely weighing about 18mg of rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a 100ml measuring flask, dissolving and diluting the rabeprazole sodium reference substance to a scale mark by using methanol, and shaking up the solution. Precisely measure 4.5ml, put into a 50ml measuring flask, add 5ml of 1mol/L hydrochloric acid solution, dilute to the scale with pH6.0 medium, shake up, as a control solution.
S3 preparation of blank auxiliary material solution
And dissolving 145mg of blank auxiliary material in 1000ml of pH6.0 dissolution medium to obtain blank auxiliary material solution.
S4, detection
Taking blank adjuvant solution, sample solution to be tested and reference solution sampled at different time, and scanning spectrum in 200-400 nm wavelength range by ultraviolet-visible spectrophotometry, wherein the spectrum superposition spectrum is shown in figure 1-figure 3.
The spectra in figures 1-3 show that the spectra of the reference solution and the test solution are substantially crossed at 299nm within 0-120 min and have relatively stable absorbance. Meanwhile, the blank adjuvant solution has no ultraviolet absorption at 299nm, which shows that the adjuvant interference is eliminated.
Example 2
A method for determining the dissolution curve of rabeprazole sodium enteric-coated tablets in a dissolution medium with pH6.8 comprises the following steps:
s1 preparation of test solution
Weighing 20mg of rabeprazole sodium and 145mg of blank auxiliary materials, placing the rabeprazole sodium and the blank auxiliary materials in a dissolution cup, adding 1000ml of dissolution medium with the pH value of 6.8 at 37 ℃, rapidly stirring for 1min to dissolve the rabeprazole sodium, setting the rotation speed to be 50rpm, starting an experiment according to a dissolution and release degree measurement method, precisely measuring 8ml of dissolution liquid in 0, 30, 60, 90, 120, 150 and 180min respectively, immediately and uniformly mixing the dissolution liquid with 1ml of a preset 1mol/L hydrochloric acid solution and 1ml of methanol, standing for 30min at room temperature, filtering by using a 0.45 mu m filter membrane, and taking filtrate as a test solution.
S2 preparation of control solution
Precisely weighing about 16mg of rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a 100ml measuring flask, dissolving and diluting the rabeprazole sodium reference substance to a scale mark by using methanol, and shaking up the solution. Precisely measure 5ml, place in a 50ml measuring flask, add 5ml of 1mol/L hydrochloric acid solution, dilute to the scale with pH6.8 medium, shake up, as a control solution.
S3 preparation of blank auxiliary material solution
And dissolving 145mg of blank auxiliary material in 1000ml of pH6.8 dissolution medium to obtain a blank auxiliary material solution.
S4, detection
Taking blank adjuvant solution, sample solution to be tested and reference solution sampled at different time, and scanning spectrum in 200-400 nm wavelength range by ultraviolet-visible spectrophotometry, wherein the spectrum superposition spectrum is shown in fig. 4-6.
The spectra in FIGS. 4-6 show that the spectra of the reference solution are substantially crossed at 297nm within 0-150 min and the spectra of the test solution within 0-180 min, and have relatively stable absorbance. Meanwhile, the blank adjuvant solution has no ultraviolet absorption at 297nm, which indicates that the interference of the adjuvant is eliminated.
From the results of examples 1 and 2, it is clear that, although there is degradation of rabeprazole sodium enteric-coated tablets in dissolution media at PH6.0 and PH6.8, detection using the wavelengths at which the spectra intersect according to the present invention is feasible regardless of the degradation ratio.
Example 3
A method for determining the dissolution curve of rabeprazole sodium enteric-coated tablets in a dissolution medium with pH6.0 comprises the following steps: taking 6 rabeprazole sodium enteric-coated tablets, carrying out dissolution test according to the following steps, and repeatedly measuring 3 times by the same method on different dates.
S1 pretreatment of test piece
Taking 700ml of 0.1mol/L hydrochloric acid solution as a dissolution medium, rotating at a speed of 50r/min, and taking out the test piece after 120min according to the method when the temperature of the obtained dissolution medium reaches 37.0 +/-0.5 ℃, wherein the test piece does not have the phenomena of color change, cracks or disintegration.
S2 preparation of test solution
1000ml of phosphate buffer solution with pH of 6.0 is used as a dissolution medium, the rotating speed is unchanged, and when the temperature of the dissolution medium reaches 37.0 +/-0.5 ℃, the pretreated test piece is taken out and the operation is continued according to the method. Adding 1ml of 1mol/L hydrochloric acid solution and 0.9ml of methanol in a sampling test tube in advance, taking 8.1ml of solution after 20, 30, 40, 50, 60, 70, 80 and 90 minutes, uniformly mixing with the 1mol/L hydrochloric acid solution and the methanol in advance, standing for 30 minutes, and filtering to obtain a sample solution.
S3 preparation of control solution
Precisely weighing about 18mg of rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a 100ml measuring flask, dissolving and diluting the rabeprazole sodium reference substance to a scale mark by using methanol, and shaking up the solution. Precisely measuring 4.5ml, placing in a 50ml measuring flask, adding 5ml of 1mol/L hydrochloric acid solution, diluting to scale with pH6.0 medium, shaking, and standing at room temperature for 30min to obtain control solution.
S4, detection
Taking appropriate amount of reference solution and sample solution, respectively measuring absorbance at 299nm wavelength by ultraviolet-visible spectrophotometry, and calculating. The results are shown in Table 3.
TABLE 3 comparison of the results of the determination of the dissolution curves of pH6.0 medium at different dates in example 3
The results in table 3 show that due to the prescription and the process characteristics of the rabeprazole sodium enteric-coated tablet, the RSD of the release rate result at each time point is larger, and the dissolution results at the final time points on different dates are basically consistent and close to 100%, which indicates that the determination result of the determination method of the invention is accurate and repeatable.
Example 4
A method for determining the dissolution curve of rabeprazole sodium enteric-coated tablets in a dissolution medium with pH6.8 comprises the following steps: taking 6 rabeprazole sodium enteric-coated tablets, carrying out dissolution test according to the following steps, and repeatedly measuring 3 times by the same method on different dates.
S1 pretreatment of test piece
Taking 700ml of 0.1mol/L hydrochloric acid solution as a dissolution medium, rotating at a speed of 50r/min, and taking out the test piece after 120min according to the method when the temperature of the obtained dissolution medium reaches 37.0 +/-0.5 ℃, wherein the test piece does not have the phenomena of color change, cracks or disintegration.
S2 preparation of test solution
1000ml of phosphate buffer solution with pH6.8 is used as a dissolution medium, the rotating speed is unchanged, and when the temperature of the dissolution medium reaches 37.0 +/-0.5 ℃, the pretreated test piece is taken out and the operation is continued according to the method. Adding 1ml of 1mol/L hydrochloric acid solution and 1ml of methanol in a sampling test tube in advance, taking 8ml of solution after 20, 25, 30, 35, 40 and 50min, uniformly mixing with the 1mol/L hydrochloric acid solution and the methanol in advance, standing for 30min, and filtering to obtain a sample solution.
S3 preparation of control solution
Precisely weighing about 16mg of rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a 100ml measuring flask, dissolving and diluting the rabeprazole sodium reference substance to a scale mark by using methanol, and shaking up the solution. Precisely measuring 5ml, placing into a 50ml measuring flask, adding 5ml of 1mol/L hydrochloric acid solution, diluting with pH6.8 medium to scale, shaking, and standing for 1 hr to obtain control solution.
S4, detection
Taking appropriate amount of control solution and sample solution, respectively measuring absorbance at 297nm wavelength by ultraviolet-visible spectrophotometry, and calculating to obtain the results shown in Table 4.
TABLE 4 comparison of the results of the determination of the dissolution curves of pH6.8 medium at different dates in example 4
The results in table 4 show that the release rate average values of the rabeprazole sodium enteric-coated tablets measured at pH6.8 on different dates are basically consistent, which indicates that the measurement result of the method of the invention is accurate and repeatable.
Second, effect comparison
The dissolution rate of rabeprazole sodium enteric-coated tablets is respectively measured by taking rabeprazole sodium and auxiliary materials in a prescription amount, taking a method disclosed by a document of Development and identification of dissolution in acidic media for rabeprazole and a Chinese patent CN105021559A as a comparative example 1 and a comparative example 2, taking the method disclosed by the invention as an experimental example 1, measuring 3 parts of each medium in parallel, sampling and measuring at 0min, 30min, 60min, 120min and 180min, taking the measured amount/added amount as a recovery rate, and comparing the accuracy of different methods, wherein the result is shown in a table 5.
TABLE 5 comparison of accuracy of comparative example 1, comparative example 2 and Experimental example 1
The results in Table 5 show that the accuracy recovery rate of the method of the invention is between 95% and 105%, and meets the detection requirement of the dissolution method, while the comparative example 1 and the comparative example 2 do not meet the specification.
In conclusion, the determination method provided by the invention can effectively remove the interfering auxiliary materials in the rabeprazole sodium enteric-coated tablets, and can ensure that the solvent compositions of the test solution and the reference solution are consistent, so that the accuracy of the dissolution determination result is ensured, the operation is simple, convenient and rapid, the method is suitable for the dissolution curve determination with large sample amount, and the problems of complex operation and low efficiency in the centrifugal mode in the prior art are effectively solved.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (8)
1. A dissolution curve determination method of rabeprazole sodium enteric-coated tablets is characterized by comprising the following steps: the method comprises the following steps:
s1, pretreatment of the test piece: taking 0.1mol/L hydrochloric acid solution as a dissolution medium, rotating at 50r/min, operating according to the method when the temperature of the dissolution medium reaches 37.0 +/-0.5 ℃, and taking out a test piece after 90-150 min;
s2, preparation of a test solution: taking a phosphate buffer solution with the pH of 6.0-6.8 as a dissolution medium, rotating at the speed of 50r/min, taking a pretreated test piece when the temperature of the dissolution medium reaches 37.0 +/-0.5 ℃, and continuing to operate according to the method; in a sampling tube, the ratio of hydrochloric acid: pre-adding 1mol/L hydrochloric acid solution and methanol according to the volume ratio of 1: 0.9-1, and respectively adding the hydrochloric acid solution: taking a proper amount of the dissolution liquid according to the volume ratio of 1: 8-8.1, placing the dissolution liquid in a sampling test tube, uniformly mixing, standing for 15-45 min, and filtering by using a filter membrane to obtain a test solution;
s3, preparation of control solutions: precisely weighing a rabeprazole sodium reference substance, placing the rabeprazole sodium reference substance into a measuring flask, dissolving and diluting the rabeprazole sodium reference substance by using methanol to scale, and shaking up; precisely measuring a proper amount of a placing bottle according to the mass ratio of methanol: 0.9-1% of hydrochloric acid: 1mol/L hydrochloric acid solution is added in the volume ratio of 1, a dissolution medium of phosphate buffer solution with the pH value of 6.0-6.8 is used for diluting to a scale, the volume ratio of the hydrochloric acid to the dissolution medium is 1: 8-8.1, the mixture is shaken up and kept stand at room temperature for 0.5-1 h to be used as a reference solution;
s4, measurement: and taking a proper amount of the reference substance solution and the test solution, respectively measuring the absorbance at the wavelength of 297-299 nm by an ultraviolet-visible spectrophotometry, and calculating.
2. The method for measuring the dissolution curve of rabeprazole sodium enteric-coated tablets according to claim 1, wherein: when the pH of the phosphate buffer solution of the dissolution medium in step S2 is 6.0, the volume ratio of hydrochloric acid to methanol in step S2 is 1:0.9, and after 20, 30, 40, 50, 60, 70, 80, and 90min, the following solutions of hydrochloric acid are added: taking the eluate at a volume ratio of 1:8.1, mixing with pre-added 1mol/L hydrochloric acid solution and methanol, standing for 30min, and filtering with filter membrane to obtain sample solution.
3. The method for measuring the dissolution curve of rabeprazole sodium enteric-coated tablets according to claim 2, wherein: the volume ratio of methanol to hydrochloric acid in step S3 was 0.9: 1, diluting to scale with a dissolution medium of a phosphate buffer solution with the pH value of 6.0, shaking uniformly, and standing for 0.5h at room temperature, wherein the volume ratio of hydrochloric acid to the dissolution medium is 1: 8.1.
4. The method for measuring the dissolution curve of rabeprazole sodium enteric-coated tablets according to claim 3, wherein: the detection wavelength of step S4 is 299 nm.
5. The method for measuring the dissolution curve of rabeprazole sodium enteric-coated tablets according to claim 1, wherein: when the pH of the phosphate buffer solution of the dissolution medium in the step S2 is 6.8, the volume ratio of hydrochloric acid to methanol in the step S2 is 1:1, and after 20, 25, 30, 35, 40 and 50min, the following solutions of hydrochloric acid are added: taking the dissolution liquid according to the volume ratio of 1:8, uniformly mixing the dissolution liquid with a pre-added 1mol/L hydrochloric acid solution and methanol, standing for 30min, and filtering by using a filter membrane to obtain a test solution.
6. The method for measuring the dissolution curve of rabeprazole sodium enteric-coated tablets according to claim 5, wherein: in the step S3, the volume ratio of methanol to hydrochloric acid is 1:1, the mixture is diluted to scale by using a dissolution medium of phosphate buffer solution with pH of 6.8, the volume ratio of hydrochloric acid to the dissolution medium is 1:8, the mixture is shaken up and kept stand at room temperature for 1 h.
7. The method for measuring the dissolution curve of rabeprazole sodium enteric-coated tablets according to claim 6, wherein: the detection wavelength of step S4 was 297 nm.
8. The method for measuring an elution profile of rabeprazole sodium enteric-coated tablets according to any one of claims 1 to 7, wherein: the phosphate of the phosphate buffer solution in steps S2 and S3 is selected from one of sodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, potassium phosphate, dipotassium hydrogen phosphate, and potassium dihydrogen phosphate; the pH regulator for regulating the pH value of the phosphate buffer solution is sodium hydroxide or potassium hydroxide.
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