2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Names and Identifiers
Name | AMLODIPINE BESYLATE
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Synonyms | Vazkor AMlodipine bes amlodipine besilate Amlodipine Beaylate AMLODIPINE BESYLATE Amlodopine Besilate raw material amlodipine besylate Amlodipine besilate (crystalline) 3-ethyl 5-methyl 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-6-methyl-1,4-dihydropyridine-3,5-dicarboxylate 3-ethyl 5-Methyl 2-((2-aMinoethoxy)Methyl)-4-(2-chlorophenyl)-6-Methyl-1,4-dihydropyridine-3,5-dicarboxylate benzenesulfonate 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate 2-[(2-Aminoethoxy)methyl]-4-(2-chlorophenyl)-1,4-dihydro-6-methyl-3,5-pyridinedicarboxylic acid 3-ethyl 5-methyl ester benzenesulfonate 3-Ethyl 5-Methyl 2-(2-Aminoethoxy)methyl-4-(2-chlorophenyl)-6-methyl-1,4-dihydropyridine-3,5-dicarboxylate Benzenesulfonate2-(2-Aminoethoxy)methyl-4-(2-chlorophenyl)-6-methyl-1,4-dihydropyridine-3,5-dicarboxylic Acid 3-Ethyl 5-Methyl Ester Benzenesulfona
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CAS | 111470-99-6
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EINECS | 1312995-182-4 |
InChI | InChI=1/C20H25ClN2O5.CH4O3S/c1-4-28-20(25)18-15(11-27-10-9-22)23-12(2)16(19(24)26-3)17(18)13-7-5-6-8-14(13)21;1-5(2,3)4/h5-8,17,23H,4,9-11,22H2,1-3H3;1H3,(H,2,3,4) |
InChIKey | ZPBWCRDSRKPIDG-UHFFFAOYSA-N |
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Physico-chemical Properties
Molecular Formula | C26H31ClN2O8S
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Molar Mass | 567.05094 |
Melting Point | 199-201°C |
Boling Point | 527.2°C at 760 mmHg |
Flash Point | 272.6°C |
Water Solubility | Soluble in DMSO (20 mg/mL), water (10 mM), chloroform, ethanol (14 mg/mL), and methanol. |
Solubility | DMSO: 20 mg/mL |
Vapor Presure | 3.34E-11mmHg at 25°C |
Appearance | white powder |
Color | white |
Merck | 14,491 |
pKa | 8.6 |
Storage Condition | 2-8°C |
MDL | MFCD00887594 |
Physical and Chemical Properties | Melting point 199-201°C
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In vitro study | Amlodipine benzenesulfonic acid reduces the decrease of p85aPI3K, phosphorylated Akt, phosphorylated GSK-3β, heat-shock transcription factor 1 and Bcl-2-induced H2O2, and cyclooxygenase-2, cytoplasmic cytochrome c, lysis of caspase9, and an increase in neuronal cell lysis of caspase3. In angiotensin Ⅱ-infused mice, Amlodipine significantly reduced systolic blood pressure (SBP), aortic hypertrophy, endothelial dysfunction, expression of LOX-1, aortic O2(-) and ONOO(-) production and plasma free 8-F(2) α-isoprostane levels. In isolated, precontracted, endothelium intact porcine coronary arteries, Amlodipine elicited NO-mediated relaxation and left-shift of concentration-relaxation curves of bradykinin. In native endothelial cells, Amlodipin increased NO production, detected by electron spin resonance spectroscopy, and stimulated cyclic GMP levels up to 8-fold in cultured endothelial cells. Amlodipine induces NO-mediated relaxation of rat aortic rings and does not express B2 receptors. In endothelial cells, Amlodipine time-dependently attenuates phosphorylation of protein kinase C(PKC), similar to the time course of phosphorylation of eNOS, and prevent the activation of PKC induced by phorbol -12-myristate -13-acetate. |
In vivo study | In cats, in porcine coronary arteries with intact endothelium, Amlodipine significantly reduced mean indirect systolic blood pressure from 198mm Hg to 155mm Hg. Amlodipine benzenesulfonic acid appears to be a safe and effective oral drug for the treatment of systemic hypertension in cats. |
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Risk and Safety
Hazard Symbols | Xn - Harmful
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Risk Codes | R22 - Harmful if swallowed
R36/37/38 - Irritating to eyes, respiratory system and skin.
R20/21/22 - Harmful by inhalation, in contact with skin and if swallowed.
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Safety Description | S26 - In case of contact with eyes, rinse immediately with plenty of water and seek medical advice.
S36 - Wear suitable protective clothing.
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WGK Germany | 3 |
RTECS | US7967700 |
HS Code | 29333990 |
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Standard
Authoritative Data Verified Data
This product is (±) -2-[(2-aminoethoxy) methyl] -4-(2-chlorophenyl)-1, 4-dihydro-6-methyl-3, 5-pyridinedicarboxylic acid -5-methyl ester, 3-ethyl benzenesulfonate. Calculated as dry product, containing no less than 98.5% of C20H25C1N205 • C6H6O3S.
Last Update:2024-01-02 23:10:35
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Trait
Authoritative Data Verified Data
- This product is white or off-white powder.
- This product is soluble in methanol or N,N-dimethylformamide, slightly soluble in ethanol, slightly soluble in water or acetone.
Last Update:2022-01-01 13:34:25
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Introduction
Relevant CAS code: 88150-42-9
Last Update:2022-10-16 17:12:07
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Differential diagnosis
Authoritative Data Verified Data
- a solution containing about 5mg of amlodipine per 1 ml was prepared by dissolving and diluting the product and the reference substance of amlodipine besylate with methanol, respectively, as a test solution and a reference solution. According to the thin layer chromatography (General 0502) test, each 10ml of the above two solutions are respectively put on the same silica gel G thin layer plate, and methyl isobutyl ketone-glacial acetic acid-water (2:1:1) the upper layer of liquid as the developer, after the expansion, dry, spray with dilute bismuth potassium iodide solution, the position and color of the main spot displayed by the test solution should be the same as the position and color of the main spot of the reference solution.
- take this product, add hydrochloric acid solution (0.9-1000) to dissolve and dilute to make a solution containing about 10ug of amlodipine per lml, shake, scanning in the range of 0401 to 400nm according to UV-Vis spectrophotometry (General Rule 200) has a maximum absorption at wavelengths of 239nm and 365nm and a minimum absorption at a wavelength of 225nm.
- The infrared absorption spectrum of this product should be consistent with that of the control (Spectrum set 790).
Last Update:2022-01-01 13:34:26
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Exam
Authoritative Data Verified Data
optical rotation
take 0.25g of this product, weigh it accurately, put it in a 25ml measuring flask, add methanol to dissolve and dilute it to the scale, shake it well. Determined by law (General rule 0621), the optical rotation should be a 0.10 ° to +0.10 °.
Related substances I
take an appropriate amount of this product, add methanol to dissolve and dilute to prepare a solution containing 70mg per lml as a test solution; Take an appropriate amount for precision measurement, solutions containing 0.21mg and 0.07mg, respectively, in 1 ml were prepared by dilution with methanol as Control Solutions (1) and (2). According to the thin layer chromatography (General 0502) test, absorb the above three solutions of 10 u1, respectively, on the same silica gel G thin layer plate, with methyl isobutyl ketone-glacial acetic acid-water (2:1:1) the upper layer liquid was used as a developing solvent, and after being developed, it was dried at 80 ° C. For 15 minutes, and examined under a UV lamp (254n and 365nm). Test solution such as impurity spots, compared with the control solution (1) of the main spot, not deeper (0.3%), deeper than the control solution (2) the impurity spots of the main spot should not be more than 2.
Related substances II
take an appropriate amount of this product, add the mobile phase to dissolve and dilute to prepare a solution containing lmg per lml as a test solution; Take an appropriate amount for precision measurement, A solution containing 3ug per 1 ml was prepared as a control solution by quantitative dilution with mobile phase. According to the test of high performance liquid chromatography (General rule 0512), with eighteen alkyl silane bonded Gui glue as filler (phenenex Luna Cl8 column, 4.6mm X 250mm,5um or equivalent column); the mobile phase was methanol-acetonitrile-0.7% triethylamine solution (7.0 of triethylamine was taken, diluted to 1000 with water, and adjusted to pH 3.0±0.1 with phosphoric acid)(35:15:50); the detection wavelength is 237nm, 5mg of amlodipine besylate reference substance is taken, 5ml of concentrated hydrogen peroxide solution is added, and the solution is heated at 70 ° C. For 10-30 minutes, and used as the system applicable solution. The system applicable solution 20u1 is injected into the human liquid chromatograph, record chromatogram, amlodipine peak retention time is about 18 minutes, the separation degree of amlodipine peak and amlodipine impurity I Peak (relative retention time is about 0.5) should be greater than 4.5, the number of theoretical plate is not less than 3000 according to amlodipine peak. 20 ml of the test solution and 20 ml of the control solution were respectively injected into the human liquid chromatograph, and the chromatogram was recorded to 3 times of the retention time of the main component peak. If there are impurity peaks in the chromatogram of the test solution, the peak area of amlodipine impurity I multiplied by 2 shall not be greater than the main peak area of the control solution (0.3% ) , the sum of the peak areas of other impurities shall not be greater than the main peak area of the control solution (0.3%). The chromatogram of the test solution is 0.1 times smaller than the main peak area of the control solution.
residual solvent
N-propanol about lOOmg, precision weighing, 500ml measuring flask, add N,N-dimethylformamide dissolved and diluted to the scale, shake, as an internal standard solution. Take the right amount of this product, precision weighing, plus internal standard solution dissolved and diluted into 200mg per lml solution, as a test solution. Accurately weigh the appropriate amount of methanol, ethanol, dichloromethane, tetrahydrofuran and dichloroethane respectively, accurately weigh the amount, add the internal standard solution to dissolve and dilute to make each lml respectively containing 0.6mg of methanol, A solution of 1.0 mg of ethanol, 0.12mg of dichloromethane, 0.144mg of tetrahydrofuran and 0.001 mg of dichloroethane was used as a control solution. Determined according to the residual solvent assay (General 0861 second method). (6%) cyanopropylphenyl-(94%) dimethylpolysiloxane (or polar similar) as a stationary liquid; The initial temperature is 40°C, maintain 10 minutes, the temperature was increased to 200°C at a rate of 40°C per minute for 3 minutes; The inlet temperature was 220°C and the detector temperature was 240°C; The equilibrium temperature of the headspace bottle was 80°C, the equilibration time was 20 minutes. Take the reference solution into the headspace, the separation degree between the peaks of each component should meet the requirements. Then the sample solution and the reference solution were accurately injected into the headspace, and the chromatograms were recorded. According to the internal standard method, the residual amount of methanol, ethanol, dichloromethane, tetrahydrofuran and dichloroethane shall be in accordance with the provisions.
chloride
take 0.5g of this product, add 25ml of methanol to dissolve it, put it in a 50ml Nessler's colorimetric tube, add 1.0mL of silver nitrate test solution, shake it well, and place it in the dark for 10 minutes. If it is turbid, filter it repeatedly, after the filtrate is completely clear, add 5.0 mL of standard sodium chloride solution, add water to make 50ml, shake well, and place in the dark for 5 minutes as a control solution; Take 0.5g of this product and add 25ml of methanol to dissolve, put 50ml Nessler's colorimetric tube, add 1.0ml of silver nitrate test solution, add water to make it 50ml, shake well, place in the dark for 5 minutes, and check according to law (General rule 0801), compare with the control solution, no more concentrated (0.01%).
loss on drying
take this product, dry to constant weight at 105°C, weight loss shall not exceed 0.5% (General rule 0831).
ignition residue
take l.Og of this product and check it according to law (General rule 0841). The residue left shall not exceed 0.1%.
Iron Salt
take this product l.Og, full Ash at 500~600°C, add 10% G potassium hydrogen sulfate to heat to melt, cool, add hydrochloric acid solution, heat to boiling to dissolve, cool, transfer to a 50ml measuring flask and dilute to the scale with water. Take 25ml, check according to law (General rule 0807), compared with the standard iron solution 1.0 ml of the control solution made by the same method, not deeper (0.002%).
Heavy metals
The residue left under the item of taking the ignition residue shall not contain more than 10 parts per million of heavy metal when examined by law (General Principles 0821, Law II).
Last Update:2022-01-01 13:34:27
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Content determination
Authoritative Data Verified Data
take about 0.5g of this product, precision weigh, add methanol 25ml to dissolve, Precision Add lmol/L perchloric acid solution (take 70% ~ 72% perchloric acid 8.5ml, add water to 100ml)25ml and 2 drops of ortho-diphenanthroline indicator solution, immediately with cerium sulfate titration solution (O. 1 mol/L) titration until the orange-red color disappeared, and the results of the titration were corrected with a blank test. Per 1 ml of cerium sulfate titration solution (0.1 mol/U corresponds to 28.35mg of C20H25C1N205.C6H603S.
Last Update:2022-01-01 13:34:28
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Category
Authoritative Data Verified Data
calcium channel blockers.
Last Update:2022-01-01 13:34:28
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Storage
Authoritative Data Verified Data
light shielding, sealed storage.
Last Update:2022-01-01 13:34:28
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Amlodipine besylate tablets
Authoritative Data Verified Data
This product contains amlodipine besylate according to amlodipine (C20H25C1N205), should be 90.0% ~ 110.0% of the label amount.
trait
This product is white or off-white.
identification
- take an appropriate amount of fine powder of this product (equivalent to 20mg of ammonidipine), add 4ml of methanol, sonicate for about 20 minutes to dissolve amlodipine besylate, filter, and take the filtrate as the test solution; A control substance containing amlodipine in an amount of 5mg per 1 ml was prepared by dissolving and diluting the control substance with methanol. According to the thin layer chromatography (General 0502) test, absorb the above two solutions of each lol, respectively, on the same silica gel G thin layer plate, with methyl isobutyl ketone-glacial acetic acid-water (2:1:1) the upper layer of the liquid is the developer, which is spread out, dried, and sprayed with dilute bismuth potassium chloride solution. The position and color of the main spot of the test solution should be the same as that of the reference solution.
- in the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the reference solution.
- take an appropriate amount of fine powder of this product, add hydrochloric acid solution (0.9-1000) to dissolve and dilute amlodipine besylate amlodipine 10% solution per 1 ml, shake, filter, the filtrate is scanned in the range of 0401 ~ 400nm by UV-Vis spectrophotometry (General Rule 200), with maximum absorption at wavelength of 239nm and 365nm, there is minimal absorption at a wavelength of 225nm ± 3nm.
- two items (1) and (2) above can be selected as one item.
examination
- Related Substances: take an appropriate amount of fine powder of this product (about 50mg equivalent to amlodipine), put it in a 50m l measuring flask, add about 40ml of mobile phase, sonicate for about 30 minutes to dissolve amlodipine besylate, and take it out, cool, dilute to the scale with mobile phase, shake well, filter, and take the filtrate as the test solution. Take lml with precision, put it in a 100ml measuring flask, dilute to the scale with mobile phase, as a control solution. According to the chromatographic conditions under the content determination item, 20ul of each of the test solution and the control solution are accurately measured and injected into the human liquid chromatograph respectively, and the chromatogram is recorded to 3 times of the retention time of the main component peak. If there is an impurity peak in the chromatogram of the test solution, the peak area of amlodipine impurity I Peak (relative retention time about 0.5) multiplied by 2 shall not be greater than the main peak area (1.0%) of the control solution, other single impurity peak area shall not be greater than 0.5 times (0.5%) of the main peak area of the control solution, the sum of the peak area of amlodipine impurity I peak multiplied by 2 and the peak area of each other impurity shall not be greater than 1.5 times (1.5%) of the main peak area of the control solution. The chromatogram of the test solution is 0.03 times smaller than the main peak area of the control solution.
The content uniformity of - shall be calculated from the content of each tablet measured under the content determination item, and shall comply with the regulations (General rule 0941).
- dissolution of this product, according to the dissolution and release determination method (General 0931 second method), with hydrochloric acid solution (0.9-1000)500ml as the dissolution medium, the rotation speed is 75 rpm, and the operation is carried out according to law. After 30 minutes, the appropriate amount of the solution is taken, filtered, and the appropriate amount of the filtrate is taken, the solution containing amlodipine 5ug per 1 ml was prepared by quantitative dilution with dissolution medium as the test solution, an appropriate amount of methanol was added and dissolved, and then diluted with a dissolution medium to prepare a solution containing about 5% of amlodipine per 1 ml as a reference solution. The dissolution amount of each tablet was calculated as measured by the method under the content measurement item. The limit is 80% of the labeled amount and shall be in accordance with the provisions.
- others shall be in accordance with the relevant provisions under the item of tablets (General rule 0101).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system suitability test using eighteen alkyl silane bonded silica gel as filler (phenmenex Luna Cl8 column, 4.6mm X 250mm,5um or equivalent chromatography column with methanol-acetonitrile-0.7% triethylamine solution (take triethylamine 7.0ml, add water to 3.0 ml, adjust the pH value to 0.1 ± with phosphoric acid) (35:15:50) mobile phase; The detection wavelength was 237nm. Take 5mg of benzenesulfonic acid ammonia dipine reference substance, add 5ml of concentrated hydrogen peroxide solution, heat at 70°C for 10~30 minutes, as the system applicable solution, take 20ul of system applicable solution and inject human liquid chromatograph, record chromatogram, the retention time of amlodipine peak is about 18 minutes, the separation degree of amlodipine peak and amlodipine impurity I Peak (relative retention time is about 0.5) should be more than 4.5, and the number of theoretical plates is not less than 3000 based on the amlodipine peak.
- determination of 10 tablets of this product, respectively, in 50ml(15mg specification), 100ml(5m g specification) or 200ml (10 mg specification) measuring flask, add about 30ml mobile phase, ultrasound for about 30 minutes to dissolve amlodipine besylate, cool, dilute to the scale with mobile phase, shake, filter, take the filtrate as the test solution, and inject it into the liquid chromatograph, the chromatogram was recorded. In addition, an appropriate amount of amlodipine besylate reference substance was carefully weighed, dissolved and quantitatively diluted with mobile phase to prepare a solution containing about 50% amlodipine per 1 ml, which was determined by the same method. The content of each tablet was calculated by peak area according to external standard method, and the average content of 10 tablets was obtained.
category
Same as amlodipine besylate.
specification
Based on C20H25C1N205 (l) 2.5mg (2) 5mg(3) 10 mg
storage
light shielding, sealed storage.
Last Update:2022-01-01 13:34:29
2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine benzenesulfonate - Amlodipine besylate capsules
Authoritative Data Verified Data
This product contains amlodipine besylate according to amlodipine (C20H25C1N205), should be 90.0% ~ 110.0% of the label amount.
trait
The content of this product is white or white particles or powder.
identification
- take an appropriate amount of the contents of this product (equivalent to 20mg of amlodipine), add 4ml of methanol, sonicate for 20 minutes to dissolve amlodipine besylate, filter, and take the filtrate as the test solution; an additional amlodipine besylate control was dissolved in methanol and diluted to prepare a solution containing 5mg of amlodipine per 1 ml as a control solution. According to the thin layer chromatography (General 0502) test, absorb the above two solutions of 10 u1, respectively, on the same silica gel G thin layer plate, with methyl isobutyl ketone-glacial acetic acid (2:1:1) the upper layer of the liquid is the developing agent, which is spread out, dried, and sprayed with dilute bismuth potassium iodide solution. The position and color of the main spot of the test solution should be the same as that of the reference solution.
- in the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the reference solution.
- take an appropriate amount of the contents of this product, add hydrochloric acid solution (0.9-1000) to dissolve amlodipine besylate and dilute it to make a solution containing amlodipine 10ug per 1 ml, shake well, filter, the filtrate is scanned in the range of 0401 ~ 400nm by UV-Vis spectrophotometry (General Rule 200), with maximum absorption at wavelength of 239nm and 365nm, there is minimal absorption at a wavelength of 225mn.
- two items (1) and (2) above can be selected as one item.
examination
- relevant substances: take an appropriate amount of the contents of this product (about 50mg equivalent to that of ammonia and amlodipine), put it in a 50ml measuring flask, add about 40ml of mobile phase, sonicate it for about 30 minutes to dissolve amlodipine besylate, take it out and cool it, dilute to the scale with mobile phase, shake, filter, and take the filtrate as the test solution; Take 1ml with precision, put it in a 100ml measuring flask, dilute to the scale with mobile phase, and shake well, as a control solution. According to the chromatographic conditions under the content determination item, 20ul of each of the test solution and the control solution are accurately measured and injected into the human liquid chromatograph respectively, and the chromatogram is recorded to 3 times of the retention time of the main component peak. If there is an impurity peak in the chromatogram of the test solution, the peak area of amlodipine impurity I (relative retention time about 0.5) multiplied by 2 shall not be greater than the main peak area of the control solution (1.0%), other single impurity peak area shall not be greater than 0.5 times (0.5%) of the main peak area of the control solution, the sum of the peak area of amlodipine impurity 1 multiplied by 2 and the peak area of each other impurity shall not be greater than 1.5 times (1.5%) of the main peak area of the control solution. The chromatogram of the test solution is 0.03 times smaller than the main peak area of the control solution.
The content uniformity of - shall be calculated based on the content of each particle measured under the content determination item, and shall comply with the regulations (General rule 0941).
- dissolution of this product, according to the dissolution and release determination method (General rule 0931 The first method), with hydrochloric acid solution (0.9-1000)500ml as the dissolution medium, after 30 minutes, take the appropriate amount of solution, filter, and take the filtrate as the test solution; Take the appropriate amount of amlodipine besylate reference product, and weigh it precisely, A solution containing about 10ug of amlodipine per 1 ml was prepared as a control solution by quantitative dilution with a dissolution medium after dissolving in an appropriate amount of methanol. According to the method under the content determination item, according to the law, the dissolution amount of each grain is calculated. The limit is 80% of the labeled amount and shall be in accordance with the provisions.
- others should comply with the relevant provisions under the capsule (General 0103).
Content determination
- measured by high performance liquid chromatography (General 0512).
- chromatographic conditions and system suitability test using eighteen alkyl silane bonded silica gel as filler (phenmenex Luna Cl8 column, 4.6mm X 250mm,5um or equivalent performance column); using methanol-acetonitrile-0.7% triethylamine solution (take triethylamine 7.0ml, add water to 3.0 ml, adjust the pH value to 0.1 ± with phosphoric acid)(35:15:50) as mobile phase; the detection wavelength was 237nm. Take 5mg of the reference substance of amidipine benzenesulfonate, add 5ml of concentrated hydrogen peroxide solution, and heat at 70°C for 10-30 minutes as the applicable solution for the system. Take 20ul of the applicable solution for the system and inject it into the liquid chromatograph to record the chromatogram, the retention time of amlodipine peak is about 18 minutes, the separation degree of amlodipine peak and amlodipine impurity I Peak (relative retention time is about 0.5) should be more than 4.5, and the number of theoretical plates is not less than 3000 based on the amlodipine peak.
- determination method 10 capsules of this product were poured into a 100ml measuring flask, the capsule shell was washed with an appropriate amount of mobile phase, and the liquid was washed into the measuring flask, add appropriate amount of mobile phase and ultrasound for about 30 minutes to dissolve amlodipine besylate, cool down, dilute to the scale with mobile phase, shake well, filter, take the continued filtrate as the test solution, and take 20ul with precision, human liquid chromatograph was used and the chromatogram was recorded. In addition, an appropriate amount of amlodipine besylate reference substance was carefully weighed, dissolved and quantitatively diluted with mobile phase to prepare a solution containing about 50% amlodipine per 1 ml, which was determined by the same method. According to the external standard method, the content of each grain is calculated by Peak area, and the average content of 10 grains is obtained.
category
Same as amlodipine besylate.
specification
5mg (according to C20H25ClN205)
storage
light shielding, sealed storage.
Last Update:2022-01-01 13:34:31