125-69-9 - Names and Identifiers
Name | dextromethorphan hydrobromide
|
Synonyms | dextromethorphan HBR Dextromethorphan maleate HBR dextromethorphan hydrobromide Destromethorphan hydrobromide 3-methoxy-17-methylmorphinan hydrobromide (9alpha,13alpha,14alpha)-3-methoxy-17-methylmorphinan hydrobromide (9alpha,13alpha,14alpha)-3-methoxy-17-methylmorphinan hydrobromide hydrate
|
CAS | 125-69-9
|
EINECS | 204-750-1 |
InChI | InChI=1/C18H25NO.BrH.H2O/c1-19-10-9-18-8-4-3-5-15(18)17(19)11-13-6-7-14(20-2)12-16(13)18;;/h6-7,12,15,17H,3-5,8-11H2,1-2H3;1H;1H2/t15-,17+,18+;;/m1../s1 |
125-69-9 - Physico-chemical Properties
Molecular Formula | C18H28BrNO2
|
Molar Mass | 370.324 |
Boling Point | 486.1°C at 760 mmHg |
Flash Point | 247.8°C |
Vapor Presure | 2.92E-10mmHg at 25°C |
Use | Used as a central nervous antitussive |
125-69-9 - Standard
Authoritative Data Verified Data
This product is 3-methoxy-17-methyl-(9a,13a,14a)-morphopyran hydrobromide monohydrate, calculated as anhydrous, the C18 h25no. HBr should be 98.0% to 102.0%.
Last Update:2024-01-02 23:10:35
125-69-9 - Trait
Authoritative Data Verified Data
- This product is white or off-white crystalline powder, odorless.
- This product is soluble in ethanol, dissolved in chloroform, slightly soluble in water, insoluble in ether.
specific rotation
take this product, precision weighing, add 0.1 mol/L hydrochloric acid solution was dissolved and quantitatively diluted to give a solution containing about 20mg per 1 ml, which was measured according to law (General 0621). The specific rotation was 28.0 ° to 30.0 °.
Last Update:2022-01-01 13:42:12
125-69-9 - Differential diagnosis
Authoritative Data Verified Data
- take about 25mg of this product, add 5ml of water to dissolve, add 5 drops of 2mol/L nitric acid solution and 2ml of silver nitrate test solution to produce yellow precipitate.
- take this product and use 0.1 mol/L hydrochloric acid solution is prepared to contain about 0. A solution of 1 mg has a maximum absorption at a wavelength of 0401 mn and a minimum absorption at a wavelength of 245mn, as determined by UV-Vis spectrophotometry (general rule).
- The infrared absorption spectrum of this product should be consistent with that of the reference product (General rule 0402).
Last Update:2022-01-01 13:42:12
125-69-9 - Exam
Authoritative Data Verified Data
acidity
take 0.20g of this product, add 20ml of water to dissolve, and then measure it according to law (General rule 0631). The pH value should be 5.2~6.5.
clarity and color of ethanol solution
take 0.5g of this product and add 10ml of ethanol to dissolve. The solution should be clear and colorless. N,N-dimethylaniline take 0.50g of this product, add water 20ml, heat and dissolve in water bath and cool, add 1 mol/L acetic acid solution 2ml and 1% sodium nitrite solution 1 ml, add water to make 25ml, shake; If color, with the control solution (take N,N-dimethylaniline reference material 20mg, precision weighing, put into 20ml measuring flask, add appropriate amount of water, dissolve in water bath with warm heat, dilute to scale with water, shake well, take 1.0ml, put it in 200ml measuring flask, dilute to scale with water, shake well) lml, the color comparison after treatment with the same method shall not be deeper (0.001%). Take about 5mg of quinone compound, add 1 drop of 3mol/L hydrochloric acid solution, 2 drops of water 1 ml and ferric chloride solution, mix well, add 2 drops of potassium ferricyanide solution, and do not show blue-green after 2 minutes.
Related substances
take an appropriate amount of this product, add the mobile phase to dissolve and dilute to make a solution containing about 1.5mg per lml as a test solution; Take lml for precision measurement and put it in a 100ml measuring flask, dilute to the scale with the mobile phase, shake, and serve as a control solution. The control solution (1 ml) was accurately weighed, placed in a 20ml measuring flask, diluted to the scale with mobile phase, and shaken to obtain a sensitivity solution. According to the chromatographic conditions under the content determination item, take the sensitivity solution 20 u1 and inject the human Liquid Chromatograph. The signal-to-noise ratio of the main component peak height should be greater than 10. 20ul of the test solution and the control solution were respectively injected into the human liquid chromatograph, and the chromatogram was recorded to 2.5 times of the retention time of the main component peak. If there are impurity peaks in the chromatogram of the test solution shown in the table below, impurities I, II, IV and impurity III multiplied by the correction factor (correction factor is 0.2) the peak area shall not be greater than 0.5 times (0.5%) of the main peak area of the control solution, and the peak area (or corrected peak area) no more than 1 impurity peak shall be included between 0.25 and 0.5 times of the main peak area of the control solution; The area of other single impurity peak shall not be greater than 0.1 times (0.1%) of the main peak area of the control solution, the sum of each impurity peak area after correction shall not be greater than the main peak area of the control solution (1.0%). The chromatographic peaks in the chromatogram of the test solution which are smaller than the main peak area of the sensitivity solution are ignored.
residual solvent
take this product about lg, precision weighing, put in 20ml headspace bottle, Precision Add 5ml dimethyl sulfoxide to dissolve, seal, as a test solution; Another methanol, the appropriate amount of acetone and toluene, precision weighing, diluted with dimethyl sulfoxide made each lml containing 0.6mg, l. 5ml of a mixed solution of 0 mg and 0.18mg was precisely weighed, placed in a 20ml headspace bottle, sealed, and used as a reference solution. According to the test for determination of residual solvents (General rule 0861 second method), the capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane (or similar polarity) as stationary liquid is used as the column; The initial temperature is 32°C, maintain 7 minutes, at a rate of 50°C per minute to 200°C, maintain 3 minutes; Injection port temperature of 150°C, detector temperature of 250°C; Headspace bottle equilibrium temperature of 80°C, the equilibration time was 30 minutes. Take the reference solution into the headspace, record the chromatogram, and the separation degree between the chromatographic peaks should meet the requirements. Then the sample solution and the reference solution were injected with headspace, and the chromatogram was recorded. According to the external standard method to calculate the peak area, methanol, acetone and toluene residues should be in accordance with the provisions.
moisture
take this product, according to the moisture determination method (General 0832 first method 1), the moisture should be 3.5% ~ 5.5%.
ignition residue
not more than 0.1% (General rule 0841).
Last Update:2022-01-01 13:42:14
125-69-9 - Content determination
Authoritative Data Verified Data
measured by high performance liquid chromatography (General 0512).
chromatographic conditions and system suitability test
silica gel bonded with octanoalkyl silane as a filler (Agilent Zorbax SBC18, 4.6mm X 250mm, 5um or equivalent chromatography column); Buffer solution (sodium sulfosuccinate dioctyl ester 3.llg and ammonium nitrate 0.56g, add water 450ml and acetonitrile 300ml to dissolve, adjust pH to 2.0 with glacial acetic acid 220ml, dilute to 1000ml with water)-acetonitrile (72:28) as mobile phase; the detection wavelength was 280mn. Take an appropriate amount of dextromethorphan hydrobromide, add water to dissolve and dilute to make a solution containing about 1.5mg per 1 ml, put under UV lamp (365mn) for 24 hours, as the system applicable solution, take 20fxl injection liquid chromatograph, the flow rate or column temperature is adjusted so that the retention time of the main component chromatographic peak is about 16 minutes, and the separation degree of the dextromethorphan peak and the impurity II peak should be greater than 3.5.
assay
take an appropriate amount of this product, precision weigh, add mobile phase to dissolve and quantitatively dilute to make a solution containing about 0.5mg per lml, take a 20ul injection into the human liquid chromatograph, record the chromatogram; another amount of dextromethorphan hydrobromide reference substance was determined by the same method. According to the external standard method to calculate the peak area, that is.
Last Update:2022-01-01 13:42:14
125-69-9 - Category
Authoritative Data Verified Data
Last Update:2022-01-01 13:42:14
125-69-9 - Storage
Authoritative Data Verified Data
light shielding, sealed storage.
Last Update:2022-01-01 13:42:15
125-69-9 - Dextromethorphan Hydrobromide Oral Solution
Authoritative Data Verified Data
dextromethorphan hydrobromide (C18H25NO • HBr • H20) should be 90.0% to 110.0% of label load.
trait
This product is a yellowish to yellow clear liquid.
identification
- 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.
- This product bromide identification (1) of the reaction (General 0301).
examination
- relative density the relative density of this product (General 0601) should not be less than 1.10.
- the pH value should be 4.0 to 6.0 (General 0631).
- appropriate amount of related substances should be taken, dissolved and diluted with mobile phase to make a solution containing about 1.5mg per 1ml, which should be used as a test solution; 1ml should be accurately measured and placed in a 100ml measuring flask, dilute to the scale with the mobile phase, shake, and serve as a control solution. 1ml of the control solution was accurately measured, placed in a 20ml measuring flask, diluted to the scale with mobile phase, and shaken to serve as a sensitivity solution. The determination was carried out according to the method described under dextromethorphan hydrobromide related substances. If there are impurity peaks shown in the following table in the chromatogram of the test solution, except for the peaks of excipients before the relative retention time of 0.3, impurities I, II, the Peak area of IV and impurity III (correction factor is 0.2) multiplied by the correction factor shall not be greater than the main peak area of the control solution (1.0% ) , and the peak area (or corrected peak area) no more than 1 impurity peak shall be found between 0.5 and 1.0 times of the main peak area of the control solution; The area of other single impurity peak shall not be greater than the main peak area of the control solution (1.0% ) , the sum of each impurity peak area after correction shall not be greater than 2 times (2.0%) of the main peak area of the control solution. The chromatographic peaks in the chromatogram of the test solution which are smaller than the main peak area of the sensitivity solution are ignored.
- others should comply with the relevant provisions under the item of oral solution (General rule 0123).
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 (Agilent Zorbax SBC18, 4.6mm X 250mm, 5um or equivalent performance column); with buffer solution (sodium sulfosuccinate dioctyl ester 3.llg and ammonium nitrate 0.56g, add water 450ml and acetonitrile 300ml to dissolve, adjust pH to 2.0 with glacial acetic acid 220ml, dilute to 1000ml with water)-acetonitrile (72:28) as mobile phase; the detection wavelength was 280nm. An appropriate amount of dextromethorphan hydrobromide was taken, dissolved in water and diluted to prepare a solution containing about 1.5mg per 1 ml, and irradiated with a UV lamp (365nm) for 24 hours as a system-suitable solution. 20ul injection liquid chromatograph, adjust the flow rate or column temperature, so that the retention time of the main component chromatographic peak is about 16 minutes, and the separation degree of dextromethorphan peak and impurity DI peak should be greater than 3.5.
- determination precision: take an appropriate amount of this product, quantitatively dilute it with mobile phase to prepare a solution containing about 0.75mg per lml, shake well, filter, and take the continued filtrate as the test solution, accurately inject 20ul into the liquid chromatograph, record the chromatogram; Take an appropriate amount of dextromethorphan hydrobromide reference, and precisely weigh it, A solution containing about 0.75mg of dextromethorphan hydrobromide (calculated as C18H25NO. HBr. H20) per 1 ml was prepared by dissolution and quantitative dilution with the mobile phase and determined by the same method. According to the external standard method to calculate the peak area, that is.
category
Same as dextromethorphan hydrobromide.
specification
(l)lOml:15mg; (2) 120ml:180mg (3)100ml:150mg
storage
light shielding, sealed storage.
Last Update:2022-01-01 13:42:16
125-69-9 - Dextromethorphan Hydrobromide Tablets
Authoritative Data Verified Data
dextromethorphan hydrobromide (C18H25NO • HBr • H20) should be 90.0% to 110.0% of label load.
trait
This product is a white tablet or sugar-coated tablet, White after removing the sugar coating.
identification
- 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, shake with water, filter, and identify (1) bromides in the filtrate (General rule 0301).
examination
- relevant substances: take an appropriate amount of fine powder of this product, dissolve it with mobile phase and dilute it to make a solution containing about 1.5mg per 1ml as a test solution; Take 1ml for precision measurement and put it in a 100ml measuring flask, dilute to the scale with the mobile phase, shake, and serve as a control solution. 1ml of the control solution was accurately measured, placed in a 20ml measuring flask, diluted to the scale with mobile phase, and shaken to serve as a sensitivity solution. According to the method for the determination of related substances of dextromethorphan hydrobromide, if there are impurity peaks shown in the table below in the chromatogram of the test solution, except for the peaks of excipients before the relative retention time of 0.3 times, impurities I, II, the Peak area of IV and impurity III (correction factor is 0.2) multiplied by the correction factor shall not be greater than the main peak area of the control solution (1.0% ) , and the peak area (or corrected peak area) no more than 1 impurity peak shall be found between 0.5 and 1.0 times of the main peak area of the control solution; The area of other single impurity peak shall not be greater than that of the main peak area of the control solution (1.0% ) , the sum of each impurity peak area after correction shall not be greater than 2 times (2.0%) of the main peak area of the control solution. The chromatographic peaks in the chromatogram of the test solution which are smaller than the main peak area of the sensitivity solution are ignored.
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).
- the dissolution of this product, according to the dissolution and release determination method (General rule 0931 first method), water 900ml as the dissolution medium, the speed of 50 rpm, according to the law, after 30 minutes, take the appropriate amount of the solution, filter, take the filtrate as the test solution; Take the dextromethorphan hydrobromide control, precision weighing, water was added for dissolution and quantitative dilution to prepare a solution containing about 17ug of dextromethorphan hydrobromide (calculated as C18H25NO. HBr. H20) per 1 ml as a control solution. According to the chromatographic conditions under the content determination item, 100 u1 of each of the above two solutions is accurately measured, respectively injected into human liquid chromatography, the chromatogram is recorded, and the dissolution amount of each tablet is calculated by peak area according to external standard method. 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 (Agilent Zorbax SBC18,4.6mm x 250mm, 5um or equivalent performance column); with buffer solution (sodium sulfosuccinate dioctyl ester 3.llg and ammonium nitrate 0.56g, add water 450ml and acetonitrile 300ml to dissolve, adjust pH to 2.0 with glacial acetic acid 220ml, dilute to 1000ml with water)-acetonitrile (72:28) as mobile phase; the detection wavelength was 280nm. An appropriate amount of dextromethorphan hydrobromide was taken, dissolved in water and diluted to prepare a solution containing about 1.5mg per 1 ml, and irradiated with a UV lamp (365nm) for 24 hours as a system-suitable solution. 20u1 is injected into the liquid chromatograph to adjust the flow rate or column temperature so that the retention time of the main component chromatographic peak is about 16 minutes, and the separation degree of the dextromethorphan peak and the impurity HI peak should be greater than 3.5.
- determination: 10 tablets of this product were placed in a 20ml measuring flask respectively, and the appropriate amount of mobile phase was added. Dextromethorphan hydrobromide was dissolved by ultrasound and allowed to cool, the continuous filtrate was taken as the test solution, and injected into the liquid chromatograph with precise volume to record the chromatogram, A solution containing about 0.75mg of dextromethorphan hydrobromide (calculated as C18H25NO. HBr. H20) per 1 ml was prepared by dissolution and quantitative dilution with the mobile phase and 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 dextromethorphan hydrobromide.
specification
15mg
storage
light shielding, sealed storage.
Last Update:2022-01-01 13:42:17
125-69-9 - Dextromethorphan Hydrobronmde Capsules
Authoritative Data Verified Data
This product contains dextromethorphan hydrobromide (C18H25NO • HBr • H20) should be 90.0% to 110.0% of the sample size.
trait
The content of this product is white powder.
identification
- take an appropriate amount of the content of this product (about 0.15g equivalent to dextromethorphan hydrobromide), add 15ml of water to dissolve dextromethorphan hydrobromide, shake, filter, take the filtrate, identify the bromide (1) response (General rule 0301).
- 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.
examination
- relevant substances: take an appropriate amount of the contents of this product, add the mobile phase, dissolve it and dilute it to make a solution containing about 1.5mg per 1 ml, which is used as a test solution; Take a precise amount of lml and place it in a 100ml measuring flask, dilute to the scale with the mobile phase, shake, and serve as a control solution. Take 1 ml of the control solution in a 20m l volumetric flask, dilute to the scale with the mobile phase, and shake to obtain the sensitivity solution. According to the method for the determination of related substances of dextromethorphan hydrobromide, if there are impurity peaks shown in the table below in the chromatogram of the test solution, except for the peaks of excipients before the relative retention time of 0.3, impurities I, II, the Peak area of 1V and impurity III (correction factor is 0.2) multiplied by the correction factor shall not be greater than the main peak area of the control solution (1.0% ) , and the peak area (or corrected peak area) no more than 1 impurity peak shall be found between 0.5 and 1.0 times of the main peak area of the control solution; The area of other single impurity peak shall not be greater than that of the main peak area of the control solution (1.0% ) , the sum of each impurity peak area after correction shall not be greater than 2 times (2.0%) of the main peak area of the control solution. The chromatographic peaks in the chromatogram of the test solution which are smaller than the main peak area of the sensitivity solution are ignored.
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 0931 first method), with 0.100 ml of 1 mol/L hydrochloric acid solution is the dissolution medium, the rotation speed is rpm, and the operation is carried out according to law. After 30 minutes, the appropriate amount of the solution is taken, filtered, and the filtrate is taken as the test solution; an appropriate amount of dextromethorphan hydrobromide control product was carefully weighed, dissolved and quantitatively diluted with dissolution medium to prepare a solution containing about 30ug of dextromethorphan hydrobromide (calculated as C18H25NO. HBr. H20) per 1 ml as a control solution. According to the chromatographic conditions under the content determination item, respectively inject the above two kinds of solutions respectively into the liquid chromatograph, record the chromatogram, and calculate the dissolution amount of each particle by peak area according to the external standard method. The limit is 85% 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 (Agilent Zorbax SBC18,4.6mm X 250mm,5um or equivalent performance column); with buffer solution (sodium sulfosuccinate dioctyl ester 3.llg and ammonium nitrate 0.56g, add water 450ml and acetonitrile 300ml to dissolve, adjust pH to 2.0 with glacial acetic acid 220ml, dilute to 1000ml with water)-acetonitrile (72:28) as mobile phase; the detection wavelength was 280nm. An appropriate amount of dextromethorphan hydrobromide was taken, dissolved in water and diluted to prepare a solution containing about 1.5mg per 1 ml, and irradiated with a UV lamp (365nm) for 24 hours as a system-suitable solution. 20ul injection liquid chromatograph, adjust the flow rate or column temperature, so that the retention time of the main component chromatographic peak is about 16 minutes, and the separation degree of dextromethorphan peak and impurity III peak should be greater than 3.5.
- determination method: 10 capsules of this product were poured into 50ml measuring flask, the capsule shell was washed with a small amount of mobile phase, the washing solution was incorporated into the measuring flask, the appropriate amount of mobile phase was added, and dextromethorphan hydrobromide was dissolved by ultrasound, cool, dilute to the scale with mobile phase, shake, filter, take the filtrate as the test solution, and inject 20ul into the liquid chromatograph to record the chromatogram, precision weighing, plus mobile phase dissolution and quantitative dilution of dextromethorphan hydrobromide (according to C18H25NO • HBr • H20) 0.3mg per 1 ml of the solution, 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 dextromethorphan hydrobromide.
specification
15mg
storage
light shielding, sealed storage.
Last Update:2022-01-01 13:42:18
125-69-9 - Dextromethorphan Hydrobromide sustained release tablets
Authoritative Data Verified Data
This product contains dextromethorphan hydrobromide (C18H25NO • HBr • H20) should be the standard 7K amount of 90.0% ~ 110.0%.
trait
This product is white or off-white.
identification
- take an appropriate amount of fine powder of this product (about 0.15g equivalent to dextromethorphan hydrobromide), add 15ml of water, shake to dissolve dextromethorphan hydrobromide, filter, take 0.5ml of filtrate, and put it on a water bath to evaporate, A few drops of the new molybdenum sulfuric acid test solution were added to the residue, which showed yellow green.
- The filtrate remaining under identification (1) was taken and the bromide was identified for the reaction of (1) (General 0301).
- 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.
examination
- the dissolution of this product, according to the dissolution and release determination method (General rule 0931 third method), with water as the dissolution medium, the speed is 50 rpm, according to the law, at 2 hours, 4 hours, 8 hours, respectively, take 10ml solution, filtered, and immediately supplemented with the same temperature, the same volume of dissolution medium, the filtrate was measured at the wavelength of 278mn by UV-Vis spectrophotometry (General rule 0401); Another dextromethorphan hydrobromide reference substance was taken, water was added to dissolve and quantitatively diluted to prepare a solution containing about 8 ug per 1 ml. The absorbance was measured by the same method, and the dissolution amount of each tablet at different times was calculated. The dissolution amount of each tablet in 2 hours, 4 hours and 8 hours shall be 30% ~ 60%, 45% ~ 70% and more than 70% of the label amount, and shall comply with the regulations.
- 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, phosphate buffer (5ml each of phosphoric acid and triethylamine, add water to 1000ml, Mix)-acetonitrile (70:30) as mobile phase; The detection wavelength was 278nm. The theoretical plate number is not less than 1500 as calculated from the dextromethorphan peak.
- determination of 20 tablets of this product, precision weighing, fine, precision weighing an appropriate amount (about 37.5mg equivalent to dextromethorphan hydrobromide), put it in a 50ml measuring flask, add an appropriate amount of mobile phase, ultrasonic dissolution of dextromethorphan hydrobromide, diluted to scale with mobile phase, shake well, filter, Take 5ml of continuous filtrate precisely, put it in a 25ml measuring flask, dilute to scale with mobile phase, shake well, as the test solution, the 2CV1 was accurately measured and injected into the human liquid chromatograph to record the chromatogram, the mobile phase was added and dissolved and diluted to prepare a solution containing 0.15mg per 1 ml, which was determined by the same method. According to the external standard method, the peak area is calculated, and the calculated result is multiplied by 1.051.
category
Same as dextromethorphan hydrobromide.
specification
30mg
storage
light shielding, sealed storage.
Last Update:2022-01-01 13:42:20
125-69-9 - Dextromethorphan Hydrobromide granules
Authoritative Data Verified Data
dextromethorphan hydrobromide (C18H25NO • HBr • H20) should be 90.0% to 110.0% of label load.
trait
This product is white particles.
identification
- take an appropriate amount of fine powder of this product (about 0.15g equivalent to dextromethorphan hydrobromide), add 15ml of water, shake to dissolve dextromethorphan hydrobromide, filter, take filtrate, identify bromide (1) response (General rule 0301).
- 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.
examination
- relevant substances: take an appropriate amount of the contents of this product, add the mobile phase, dissolve it and dilute it to make a solution containing about 1 mg per 1 ml, which is used as a test solution; Take a precise amount of 1 ml and place it in a 100ml measuring flask, dilute to the scale with the mobile phase, shake, and serve as a control solution. The control solution (1 ml) was accurately weighed, placed in a 20ml measuring flask, diluted to the scale with mobile phase, and shaken to obtain a sensitivity solution. According to the method for the determination of related substances of dextromethorphan hydrobromide, if there are impurity peaks shown in the table below in the chromatogram of the test solution, except for the peaks of excipients before the relative retention time of 0.2, impurities I, II, the Peak area of IV and impurity III (correction factor is 0.2) multiplied by the correction factor shall not be greater than the main peak area of the control solution (1.0%), and the peak area (or corrected peak area) no more than 1 impurity peak shall be found between 0.5 and 1.0 times of the main peak area of the control solution; The area of other single impurity peak shall not be greater than that of the main peak area of the control solution (1.0%), the sum of each impurity peak area after correction shall not be greater than 2 times (2.0%) of the main peak area of the control solution. The chromatographic peaks in the chromatogram of the test solution which are smaller than the main peak area of the sensitivity solution are ignored.
The content uniformity of - shall be calculated from the content of each bag measured under the content determination item, and shall comply with the regulations (General rule 0941).
- others should comply with the relevant provisions under The granule (General Principle 0104).
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 (Agilent Zorbax SBC18,4.6mm X 250mm,5um or equivalent performance column); with buffer solution (sodium sulfosuccinate dioctyl ester 3.llg and ammonium nitrate 0.56g, add water 450ml and acetonitrile 300ml to dissolve, adjust pH to 2.0 with glacial acetic acid 220ml, dilute to 1000ml with water)-acetonitrile (72:28) as mobile phase; the detection wavelength was 280nm. An appropriate amount of dextromethorphan hydrobromide was taken, dissolved in water and diluted to prepare a solution containing about 1.5mg per 1 ml, and irradiated with a UV lamp (365nm) for 24 hours as a system-suitable solution. Take 20u1 injection human liquid chromatograph, adjust the flow rate or column temperature, so that the retention time of the main component chromatographic peak is about 16 minutes, and the separation degree of dextromethorphan peak and impurity El peak should be greater than 3.5.
- determination Method: Take 10 bags of this product, pour the contents into 50ml(15mg specification) or 25ml(7.5mg specification) measuring bottles respectively, and wash the inner wall of the packaging bag with a small amount of mobile phase, wash solution into the same measuring flask, add appropriate amount of mobile phase, sonicate to dissolve dextromethorphan hydrobromide, let it cool, dilute with mobile phase to scale, shake well, filter, and take continued filtrate as test solution, accurately inject 20u1 into liquid chromatograph and record the chromatogram. Take an appropriate amount of dextromethorphan hydrobromide reference, A solution containing about 0.3mg of dextromethorphan hydrobromide (calculated as C18H25NO. HBr. H20) per 1 ml was prepared by dissolution and quantitative dilution with the mobile phase and determined by the same method. The content of each bag is calculated by the peak area according to the external standard method, and the average content of 10 bags is obtained.
category
Same as dextromethorphan hydrobromide.
specification
(1)7.5mg (2)15mg
storage
light shielding, sealed storage.
Last Update:2022-01-01 13:42:21
125-69-9 - Dextromethorphan hydrobromide for injection
Authoritative Data Verified Data
This product is a sterile lyophilized product of dextromethorphan hydrobromide. Dextromethorphan hydrobromide (C18H25NO • HBr • H2O) shall be between 93.0% and 107.0% of the labeled amount.
trait
This product is white or off-white loose block or powder.
identification
- 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.
- identification of bromide in aqueous solution of this product (1) reaction (General rule 0301).
examination
- acidity: take an appropriate amount of this product, add water to dissolve and dilute to prepare a solution containing about 5mg of dextromethorphan hydrobromide per 1 ml, and measure it according to law (General rule 0631). The pH value should be 5.0~7.0.
- clarity and color of solution take this product, add water to dissolve and make a solution containing 5mg of dextromethorphan hydrobromide per 1 ml, the solution should be clear and colorless; If it is turbid, compared with No. 1 turbidity standard liquid (General rule 0902 first method), it should not be more concentrated; If the color is colored, it should not be deeper compared with yellow yellow green No. 1 Standard Colorimetric liquid (General rule 0901 first method).
- appropriate amount of related substances should be taken, dissolved and diluted with mobile phase to make a solution containing about 1.5mg per 1ml, which should be used as a test solution; 1ml should be accurately measured and placed in a 100ml measuring flask, dilute to the scale with the mobile phase, shake, and serve as a control solution.
- 1ml of the control solution was accurately measured, placed in a 20ml measuring flask, diluted to the scale with the mobile phase, and shaken to obtain a sensitivity solution. As dextromethorphan hydrobromide related substances under the square front determination. If there are impurity peaks shown in the table below in the chromatogram of the test solution, impurities I, II, IV and impurity IE multiplied by the correction factor (correction factor is 0.2) the peak area shall not be greater than 0.5 times (0.5%) of the main peak area of the control solution, and the peak area (or corrected peak area) no more than 1 impurity peak shall be included between 0.25 and 0.5 times of the main peak area of the control solution; The area of other single impurity peak shall not be greater than 0.5 times (0.5%) of the main peak area of the control solution, the sum of each impurity peak area after correction shall not be greater than the main peak area of the control solution (1.0%). The chromatographic peaks in the chromatogram of the test solution which are smaller than the main peak area of the sensitivity solution are ignored.
The content uniformity of - shall be calculated based on the content of each bottle measured under the content determination item, and shall comply with the regulations (General rule 0941).
- the moisture content of this product shall not exceed 0832 as determined by the method for determination of moisture (General rule 2.0% first method).
- bacterial endotoxin this product, according to the law inspection (General 1143 ), each 1 mg of dextromethorphan hydrobromide containing endotoxin amount should be less than 15EU.
- sterile take this product, add 0.9% sterile sodium chloride solution to dissolve the appropriate amount, after membrane filtration method, rinse with 0.1% sterile peptone aqueous solution (each membrane is not less than 100ml), staphylococcus aureus as a positive control bacteria, according to law inspection (General 1101), should comply with the provisions.
- others should comply with the relevant provisions under injection (General 0102).
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 (Agilent Zorbax SB C18, 4.6mm X 250mm,5um or equivalent performance column); with buffer solution (sodium sulfosuccinate dioctyl ester 3.llg and ammonium nitrate 0.56g, add water 450ml and acetonitrile 300ml to dissolve, adjust pH to 1.0 with glacial acetic acid 220ml, dilute to 1000ml with water)-acetonitrile (72:28) as mobile phase; the detection wavelength was 280nm. An appropriate amount of dextromethorphan hydrobromide was taken, dissolved in water and diluted to prepare a solution containing about 1.5mg per 1 ml, and irradiated with a UV lamp (365nm) for 24 hours as a system-suitable solution. 20u1 is injected into the liquid chromatograph to adjust the flow rate or column temperature so that the retention time of the main component chromatographic peak is about 16 minutes, and the separation degree of the dextromethorphan peak and the impurity DI peak should be greater than 3.5.
- determination: Take 10 bottles of this product, add appropriate amount of water to dissolve, and transfer them to 25ml measuring flask quantitatively, dilute with water to scale, shake well, and use as test solution, 20 u1 was accurately measured and injected into the liquid chromatograph to record the chromatogram, water was added to dissolve and quantitatively diluted to make a solution containing about 0.2mg of dextromethorphan hydrobromide (based on C18H25NO. HBr. H2O) per 1 ml, determined by the same method. According to the external standard method, the content of each bottle is calculated by Peak area, and the average content of 10 bottles is obtained.
category
Same as dextromethorphan hydrobromide.
specification
5mg
storage
light shielding, closed storage.
Last Update:2022-01-01 13:42:22