Azelastine Impurity
azelastine hydrochloride
CAS: 153408-27-6;153408-28-7;79307-93-0
Molecular Formula: C22H24ClN3O·HCl
Azelastine Impurity - Names and Identifiers
| Name | azelastine hydrochloride |
| Synonyms | (S)-Azelastine HCl Azelastine Impurity Azelastine Impurity 2 azelastine hydrochloride (S)-Azelastine Hydrochloride (S)-Azelastine Hydrochloride 2 (S)-4-[(4-Chlorophenyl)Methyl]-2-(hexahydro-1-Methyl-1H-azepin-4-yl)-1(2H)-phthalazinone Hydrochloride 1(2H)-Phthalazinone, 4-[(4-chlorophenyl)methyl]-2-(hexahydro-1-methyl-1H-azepin-4-yl)-, monohydrochloride, (S)- |
| CAS | 153408-27-6 153408-28-7 79307-93-0 |
| EINECS | 253-720-4 |
| InChI | InChI=1/C22H24ClN3O.ClH/c1-25-13-4-5-18(12-14-25)26-22(27)20-7-3-2-6-19(20)21(24-26)15-16-8-10-17(23)11-9-16;/h2-3,6-11,18H,4-5,12-15H2,1H3;1H/t18-;/m1./s1 |
Azelastine Impurity - Physico-chemical Properties
| Molecular Formula | C22H24ClN3O·HCl |
| Melting Point | 219-221?C |
| Solubility | Soluble in water (25 mg/mL), DMSO (>10 mg/mL), and ethanol. |
| Appearance | Solid |
| Color | White |
| Storage Condition | -20°C Freezer |
| Sensitive | Sensitive to heat |
| Physical and Chemical Properties | For Azelastine Hydrochloride Nasal Spray, ie, acerbine (AZEP): This product is colorless or almost colorless clear liquid |
| Use | [Drug Name] Common name: Azelastine Hydrochloride Nasal Spray Chinese pinyin: Yansuandanzhuositing bifenwuji [ingredients] Azelastine hydrochloride. [Properties] This product is a colorless transparent liquid, high pressure valve, medicine is sprayed in a mist. [indications] seasonal allergic rhinitis (hay fever) and perennial allergic rhinitis [dosage] 1 spray/nostril, morning and evening, twice daily (equivalent to a 0, 56mg Azelastine hydrochloride dose per day) or as described. When spraying, keep the head upright before the symptoms disappear should adhere to the use of acerbine nasal spray, but continuous use is not more than 6 months. [adverse reactions] a small number of patients spray will produce nasal mucosa irritation, individual patients appear epistaxis. If the method of administration is incorrect, there will be bitter taste. [medication for pregnant and lactating women] Although the drug test in large doses in animals did not produce a malformed response to the drug, however, the drug is not recommended for women in the first 3 months of pregnancy. The use of this product is strictly prohibited for lactating mothers. [children's medication] children over 6 years old with adult dosage [drug interaction] found no interaction with other drugs. [overdose] animal tests have shown that excessive oral doses can cause symptoms of the central nervous system, once this situation occurs, it should be symptomatic treatment or supportive therapy, no specific antidote. [Pharmacology and Toxicology] Azelastine hydrochloride is a new structure of 2, 3 diazepinone derivatives, as a potential long-acting anti-allergic compounds, with H1 receptor antagonist characteristics. Animal experimental data show that high concentrations of Azelastine hydrochloride can prevent the synthesis and release of certain chemical mediators (eg, leukotrienes, histamine, serotonin) in allergic reactions. And can prevent the migration of I-CAMI of the upregulated and eosinophilic cells to exert a wide range of anti-inflammatory effects. No local or organ-specific toxic reactions were detected at the maximum dose permitted for nasal spray administration. [pharmacokinetics] repeated daily nasal spray of 0, 56mg Azelastine hydrochloride (equivalent to 1 spray/nostril, 2 times/day), the steady-state plasma concentration of Azelastine hydrochloride Cmax in healthy volunteers was 0, 27ng/ml, its active metabolite, N-Desmethyl azelastine, can be detected at or below the limit of quantification (0, 12ng/ml). [storage] sealed and kept in a cool place. [validity period] tentative 18 months |
Azelastine Impurity - Azelastine hydrochloride
Authoritative Data Verified Data
(±) 4-(4-chlorobenzyl)-2-(hexahydro-1-methyl -1 H-azepin-4-yl)-l(2ff)-2, 3-naphthyridinone hydrochloride. Calculated as dry product, containing not less than 99.0% of C22H24C1N30 • HCl.
Last Update：2024-01-02 23:10:35
Azelastine Impurity - Trait
Authoritative Data Verified Data
- This product is white or off-white powder or crystalline powder; Odorless.
- This product is slightly soluble in methanol, slightly soluble in water or ethanol, and soluble in glacial acetic acid.
Last Update：2022-01-01 15:34:29
Azelastine Impurity - Introduction
Azelastine HCl is an effective, second-generation selective histamine antagonist.
Last Update：2022-10-16 17:14:08
Azelastine Impurity - Differential diagnosis
Authoritative Data Verified Data
- take this product, add water to dissolve and dilute to make a solution containing about 30ug per 1ml, and measure by UV-Vis spectrophotometry (General rule 0401), there is a maximum absorption at a wavelength of 286nm and a minimum absorption at a wavelength of 264nm.
- The infrared absorption spectrum of this product should be consistent with that of the reference product (General rule 0402).
- the aqueous solution of this product was chloride identification (1) of the reaction (General 0301).
Last Update：2022-01-01 15:34:30
Azelastine Impurity - Exam
Authoritative Data Verified Data
optical rotation
take this product, precision weighing, add water to dissolve and quantitatively dilute to make a solution containing about 5mg per lml (if necessary, it can be dissolved by ultrasound), and determine according to law (General 0621), the optical rotation is from 0.01 ° to +0.01 °.
acidity
take this product 50mg, add water 30ml to dissolve (if necessary, can be ultrasonic dissolution), according to the law (General 0631),pH value should be 5.0~7.0.
Related substances
take an appropriate amount of this product, add the mobile phase to dissolve and dilute to make a solution containing about 1 mg per 1ml as a test solution; Take 1ml for precision measurement and put it in a 200ml measuring flask, dilute to the scale with the mobile phase, shake, and serve as a control solution. Silica gel bonded with eighteen alkyl silane was used as a filler as determined by high performance liquid chromatography (General 0512); 4% triethylamine solution (adjusted to pH 6.0 with phosphoric acid)-acetonitrile-methanol (50:18:32) as mobile phase, the detection wavelength was 289mn. The number of theoretical plates shall not be less than 3000 calculated by azelastine peak, and the degree of separation between azelastine peak and adjacent impurity peaks shall meet the requirements. 20 u1 of the test solution and the control solution were respectively injected into the human liquid chromatograph, and the chromatogram was recorded to 2 times of the retention time of the main component peak. If there are impurity peaks in the chromatogram of the test solution, the area of a single impurity peak shall not be greater than 0.4 times (0.2%) the area of the main peak of the control solution, and the sum of the areas of each impurity peak shall not be greater than the area of the main peak of the control solution (0.5%).
residual solvent
take about 0. L g of this product, precisely weigh it, place it in the top empty bottle, and precisely add 5ml internal standard solution (50% N, dimethylformamide solution with ethyl acetate concentration of about 80ug/ml) to dissolve, seal the mouth of the bottle, as the test solution; Accurately weigh the appropriate amount of methanol, ethanol, isopropanol, acetone and dichloromethane, dissolve and quantitatively dilute with internal standard solution to prepare about 60ug of methanol per lml, the mixed solution of ethanol 100ug, acetone 100ug, isopropanol 100ug and dichloromethane 12ug, 5ml in the top empty bottle, sealed, as a reference solution. Test as residual solvent assay (General 0861 second method). With 6% cyanopropylphenyl-94% dimethylpolysiloxane (or polar similar) as stationary liquid, the initial temperature is 40°C, maintain 8 minutes, at the rate of 60°C per minute heating to 160°C, maintain 2 minutes; the inlet temperature was 200°C, the FID detector temperature was 250°C; The carrier gas was nitrogen; The headspace bottle equilibrium temperature was 85°C, and the equilibrium time was 15 minutes. Take the reference solution into the headspace, the separation degree between the peaks of each component shall meet the requirements. The test solution and the reference solution are injected into the headspace respectively, and the chromatogram is recorded. The residual amount of methanol, ethanol, isopropanol, acetone and dichloromethane shall be calculated by the peak area according to the internal standard method.
loss on drying
take this product, dry to constant weight at 105°C, weight loss shall not exceed 1.0% (General rule 0831).
ignition residue
This product l.Og, inspection according to law (General rule 0841), residual flooding shall not exceed 0.1%.
Heavy metals
The residual Tong left under the item of burning residual shall be inspected according to law (General rule 0821 second law), and the heavy metal content shall not exceed 20 parts per million.
Last Update：2022-01-01 15:34:31
Azelastine Impurity - Content determination
Authoritative Data Verified Data
take this product about 0.3g, precision weighing, add anhydrous formic acid 5ml and acetic anhydride 30ml dissolved, according to the potential titration method (General rule 0701), with perchloric acid titration solution (0.1 mol/L) titration, and the results of the titration were corrected with a blank test. Each 1 ml perchloric acid titration solution (0.1 M o l/L) corresponds to 41.84mg of C22H24C1N30 • HCl.
Last Update：2022-01-01 15:34:32
Azelastine Impurity - Category
Authoritative Data Verified Data
H, receptor antagonist.
Last Update：2022-01-01 15:34:32
Azelastine Impurity - Storage
Authoritative Data Verified Data
sealed storage.
Last Update：2022-01-01 15:34:32
Azelastine Impurity - Azelastine hydrochloride tablets
Authoritative Data Verified Data
This product contains Azelastine hydrochloride (C22H24C1N30 • HCl) should be 90.0% ~ 110.0% of the label amount.
trait
This product is white or white-like tablets or film-coated tablets, white or white-like after removing the 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 appropriate amount of fine powder of this product, add water, shake, filter, filtrate chloride to identify (1) reaction (General rule 0301).
examination
- Related substances take an appropriate amount of fine powder of this product, add mobile phase to dissolve and dilute to make Azelastine hydrochloride 0. 5 m g of solution, filter, take the continued filtrate as the test solution; Take 1 m l for precise measurement, put it in a 10 0 m l measuring flask, dilute to the scale with mobile phase, as a control solution. According to the chromatographic conditions under the content determination item, 20 ^ 1 of the test solution and the control solution are accurately measured and injected into the human liquid chromatograph respectively, the chromatogram was recorded to 2 times of the retention time of the main component peak. If there are impurity peaks in the chromatogram of the test solution, the sum of each impurity peak area shall not be greater than the main peak area of the control solution (0.2) except the chromatographic peak before the relative retention time of 1.0% 5. 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 dissolution of this product, according to the dissolution and release determination method (General rule 0931 third method), with hydrochloric acid solution (2-μ 1 0 m l as dissolution medium, speed is 50 rpm, according to the law, after 30 minutes, take the appropriate amount of solution, filtration, take the filtrate as a test solution (l m g specification); or precisely take 5 m l of the continuous filtrate, put it in a 10m l volumetric flask, dilute it to the scale with dissolution medium, shake it well, and use it as a test solution (2 m g specification); in addition, an appropriate amount of Azelastine hydrochloride reference substance was accurately weighed, dissolved and quantitatively diluted with mobile phase to prepare a solution containing about 10m g per l 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 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; 4% triethylamine solution (adjusted to pH 6.0 with phosphoric acid)-acetonitrile-methanol (50:18:32) as mobile phase; The detection wavelength was 289mn. The number of theoretical plates shall not be less than 3000 calculated by azelastine peak, and the degree of separation between azelastine peak and adjacent impurity peaks shall meet the requirements.
- determination Method: Take 10 tablets of this product, put them in 25ml measuring flask (lmg specification) or 50ml measuring flask (2mg specification) respectively, add mobile phase to dissolve and dilute to the scale, shake well, filter, the continued filtrate was taken as the test solution, and 20ul was accurately measured and injected into the human Liquid Chromatograph. The chromatogram was recorded, the mobile phase was added to dissolve and quantitatively dilute to prepare a solution containing about 40ug 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 Azelastine hydrochloride.
specification
(l )lmg (2)2mg
storage
sealed and stored in a dry place.
Last Update：2022-01-01 15:34:33
Azelastine Impurity - Azelastine Hydrochloride Nasal Spray
Authoritative Data Verified Data
This product is a multi-dose, quantitative nasal spray, containing Azelastine hydrochloride (C22H24C1N30 • HC1) should be 90.0% to 110.0% of the label amount.
trait
The contents of this product is colorless transparent liquid, pressure valve, liquid is sprayed in a mist.
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 10ml of this product and add 1ml of Phosphotungstic acid test solution to generate white precipitate.
examination
- the pH value of this product is determined according to law (General rule 063 1), and the pH value should be 5.0~7.0.
- spray main drug content take 1 bottle of this product, fully shake, remove the cap, try spraying 5 times, wash the nozzle with methanol, fully dry, insert the nozzle into a 25ml measuring flask with an inverted tilt, spray 10 times or 20 times (spray every 5 seconds and slowly shake), take out the vial, wash the inside and outside of the nozzle with mobile phase, in the washing liquid and measuring flask, dilute to the scale with the mobile phase, shake well, and prepare a solution containing about 56ug of Azelastine hydrochloride per 1 ml as a test solution. The average content of Azelastine hydrochloride per spray shall be 80.0% to 120.0% of the label amount as determined by the method under the content determination item, and the result is divided by 10 or 20.
- Quality of related substances: take an appropriate amount of the contents of this product and dilute it with mobile phase to make a solution containing 0.5mg Azelastine hydrochloride per 1 ml as a test solution; Take 1 ml for precision measurement, set in a 100ml measuring flask, dilute to the scale with the mobile phase, and shake to serve as a control solution. If there are impurity peaks in the chromatogram of the test solution, except for the chromatographic peaks before the relative retention time of 0.25, the sum of each impurity peak area shall not be greater than the main peak area of the control solution (1.0%).
- others should comply with the relevant provisions under nasal preparations (General rule 0106) and sprays (General rule 0112).
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; 4% triethylamine solution (adjusted to pH 6.0 with phosphoric acid)-acetonitrile-methanol (50:18:32) as mobile phase; The detection wavelength was 289nm. The number of theoretical plates shall not be less than 3000 calculated by azelastine peak, and the degree of separation between azelastine peak and adjacent impurity peaks shall meet the requirements.
- determination precision: take an appropriate amount of the contents of this product and quantitatively dilute it with mobile phase to prepare a solution containing about 0.05mg Azelastine hydrochloride per 1 ml, as a test solution, and take 20ul of precision measurement, inject into liquid chromatograph, record chromatogram; Take appropriate amount of Azelastine hydrochloride reference substance, precisely weigh, add mobile phase to dissolve and quantitatively dilute to prepare solution containing about 0.05mg per 1 ml, and determine with the same method. According to the external standard method to calculate the peak area, that is.
category
Same as Azelastine hydrochloride.
specification
(l ) 10ml:10mg ,70 spray, 0.14mg per spray (2)10ml:10mg,140 spray, 0.07mg per spray
storage
sealed and kept in a cool place.
Last Update：2022-01-01 15:34:34
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Multiple SpecificationsSpot supply
Product Name: Azelastine Visit Supplier Webpage Request for quotationCAS: 79307-93-0
Tel: 0714-3999186
Email: 2853786052@qq.com
Mobile: 86+15671228036
QQ: 2853786052
Wechat: 15671228036
Product Name: azelastine hydrochloride Request for quotation
CAS: 79307-93-0
Tel: 0086-551-65418684
Email: sales@tnjchem.com
info@tnjchem.com
Mobile: 0086 189 4982 3763
QQ: 2881500840
Wechat: 0086 189 4982 3763
WhatsApp: 0086 189 4982 3763
Product List: View Catalog
CAS: 79307-93-0
Tel: 0086-551-65418684
Email: sales@tnjchem.com
info@tnjchem.com
Mobile: 0086 189 4982 3763
QQ: 2881500840
Wechat: 0086 189 4982 3763
WhatsApp: 0086 189 4982 3763
Product List: View Catalog
Multiple SpecificationsSpot supply
Product Name: Azelastine HCl Visit Supplier Webpage Request for quotationCAS: 79307-93-0
Tel: 18301782025
Email: 3008007409@qq.com
Mobile: 18021002903
QQ: 3008007409
Wechat: 18301782025
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