Name | nimesulide |
Synonyms | Nide Nidol nimed nimesulide 4-Nitro-2-phenoxymethanesulfonamide 4-NITRO-2-PHENOXYMETHANE SULPHONANILIDE CETIRIZINE DIHYDROCHLORIDE MM(CRM STANDARD) CETIRIZINE DIHYDROCHLORIDE EPC(CRM STANDARD) N-(4-nitro-2-phenoxyphenyl)-methanesulfonamide |
CAS | 51803-78-2 |
EINECS | 257-431-4 |
InChI | InChI=1/C13H12N2O5S/c1-21(18,19)14-12-8-7-10(15(16)17)9-13(12)20-11-5-3-2-4-6-11/h2-9,14H,1H3 |
InChIKey | HYWYRSMBCFDLJT-UHFFFAOYSA-N |
Molecular Formula | C13H12N2O5S |
Molar Mass | 308.31 |
Density | 1.451±0.06 g/cm3(Predicted) |
Melting Point | 140-146°C |
Boling Point | 442.0±55.0 °C(Predicted) |
Water Solubility | Soluble in water (<50 µg/ml), 1:10 DMSO:PBS (pH 7.2) (<200 µg/ml), ethanol (1 mg/ml), DMSO (15 mg/ml), DMF (15 mg/ml), chloroform, dichloromethane, acetone (freely soluble), and 1N NaOH. |
Solubility | Practically insoluble in water, freely soluble in acetone, slightly soluble in anhydrous ethanol. |
Appearance | neat |
Color | Light orange to Yellow to Green |
Maximum wavelength(λmax) | ['391nm(H2O)(lit.)'] |
Merck | 14,6548 |
pKa | pKa 6.56± 0.03(H2O,t =25,I=0.02)(Approximate) |
Storage Condition | 2-8°C |
Stability | Stable. Incompatible with strong oxidizing agents. |
Physical and Chemical Properties | From ethanol to light brown crystals, melting point 143~144.5 deg C. Acute toxicity LD50 rats (mg/kg):324 oral. |
Use | Used as an antipyretic analgesic |
Risk Codes | R22 - Harmful if swallowed R36/37/38 - Irritating to eyes, respiratory system and skin. |
Safety Description | S36 - Wear suitable protective clothing. S26 - In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. |
UN IDs | UN 2811 6.1/PG 3 |
WGK Germany | 3 |
RTECS | PB0970000 |
Hazard Class | 6.1 |
Packing Group | III |
Toxicity | LD50 orally in rats: 324 mg/kg (Swingle, Moore) |
Raw Materials | Dichloromethane Ethyl Alcohol |
light brown crystals from ethanol, odorless and tasteless. The melting point was 143-144.5 °c. Soluble in chloroform, dichloromethane or sodium hydroxide solution.
brominated benzene is nitrated to produce O-nitrobrominated benzene, and nucleophilic substitution reaction is carried out with phenol sodium to produce diphenyl ether derivative, which is reduced to amino group by Raney nickel catalytic hydrogenation, the sulfonylation is carried out in the presence of methanesulfonyl chloride and an organic base, and Nimesulide is obtained by nitration.
This product is 4 '-nitro-2'-phenoxybenzenesulfonamide. Calculated as dried product, containing no less than 99.0% of C13H12N205S.
The melting point of this product (General 0612) is 148~151 ℃.
take this product, precision weighing, add 0.05mol/L sodium hydroxide solution to dissolve and quantitatively dilute to a solution containing about 12ug per 1 ml, the absorbance was measured at a wavelength of 393mn by ultraviolet-visible spectrophotometry (General rule 0401), and the absorption coefficient was 445 to 475.
developed by LPB pharmaceutical company in Italy, synthesized by LPB and enriker. It was first launched in Italy in January 1986. Non-steroidal anti-inflammatory drugs, for rheumatoid arthritis, osteoarthritis, respiratory diseases, ear nose and throat diseases, soft tissue and oral inflammation.
rat oral LD50:324mg/kg.
take this product l.Og, add water 50ml, fully shake, according to the law (General 0631),pH value should be 5.0~7.0.
take this product l. 0g, dissolved with acetone and diluted to 10ml, according to UV-visible spectrophotometry (General 0401), measured at the wavelength of 450nm, absorbance should not exceed 0.50.
take 0.5g of this product, add 0.05mol/L sodium hydroxide solution, fully shake to dissolve, Dropwise add nitric acid to make the solution from yellow to colorless, filter, the filtrate shall be taken at 20. 0ml and checked according to law (General rule 0801). Compared with the control solution made of 0.07% of standard sodium chloride solution, the solution shall not be more concentrated ().
take about 25mg of this product, put it in a 25ml measuring flask, add an appropriate amount of mobile phase, ultrasonic for 15 minutes to dissolve, let it cool, dilute it to the scale with mobile phase, shake well, and use it as a test solution; an appropriate amount was taken in a precise amount, and a solution per 1 ml was prepared by dilution with the mobile phase. As a control solution, the test was performed according to high performance liquid chromatography (General 0512). Silica gel was bonded with eighteen alkyl silane as filler; 0.1% phosphoric acid solution (adjusted to pH 7.0 with ammonia)-acetonitrile (60:40) as mobile phase; The detection wavelength was 230nm. A mixed solution containing about 20ug of p-chloroaniline and 50ug of nimesulide per 1 ml was prepared by dissolving and diluting p-phenylamine and Nimesulide with mobile phase as the applicable solution for the system. 20ul was injected into the liquid chromatograph and the chromatogram was recorded, the theoretical plate number is not less than 3000 calculated by Nimesulide peak, and the separation degree between p-chloroaniline peak and Nimesulide peak should be greater than 2.0. The 20ul of the control solution and the test solution were respectively injected into the human liquid chromatograph, and the chromatogram was recorded to 7 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 the area of the main peak of the control solution (0.1% ) , and the sum of each impurity peak area shall not be greater than 5 times the area of the main peak of the control solution (0.5%).
take this product, dry to constant weight at 105°C, weight loss shall not exceed 0.5% (General rule 0831).
take l.Og of this product and check it according to law (General rule 0841). The residue left shall not exceed 0.1%.
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).
take this product l. Put it in the crucible, slowly cauterize until complete charring, cool it, add 1ml sulfuric acid to wet it, heat it at low temperature until the sulfuric acid vapor is removed, burn it at 700°C until complete Ash, cool it, add 1ml hydrochloric acid, dry on a water bath, then dilute 1ml hydrochloric acid and water, heat on a water bath (filter if necessary), wash the Crucible with water, combine the filtrate and wash to 25ml, inspection according to law (General rule 0807), if the color, and the standard iron solution 0.001% ml with the same method of preparation of the control solution, not deeper ().
take about 0.25g of this product, weigh precisely, add 40ml of neutral acetone (neutral to phenolphthalein indicator solution) to dissolve, add 20ml of water, and use potentiometric titration (General rule 0701), with sodium hydroxide titration solution (0.1 mol/L) titration, and the results of the titration were corrected with a blank test. Each 1 ml of sodium hydroxide titration solution (0.1 mol/L) corresponds to 30.83mg of C13H12N2O5S.
antipyretic analgesic, non-steroidal anti-inflammatory drugs.
light shielding, sealed storage.
This product contains Nimesulide (C13H12N2O5S) should be 95.0% to 105.0% of the label.
This product is a yellowish or film-coated tablet, which is yellowish after removing the coating.
take an appropriate amount (about 50mg of nimesulide) of the fine powder (film-coated tablets are removed from the coating), add anhydrous ethanol 20ml, shake, dissolve nimesulide, filter, the filtrate was dried by evaporation on a water bath and then dried under reduced pressure. The residue was tested according to the identification items (1) and (2) of nimesulide and showed the same results.
Take 20 tablets of this product (film-coated tablets to remove the coating), precise weighing, fine grinding, precise weighing to take an appropriate amount of fine powder (about 20mg equivalent to Nimesulide), put it in a measuring flask of 100ml, add 50ml of 0.05mol/L sodium hydroxide solution, fully shake to dissolve nimesulide, dilute with 0.05mol/L sodium hydroxide solution to the scale, shake well, filter, and take 5ml of continued filtrate with precision, in a 0.05 measuring flask, dilute to the scale with 0401 mol/L sodium hydroxide solution, shake well, measure absorbance at the wavelength of 393mn by UV-visible spectrophotometry (general rule); another Nimesulide reference substance was dissolved and diluted with 0.05mol/L sodium hydroxide solution to prepare a solution containing about 10ug per 1 ml, which was determined by the same method.
Same as nimesulide.
specification
(l ) 50mg ( 2) 100mg
sealed and stored in a dry place.