Name | pipemidic acid |
Synonyms | pipram 1489rb pipemid piperamicacid pipemidic acid PIPEMIDIC ACID LABOTEST-BB LT00772244 Pipemidic Acid Anhydrous pyrido(2,3-d)pyrimidine-6-carboxylicacid,5,8-dihydro-8-ethyl-5-oxo-2-(1-piper 8-ETHYL-5,8-DIHYDRO-5-OXO-2-[1-PIPERAZINYL]PYRIDO[2,3-D]-PYRIMIDINE-6-CARBOXYLIC ACID 8-ethyl-5-oxo-2-(piperazin-1-yl)-5,8-dihydropyrido[2,3-d]pyrimidine-6-carboxylic acid |
CAS | 51940-44-4 |
EINECS | 257-530-2 |
InChI | InChI=1/C14H17N5O3/c1-2-18-8-10(13(21)22)11(20)9-7-16-14(17-12(9)18)19-5-3-15-4-6-19/h7-8,15H,2-6H2,1H3,(H,21,22) |
Molecular Formula | C14H17N5O3 |
Molar Mass | 303.32 |
Density | 1.1931 (rough estimate) |
Melting Point | 251-255℃ |
Boling Point | 717℃ |
Flash Point | >110°(230°F) |
Water Solubility | Soluble in 1N sodium hydroxide or in DMSO. Insoluble in water |
Solubility | Soluble in glacial acetic acid, insoluble in methanol, acetone, DMF, extremely insoluble in water, ethanol, chloroform, insoluble in benzene, soluble in dilute alkali or acid solution. |
Vapor Presure | 2.86E-12mmHg at 25°C |
Appearance | Light yellow crystalline powder |
pKa | 4.14±0.20(Predicted) |
Storage Condition | Amber Vial, -20°C Freezer, Under inert atmosphere |
Sensitive | Light Sensitive |
Refractive Index | 1.7000 (estimate) |
MDL | MFCD00057291 |
Physical and Chemical Properties | Light yellow crystalline powder. Melting point 251-255 °c (decomposition). Soluble in acetic acid, difficult to dissolve in methanol, acetone, DMF, very difficult to dissolve in water, ethanol, chloroform, insoluble in benzene, soluble in dilute alkali or acid solution. Odorless and bitter. |
Use | Antibacterial Drugs, Pseudomonas aeruginosa, Escherichia coli, shigella and other Gram-negative bacilli have strong antibacterial effect, for the treatment of acute urinary tract infection and other diseases |
Hazard Symbols | Xi - Irritant |
Risk Codes | 42/43 - May cause sensitization by inhalation and skin contact. |
Safety Description | S22 - Do not breathe dust. S36/37 - Wear suitable protective clothing and gloves. S45 - In case of accident or if you feel unwell, seek medical advice immediately (show the label whenever possible.) |
WGK Germany | 2 |
RTECS | UV1153800 |
HS Code | 29335990 |
Toxicity | LD50 in mice (mg/kg): 4000 orally; 1000 i.p., 50 i.v. (Ficicchia) |
This product is 8-ethyl-5-oxo-5, 8-dihydro-2-(l-piperazinyl) pyrido [2,3-d pyrimidine-6-carboxylic acid trihydrate. The content of C14H17N503 shall not be less than 98.5% calculated as anhydrous.
take 0.5g of this product, Add 10ml of sodium hydroxide solution to dissolve, the solution should be clarified (General rule 0902).
take an appropriate amount of this product, add the mobile phase to dissolve and quantitatively dilute to make a solution containing about 0.3mg per lml as a test solution; Take an appropriate amount for precision measurement, quantitative dilution with mobile phase to prepare a solution containing 0.6ug per lml as a control solution; Precise measurement of appropriate amount of control solution, quantitative dilution with mobile phase to prepare a solution containing 0.06ug per lml, as a sensitivity solution. Silica gel was bonded with decanesulfonic acid sodium solution (0512g of citric acid and 5.7g of decanesulfonic acid were dissolved in water and diluted to 1.7 ml).-Acetonitrile-methanol (60:20:20) as mobile phase; The detection wavelength was 275mn. The appropriate amount of pipemidic acid was taken, dissolved and diluted with mobile phase to prepare a solution containing about 0.3mg per 1 ml, which was placed in an open glass container and irradiated at 5cm for 3 hours (30W) under ultraviolet light. Or 6 hours (15W), the mixed solution of pipemidic acid and its degradation impurities (wherein the amount of impurities at the retention time of 0.8 and 1.2 relative to the main peak is not less than 0.2% ), and 20u1 is injected into the liquid chromatograph, the chromatogram showed that the retention time of pipemidic acid was about 18 minutes, and the separation degrees between the peaks of pipemidic acid and impurities at relative retention times 0.8 and 1.2 should be greater than 4.5 and 3.5, respectively. Take the sensitivity solution 20 u1, inject the human liquid chromatograph, record the chromatogram, the signal-to-noise ratio of the peak of the main component should be greater than 10; Then take 20ul of the test solution and the control solution, they were injected into the 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 peak area of a single impurity shall not be greater than the main peak area of the control solution (0.2% ) ; the sum of each impurity peak area shall not be greater than 5 times (1.0%) of the main peak area of the control solution. The peaks in the chromatogram of the test solution which were 0.25 times smaller than the main peak area of the control solution were ignored.
take this product, dry to constant weight at 105°C, weight loss should be 15.0% ~ 16.0% (General 0831).
take l.Og of this product, put it in a platinum crucible, and check it according to law (General rule 0841). The residue left shall not exceed 0.2%.
take this product l. (G) place it in the Baijin crucible, slowly cauterize until it is completely carbonized, cool it, add 0.5~1.0 sulfuric acid to wet it, heat it at low temperature until the sulfuric acid is removed, then add 0.5 nitric acid, it is evaporated to dryness until the nitrogen oxide vapor is removed, then it is allowed to cool, and it is completely charred by ignition at 500-600 ° C. It shall be checked according to law (General Principles 0821 second law), and the content of heavy metals shall not exceed 20 parts per million.
take this product about 0.2g, precision weighing, add glacial acetic acid dissolved in 20ml, add crystal violet indicator solution 1 drop, with perchloric acid titration solution (0.1 mol/L) titration to a clear blue color of the solution, and the results of the titration were corrected with a blank test. Each 1 ml of perchloric acid titration solution (0.1 mol/L) corresponds to 30.33mg of C14H17N503.
quinolones.
sealed storage.
This product contains pipemidic acid (C14H17N503 • 3H20) should be labeled the amount of 95.0% to 105.0%.
This product is a light yellow tablet or film-coated tablet, which shows a light yellow color after removing the coating.
Take 10 tablets of this product, precision weighing, fine grinding, precision weighing an appropriate amount (equivalent to C14H17N503 • 3H20 0.2g), put it in a 500ml measuring flask, add 0. The appropriate amount of Olmol/L hydrochloric acid solution was dissolved and diluted to the scale by ultrasound. The solution was shaken and filtered, and 2ml of the continuous filtrate was accurately measured, and then placed in a 250ml measuring flask. Olmol/L hydrochloric acid solution was diluted to the scale, then shaken, and the absorbance was measured at the wavelength of 275nm by UV-Vis spectrophotometry (General rule 0401), plus O.Olmol/L hydrochloric acid solution was dissolved and quantitatively diluted to prepare a solution containing about C14H17N503 • 3H203ug per 1 ml, which was determined by the same method. The content of C14H17N503. 3H20 in the test article was calculated.
with pipemidic acid.
Based on C14H17N503 • 3H20 (1)0.25g(2)0.5g
sealed storage.
This product contains pipemidic acid (C14H17N503 • 3H20) should be labeled the amount of 95.0% to 105.0%.
(1) take an appropriate amount of the contents of this product, add the mobile phase to dissolve and dilute to make about 0.1 mg of the solution was filtered, and the filtrate was taken as a test solution, and the same results were shown according to the identification (1) Test under the item of pipemidic acid.
(2) take an appropriate amount of the contents of this product, add 0.Olmol/L hydrochloric acid solution was dissolved and diluted to prepare a solution containing about 3% of pipemidic acid per 1 ml, filtered, and the filtrate was taken off, according to the identification (2) test under pipemidic acid, the same results are shown.
take the contents under the item of difference in loading amount, mix them evenly, weigh an appropriate amount (approximately equivalent to 0.2g of C14H17N503 • 3H20) precisely, and place it in a 500ml measuring flask, add an appropriate amount of 0.01mol/L hydrochloric acid solution to dissolve pipemidic acid and use O. Dilute Olmol/L hydrochloric acid solution to the scale, shake well, filter, take 2ml of continuous filtrate accurately, put it in a 250ml measuring flask, use 0.Olmol/L hydrochloric acid solution was diluted to the scale, then shaken, and the absorbance was measured at the wavelength of 275nm by UV-Vis spectrophotometry (General rule 0401), A solution containing about C14H17N503 • 3H203ug per 1 ml was prepared by dissolving and quantitatively diluting with a 0.01mol/L hydrochloric acid solution, and measured by the same method to calculate the content of C14H17N503 • 3H20 in the test product.
with pipemidic acid.
0.25g (C14H17N503 • 3H20)
sealed storage.