Name | CEFACLOR HYDRATE |
Synonyms | CEFACLOR HYDRATE Cefaclor monohydrate 3-chloro-7-D-(2-phenylglycinamido)-3-cephem-4-carboxylic acid monohydrate (6R,7R)-7-{[amino(phenyl)acetyl]amino}-3-chloro-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid hydrate |
CAS | 70356-03-5 |
InChI | InChI=1/C15H14ClN3O4S.H2O/c16-8-6-24-14-10(13(21)19(14)11(8)15(22)23)18-12(20)9(17)7-4-2-1-3-5-7;/h1-5,9-10,14H,6,17H2,(H,18,20)(H,22,23);1H2 |
Molecular Formula | C15H16ClN3O5S |
Molar Mass | 385.82 |
Melting Point | >180°C (dec.) |
Boling Point | 778.4°C at 760 mmHg |
Flash Point | 424.6°C |
Solubility | Soluble in water, almost insoluble in methanol, chloroform or benzene. |
Vapor Presure | 1.65E-25mmHg at 25°C |
Appearance | White or white-like crystalline powder |
Storage Condition | 2-8℃ |
MDL | MFCD00071999 |
Use | Cephalosporins, mainly used for urinary tract infections and respiratory tract infections |
white or off-white crystalline powder. Soluble in water, almost insoluble in methanol, chloroform or benzene. Stable at pH = 2.5-4.5. UV absorption maximum (pH = 7 buffer):265nm(& epsilon;6800).
calculated as anhydrous, containing C15H14CIN304S shall not be less than 95%; PH value, pH value should be 3O ~ 4.5 (containing 25mg of the product suspension per mL), the related substances should comply with the provisions; water content should be 3.0% ~ 6.5%; Containing heavy metals shall not exceed 0.003%.
This product is (6R,7R)-7-[(K) 2-amino-2-phenylacetylamino]-3-chloro-8-oxo-5-thia-1-azabicyclo [4.2.0] oct-2-ene-2-Formic acid monohydrate, calculated as anhydrous, containing cefaclor (C15H14C1N304S) shall not be less than 95.0%.
take this product, precision weighing, water dissolution and quantitative dilution of about 4mg per lml solution, according to the law (General 0621), specific rotation of 105 ° to 120 °.
take this product, precision weighing, add water to dissolve and quantitatively dilute to make a solution containing about 20ug per lml, according to UV-visible spectrophotometry (General 0401 ), the absorbance was measured at a wavelength of 264mn, and the absorption coefficient was 230 to 255.
with penicillin as raw material. The carboxyl groups on penicillin are first protected with P-nitrobenzyl and then oxidized to sulfoxide with hydrogen peroxide or peracetic acid. Chlorination and ring expansion are carried out under the action of N-chlorosuccinimide or N-chlorophosphorylphthalamide, etc. After ozonation, the 3-position is reduced to form a hydroxyl group. The 3-position is then converted to chloro under phosphorus trichloride, followed by the action of phosphorus pentachloride and pyridine, followed by alcoholysis of the 7-position to form the hydrochloride salt of the free amino group. This was dissolved in a solution of tetrahydrofuran and methanol, a solution of palladium on carbon in ethanol was added, the reaction was followed by filtration, the filter cake was washed with tetrahydrofuran and water, and the solvent was evaporated to dryness. The resulting material was dissolved in a mixture of water and ethyl acetate, and the pH was adjusted to 3. A solid was precipitated, filtered, soaked with acetone, and then dried to give 7-amino-3-chloro-3-cefene-4-carboxylic acid. This was dissolved in acetonitrile, and N,O-bis (trimethylsilyl) acetamide was added with stirring at room temperature to form a soluble bis-silyl ester. Cooled to 0 ° C., in the presence of two drops of N,N-dimethylbenzylamine, the sodium salt of methyl 3-(l-carboxybenzylamine) crotonate and methyl chloroformate were slowly added to the reaction solution in acetonitrile. Stirring was continued, methanol was added and insoluble materials were removed by filtration. Water was added and the pH was adjusted to 1.5, followed by triethylamine to 4.5. Stir the th again in a water bath, The precipitated crystalline precipitate was filtered, washed with acetonitrile and dried under vacuum to give cefaclor.
First generation cephalosporin antibiotics, antibacterial properties and cefazolin approximation. The product is a broad-spectrum semi-synthetic cephalosporin antibiotics. The activity of Group A hemolytic Streptococcus, Streptococcus viridans and Staphylococcus epidermidis was the same as that of cefadroxil, and the antibacterial effect on Pneumonia coccus was 2~4 times stronger than that of cefadroxil. Clinically, it is mainly used for urinary tract infection, respiratory tract infection, skin and soft tissue infection, ENT infection and so on.
take this product, add water to make a suspension containing about 25mg per lml, according to the law (General 0631),pH value should be 3.0~4.5.
take about 50mg of this product, put it in a 10ml measuring flask, add 0.27% sodium dihydrogen phosphate solution (pH 2.5) to dissolve and dilute to the scale, shake well, as a test solution; take 1ml accurately, put it in a 0.27% measuring flask, dilute it to the scale with 2.5 sodium dihydrogen phosphate solution (pH), and shake it well to serve as a control solution. 0512 sodium dihydrogen phosphate solution (0.78% g) was added with water to dissolve and diluted to 7.8 ML, as determined by high performance liquid chromatography (general rule), adjust pH to 4.0 with phosphoric acid), mobile phase B was 0.78% sodium dihydrogen phosphate solution (pH 4.0)-acetonitrile (55:45); Linear gradient elution was carried out according to the following table; Detection wavelength was 220mn. Cefaclor control and cefaclor 5-3-isomer control, respectively, were added 0.27% sodium dihydrogen phosphate solution (pH 2.5) dissolved and diluted to prepare mixed solutions containing about 25ug and 50ug per 1 ml, respectively, take 20ul injection human liquid chromatograph and record the chromatogram, the retention time of cefaclor peak is about 23 minutes, the separation degree between cefaclor peak and cefaclor 3-isomer peak should not be less than 2.0, the tailing factor of cefaclor peak should be less than 1.2. 20ul of the test solution and the control solution were respectively injected into the liquid chromatograph, and the chromatograms were recorded. If there are impurity peaks in the chromatogram of the test solution, the area of a single impurity peak shall not be greater than 0.5 times (0.5%) of the area of the main peak of the control solution, the Peak area of each impurity shall not be greater than 2 times (2.0%) of the main peak area of the control solution, and the peak smaller than 0.1 times of the main peak area of the control solution in the chromatogram of the test solution shall be ignored.
weigh about 0.2g of this product accurately, place it in the top empty bottle, add internal standard solution (containing 20ug of N-propanol in 0.2mol/L sodium hydroxide solution per 1 ml) to dissolve, Seal, as a test solution. The appropriate amount of dichloromethane was accurately weighed and diluted quantitatively with internal standard solution to make a solution containing about 20ug of dimethane per lml, and then 5ml was accurately weighed and placed in a headspace bottle as a reference solution, according to the determination method of residual solvent (General Principle 0861 second method), the capillary column with polyethylene glycol (PEG-20M)(or similar polarity) as stationary liquid is used as the column, and the column temperature is 60°C, the inlet temperature was 120°C; The detector temperature was 150°C; The headspace bottle equilibrium temperature was 80°C, and the equilibrium time was 20 minutes, the resolution between the dichloromethane peak and the N-propanol peak should be greater than 2.0. Take the reference solution and the test solution into the headspace respectively, record the chromatogram, and calculate the ratio of peak area according to the internal standard method. The residual amount of dichloromethane should comply with the regulations.
take this product, according to the moisture determination method (General 0832 first method 1), the moisture content should be 3.0% ~ 6.5%.
take this product 1.Og, determination according to law (General Principles 0821 second method), containing heavy metals shall not exceed 30 parts per million.
measured by high performance liquid chromatography (General 0512).
silica gel bonded with eighteen alkyl silane as filler; Potassium dihydrogen phosphate solution (take potassium dihydrogen phosphate 6.8g, dissolve and dilute to 3.4 with water, adjust pH to with phosphoric acid)-acetonitrile (92:8) as mobile phase; The detection wavelength was 254nm. Appropriate amounts of cefaclor reference and cefaclor -3-isomer reference were dissolved and diluted with mobile phase to prepare mixed solutions containing about 0.2mg each in 1 ml, and 20 ml was injected into human liquid chromatograph, and the chromatogram was recorded, the resolution between cefaclor peak and cefaclor 5-3-isomer peak should meet the requirements.
take about 20mg of this product, weigh it accurately, put it in a 100ml measuring flask, add the mobile phase to dissolve and dilute to the scale, shake it well, and use it as a test solution, A 20ul injection liquid chromatograph was used for precise measurement, and the chromatogram was recorded. According to the external standard method to calculate the peak area, that is.
B-lactam antibiotics, cephalosporins
light shielding, sealed storage.
This product contains cefaclor (C15H14C1N304S) should be 90.0% to 110.0% of the label amount.
This product is fine particles or powder; Aromatic.
take an appropriate amount of this product, add water to dissolve and dilute to prepare a solution containing about 2mg of cefaclor (based on C15H14C1N304S) per 1 ml, filter, and take the continued filtrate as the test solution, the same results should be shown in the identification tests (1) or (2) for cefaclor.
The contents under the item of difference in loading amount shall be collected, mixed evenly, and the appropriate amount shall be accurately weighed (approximately equivalent to cefaclor, 0.1g based on C15H14C1N304S), add mobile phase to dissolve and quantitatively dilute to prepare a solution containing about 0.2mg of cefaclor (based on C15H14C1N304S) per 1 mL (sonication is necessary), shake well, filter, the filtrate was taken as the test solution, and determined according to the method under the item of cefaclor.
Same as cefaclor.
Based on C15H14C1N304S (l)0.125g (2)0.25g(3)0.375g (4)0.75g (5)1.5g
It was shielded from light, sealed, and stored in a cool-dark dry place.
This product contains cefaclor (C15H14C1N304S) should be 90.0% to 110.0% of the label amount.
This product is a film-coated tablet, white to yellowish after removing the coating.
take an appropriate amount of the fine powder of this product, add water to dissolve and make a solution containing about 2mg of cefaclor (based on C15H14C1N304S) per 1 ml, filter, and take the continued filtrate as the test solution, the same results should be shown in the identification tests (1) or (2) for cefaclor.
Take 10 tablets of this product, precision weighing, fine grinding, precision weighing to take appropriate amount (about equivalent to cefaclor, according to C15H14C1N304S 0.25g), add mobile phase to dissolve and quantitatively dilute to prepare a solution containing about 0.2mg of cefaclor (based on C15H14C1N304S) per 1 mL (sonication is necessary), shake well, filter, the filtrate was taken as the test solution, and determined according to the method under the item of cefaclor.
Same as cefaclor.
0.25g (based on C15H14C1N304S)
It was shielded from light, sealed, and stored in a cool, dark and dry place.
This product contains cefaclor (C15H14C1N304S) should be 90.0% to 110.0% of the label amount.
The content of this product is white to yellowish powder.
take an appropriate amount of the contents of this product, add water to dissolve and dilute to prepare a solution containing about 2mg of cefaclor (C15H14C1N304S) per 1 ml, filter, and take the filtrate as the test solution, the same results should be shown in the identification tests (1) or (2) for cefaclor.
take the contents under the item of difference in loading amount, mix evenly, and accurately weigh an appropriate amount (about equivalent to cefaclor, 0.254 based on C15H14C1N304S), add mobile phase to dissolve and quantitatively dilute to prepare a solution containing about 0.2mg of cefaclor (based on C15H14C1N304S) per 1 mL (sonication is necessary), shake well, filter, the filtrate was taken as the test solution, and determined according to the method under the item of cefaclor.
Same as cefaclor.
Based on C15H14C1N304S (1)0.25g (2)0.5g
It was shielded from light, sealed, and stored in a cool-dark dry place.
This product contains cefaclor (C15H14C1N304S) should be 90.0% to 110.0% of the label amount.
This product is soluble particles or suspended particles; Gas fragrance.
take an appropriate amount of this product, add water to dissolve and dilute to prepare a solution containing about 2mg of cefaclor (based on C15H14C1N304S) per 1 ml, filter, and take the continued filtrate as the test solution, the same results should be shown in the identification tests (1) or (2) for cefaclor.
The contents under the item of difference in loading amount shall be collected, mixed evenly, and the appropriate amount shall be accurately weighed (approximately equivalent to cefaclor, 0.1g based on C15H14C1N304S), add mobile phase to dissolve and quantitatively dilute to prepare a solution containing about 0.2mg of cefaclor (based on C15H14C1N304S) per 1 mL (sonication is necessary), shake well, filter, the filtrate was taken as the test solution, and determined according to the method under the item of cefaclor.
Same as cefaclor.
calculated as C15H14C1N304S (1)0.lg (2)0.125g(3)0.25g (4)0.5g
It was shielded from light, sealed, and stored in a cool-dark dry place.