头孢卡品酯

430JP XV

Cefcapene Pivoxil Hydrochloride Hydrate /O‹cial Monographs solution and the mobile phase to make 50mL,and use these solutions as the sample solution and standard solution.Per-form the test with 10m L each of the sample solution and stan-dard solution as directed under Liquid Chromatography <2.01>according to the following conditions,and determine the ratios,Q T and Q S ,of the peak area of cefbuperazone to that of the internal standard.

Amount [m g (potency)]of cefbuperazone (C 22H 29N 9O 9S 2)＝W S ×(Q T /Q S )×1000

W S :Amount [mg (potency)]of Cefbuperazone Reference

Standard Internal standard solution —A solution of acetonitrile in the mobile phase (1in 4000).Operating conditions —

Detector:An ultraviolet absorption photometer (wave-length:254nm).

Column:A stainless steel column 4.6mm in inside di-ameter and 15cm in length,packed with octadecylsilanized silica gel for liquid chromatography (5m m in particle di-ameter).

Column temperature:A constant temperature of about 259C.

Mobile phase:Dissolve 2.0g of tetra-n -propylammonium bromide in 1000mL of a mixture of water,acetonitrile and acetic acid-sodium acetate buŠer solution,pH 5.0(83:13:4).Flow rate:Adjust the ‰ow rate so that the retention time of cefbuperazone is about 16minutes.System suitability —

System performance:When the procedure is run with 10m L of the standard solution under the above operating conditions,the internal standard and cefbuperazone are elut-ed in this order with the resolution between these peaks being not less than 3.

System repeatability:When the test is repeated 6times with 10m L of the standard solution under the above operating conditions,the relative standard deviation of the ratios of the peak area of cefbuperazone to that of the internal standard is not more than 1.0z .

Containers and storage Containers—Hermetic containers.Storage—In a cold place.

Cefcapene Pivoxil Hydrochloride Hydrate

セフカペン

ピボキシル塩酸塩水和物

C 23H 29N 5O 8S 2.HCl.H 2O:622.11

2,2-Dimethylpropanoyloxymethyl (6R ,7R )-7-[(2Z )-2-(2-aminothiazol-4-yl)pent-2-enoylamino]-3-carbamoyloxymethyl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-caboxylate monohydrochloride monohydrate [147816-24-8]

Cefcapene Pivoxil Hydrochloride Hydrate contains not less than 722m g (potency)and not more than 764m g (potency)per mg,calculated on the anhydrous ba-sis.The potency of Cefcapene Pivoxil Hydrochloride Hydrate is expressed as mass (potency)of cefcapene (C 17H 19N 5O 6S 2:453.49).

Description Cefcapene Pivoxil Hydrochloride Hydrate oc-curs as a white to pale yellowish white,crystalline powder or mass.It has slightly a characteristic odor.

It is freely soluble in N ,N -dimethylformamide and in methanol,soluble in ethanol (99.5),slightly soluble in water,and practically insoluble in diethyl ether.

Identiˆcation (1)Determine the infrared absorption spec-tra of Cefcapene Pivoxil Hydrochloride Hydrate and Cefca-pene Pivoxil Hydrochloride Reference Standard as directed in the paste method under Infrared Spectrophotometry <2.25>,and compare these spectra:both spectra exhibit simi-lar intensities of absorption at the same wave numbers.(2)Determine the spectrum of a solution of Cefcapene Pivoxil Hydrochloride Hydrate in deuterated methanol for nuclear magnetic resonance spectroscopy (1in 50)as directed under Nuclear Magnetic Resonance Spectroscopy <2.21>(1H),using tetramethylsilane for nuclear magnetic resonance spectroscopy as an internal reference compound:it exhibits a triplet signal A at around d 6.3ppm,and a single signal B at around d 6.7ppm,and the ratio of integrated intensity of each signal,A:B,is about 1:1.

(3)Dissolve 10mg of Cefcapene Pivoxil Hydrochloride Hydrate in 2mL of a mixture of water and methanol (1:1),and add 1drop of silver nitrate TS:a white precipitate is formed.

Absorbance <2.24>E 1z

1cm (265nm):255–285(30mg calcu-lated on the anhydrous basis,a mixture of acetate buŠer solu-tion,pH 5.5and methanol (1:1),2000mL).

Optical rotation <2.49>[a ]20D :＋51–＋549

(0.1g calculated on the anhydrous basis,methanol,10mL,100mm).Purity (1)Heavy metals <1.07>—Proceed with 2.0g of Cefcapene Pivoxil Hydrochloride Hydrate according to Method 4,and perform the test.Prepare the control solution with 2.0mL of Standard Lead Solution (not more than 10ppm).

(2)Related substance I—Dissolve an amount of Cefca-pene Pivoxil Hydrochloride Hydrate,equivalent to about 10mg (potency),in 2mL of methanol,add a mixture of water and methanol (1:1)to make 50mL,and use this solution as the sample solution.Perform the test with 30m L of the sam-ple solution as directed under Liquid Chromatography <2.01>according to the following conditions,and determine each peak area by the automatic integration method.If necessary,compensate the base-line by performing in the same manner as the test with 30m L of a mixture of water and methanol (1:1).Measure the amount of the peak other than cefcapene pivoxil by the area percentage method:the amounts of the peaks,having the relative retention times of about 1.5and about 1.7with respect to cefcapene pivoxil,are not more than 0.2z ,respectively.The amount of the peak other than the peaks mentioned above is not more than 0.1z ,and the total of them is not more than 1.5z .Operating conditions —