Cefapirin-Sodium-441
424JP XV Cefapirin Sodium/O?cial Monographs
Cefalotin Sodium in5mL of water:the solution is clear and light yellow.
(2)Heavy metals<1.07>—Proceed with1.0g of Cefalotin Sodium according to Method2,and perform the test.Pre-pare the control solution with 2.0mL of Standard Lead Solution(not more than20ppm).
(3)Arsenic<1.11>—Prepare the test solution with1.0g of Cefalotin Sodium according to Method3,and perform the test(not more than2ppm).
(4)Related substances—Pipet1mL of the standard solution obtained in the Assay,add the mobile phase to make exactly100mL,and use this solution as the standard solu-tion.Perform the test with exactly10m L each of the sample solution obtained in the Assay and the standard solution pre-pared here as directed under Liquid Chromatography<2.01> according to the following conditions,and determine each peak area by the automatic integration method:the peak area other than cefalotin from the sample solution is not more than the peak area of cefalotin from the standard solution, and the total area of the peaks other than cefalotin from the sample solution is not more than3times the peak area of cefalotin from the standard solution.
Operating conditions—
Detector,column,column temperature,mobile phase,and ‰ow rate:Proceed as directed in the operating conditions in the Assay.
Time span of measurement:About4times as long as the retention time of cefalotin.
System suitability—
Test for required detectability:Measure exactly1mL of the standard solution,and add the mobile phase to make exactly10mL.Con?rm that the peak area of cefalotin obtained from10m L of this solution is equivalent to7to13z of that from10m L of the standard solution.
System performance:Heat the standard solution in a water bath of909C for10minutes,and cool.Measure exactly2.5 mL of this solution,and add the mobile phase to make ex-actly100mL.When the procedure is run with10m L of this solution under the above operating conditions,the resolution between the peak of cefalotin and the peak,having the rela-tive retention time of about0.5with respect to cefalotin,is not less than9,and the symmetry factor of the peak of cefalotin is not more than1.8.
System repeatability:When the test is repeated3times with 10m L of the standard solution under the above operating conditions,the relative standard deviation of the peak area of cefalotin is not more than2.0z.
Water<2.48>Not more than1.0z(0.5g,volumetric titra-tion,back titration).
Assay Weigh accurately an amount of Cefalotin Sodium and Cefalotin Sodium Reference Standard,equivalent to about25mg(potency),and dissolve each in the mobile phase to make exactly25mL,and use these solutions as the sample solution and standard solution.Perform the test with exactly 10m L each of the sample solution and standard solution as directed under Liquid Chromatography<2.01>according to the following conditions,and determine the peak areas,A T and A S,of cefalotin of the solutions.
Amount[m g(potency)]of cefalotin(C16H16N2O6S2)＝W S×(A T/A S)×1000
W S:Amount[mg(potency)]of Cefalotin Sodium Refer-
ence Standard
Operating conditions—
Detector:An ultraviolet absorption photometer(wave-length:254nm).
Column:A stainless steel column 4.6mm in inside di-ameter and25cm in length,packed with octadecylsilanized silica gel for liquid chromatography(5m m in particle di-ameter).
Column temperature:A constant temperature of about 409C.
Mobile phase:Dissolve17g of sodium acetate trihydrate in 790mL of water,and add0.6mL of acetic acid(100).If necessary adjust the pH to5.9±0.1with0.1mol/L sodium hydrochloride TS or acetic acid(100).To this solution add 150mL of acetonitrile and70mL of ethanol(95).
Flow rate:Adjust the‰ow rate so that the retention time of cefalotin is about12minutes.
System suitability—
System performance:Heat the standard solution in a water bath of909C for10minutes,and cool.Measure exactly2.5 mL of this solution,and add the mobile phase to make exactly100mL.When the procedure is run with10m L of this solution under the above operating conditions,the resolution between the peak of cefalotin and the peak,having the rela-tive retention time of about0.5with respect to cefalotin is not less than9,and the symmetry factor of the peak of cefalotin is not more than1.8.
System repeatability:When the test is repeated6times with 10m L of the standard solution under the above operating conditions,the relative standard deviation of the peak area of cefalotin is not more than1.0z.
Containers and storage Containers—Tight containers. Cefapirin Sodium
セファピリンナトリウム
C17H16N3NaO6S2:445.45
Monosodium(6R,7R)-3-acetoxymethyl-8-oxo-7-
[2-(pyridin-4-ylsulfanyl)acetylamino]-5-thia-1-
azabicyclo[4.2.0]oct-2-ene-2-carboxylate
[24356-60-3]
Cefapirin Sodium contains not less than865m g (potency)per mg,calculated on the anhydrous basis. The potency of Cefapirin Sodium is expressed as mass (potency)of cefapirin(C17H17N3O6S2:423.46). Description Cefapirin Sodium occurs as a white to yellow-ish white powder.
It is freely soluble in water,sparingly soluble in methanol, slightly soluble in ethanol(95),and practically insoluble in acetone.
Identi?cation(1)Determine the absorption spectrum of a solution of Cefapirin Sodium(3in200,000)as directed under
425 JP XV O?cial Monographs/Cefatrizine Propylene Glycolate
Ultraviolet-visible Spectrophotometry<2.24>,and compare the spectrum with the Reference Spectrum or the spectrum of a solution of Cefapirin Sodium Reference Standard prepared in the same manner as the sample solution:both spectra ex-hibit similar intensities of absorption at the same wavelengths.
(2)Determine the infrared absorption spectrum of Cefapirin Sodium as directed in the potassium bromide disk method under Infrared Spectrophotometry<2.25>,and com-pare the spectrum with the Reference Spectrum or the spec-trum of Cefapirin Sodium Reference Standard:both spectra exhibit similar intensities of absorption at the same wave numbers.
(3)Determine the spectrum of a solution of Cefapirin Sodium in heavy water for nuclear magnetic resonance spec-troscopy(1in10),using sodium3-(trimethylsilyl)pro-pionate-d4for nuclear magnetic resonance spectroscopy as an internal reference compound,as directed under Nuclear Magnetic Resonance Spectroscopy<2.21>(1H):it exhibits a single signal A at around d2.2ppm,and multiple signals,B and C,at around d7.3ppm and at around d8.3ppm,respec-tively.The ratio of integrated intensity of these signals, A:B:C,is about3:2:2.
(4)Cefapirin Sodium responds to the Qualitative Tests <1.09>(1)for sodium salt.
Optical rotation<2.49>[a]25
D
:＋157–＋1759(2g calculated as the anhydrous basis,water,100mL,100mm).
pH<2.54>Dissolve1.0g of Cefapirin Sodium in10mL of water:pH of the solution is between6.5and8.5.
Purity(1)Heavy metals<1.07>—Proceed with 1.0g of Cefapirin Sodium according to Method2,and perform the test.Prepare the control solution with2.0mL of Standard Lead Solution(not more than20ppm).
(2)Arsenic<1.11>—Prepare the test solution with1.0g of Cefapirin Sodium according to Method3,and perform the test(not more than2ppm).Use a solution of magnesium ni-trate hexahydrate in ethanol(95)(1in25).
(3)Related substances—Dissolve0.1g of Cefapirin Sodi-um in5mL of a mixture of acetone and water(3:1),and use this solution as the sample solution.Pipet1mL of the sample solution,add a mixture of acetone and water(3:1)to make exactly100mL,and use this solution as the standard solu-tion.Perform the test with these solutions as directed under Thin-layer Chromatography<2.03>.Spot5m L each of the sample solution and standard solution on a plate of silica gel with‰uorescent indicator for thin-layer chromatography. Develop with a mixture of ethyl acetate,acetone,water and acetic acid(100)(5:2:1:1)to a distance of about10cm,and air-dry the plate.Examine under ultraviolet light(main wavelength:254nm):the spots other than the principal spot and other than the spot at the original point from the sample solution are not more intense than the spot from the standard solution.
Water<2.48>Not more than2.0z(0.7g,volumetric titra-tion,direct titration).
Assay Weigh accurately an amount of Cefapirin Sodium and Cefapirin Sodium Reference Standard equivalent to about0.1g(potency),dissolve each in phosphate bu?er solu-tion,pH6.0to make exactly100mL.Pipet5mL of each so-lution,add exactly5mL of the internal standard solution and phosphate bu?er solution,pH6.0to make100mL,and use these solutions as the sample solution and standard solu-tion,respectively.Perform the test with20m L each of the sample solution and standard solution as directed under Liq-uid Chromatography<2.01>according to the following con-ditions,and calculate the ratios,Q T and Q S,of the peak area of cefapirin to that of the internal standard.
Amount[m g(potency)]of cefapirin(C17H17N3O6S2)＝W S×(Q T/Q S)×1000
W S:Amount[mg(potency)]of Cefapirin Sodium Refer-ence Standard
Internal standard solution—A solution of vanillin(1in 1000).
Operating conditions—
Detector:An ultraviolet absorption photometer (wavelength:254nm).
Column:A stainless steel column 4.6mm in inside di-ameter and15cm in length,packed with octadecylsilanized silica gel for liquid chromatography(5m m in particle di-ameter).
Column temperature:A constant temperature of about 409C.
Mobile phase:A mixture of0.05mol W L sodium di-hydrogenphosphate TS,pH2.6and acetonitrile(93:7).
Flow rate:Adjust the‰ow rate so that the retention time of cefapirin is about7minutes.
System suitability—
System performance:When the procedure is run with20 m L of the standard solution under the above operating condi-tions,cefapirin and the internal standard are eluted in this order with the resolution between these peaks being not less than10.
System repeatability:When the test is repeated6times with 20m L of the standard solution under the above operating conditions,the relative standard deviation of the ratios of the peak area of cefapirin to that of the internal standard is not more than1.0z.
Containers and storage Containers—Hermetic containers. Cefatrizine Propylene Glycolate
セファトリジンプロピレングリコール
C18H18N6O5S2.C3H8O2:538.60
(6R,7R)-7-[(2R)-2-Amino-2-(4-
hydroxyphenyl)acetylamino]-8-oxo-3-[2-(1H-1,2,3-
triazol-4-yl)sulfanylmethyl]-5-thia-1-
azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid
monopropane-1,2-diolate(1/1)
[51627-14-6,Cefatrizine]
Cefatrizine Propylene Glycolate contains not less than785m g(potency)and not more than876m g