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Sulbactam Sodium / Ocial Monographs

JP XV
very slightly soluble in ethanol (99.5), and practically insoluble in acetonitrile. Identication (1) Determine the infrared absorption spectrum of Sulbactam Sodium as directed in the potassium bromide disk method under the Infrared Spectrophotometry <2.25>, and compare the spectrum with the Reference Spectrum: both spectra exhibit similar intensities of absorption at the same wave numbers. (2) Sulbactam Sodium responds to the Qualitative Tests <1.09> (1) for sodium salt. Optical rotation <2.49> 100 mL, 100 mm). [a]20: 219 2339(1 g, water, D

lution. To 20 mL of the sample solution add 6 mL of dilute nitric acid and water to make 50 mL. Perform the test using this solution as the test solution. Prepare the control solution with 0.30 mL of 0.01 mol W hydrochloric acid VS (not more L than 0.005z). (3) Sulfate <1.14>To 40 mL of the sample solution obtained in (2) add 1 mL of dilute hydrochloric acid and water to make 50 mL. Perform the test using this solution as the test solution. Propare the control solution with 0.50 mL of 0.005 mol W sulfuric acid VS (not more than 0.006z). L (4) CalciumTo 10 mL of the sample solution obtained in (2) add 1 mL of ammonium oxalate TS: this solution shows immediately no change. (5) Heavy metals <1.07>Proceed with 5.0 g of White Soft Sugar according to Method 1, and perform the test. Prepare the control solution with 2.5 mL of Standard Lead Solution (not more than 5 ppm). (6) Arsenic <1.11>Prepare the test solution with 1.0 g of White Soft Sugar according to Method 1, and perform the test (not more than 2 ppm). (7) Invert sugarDissolve 5.0 g of White Soft Sugar in water to make 100 mL, lter if necessary, and use this solution as the sample solution. Separately place 100 mL of alkaline copper (II) sulfate solution in a 300-mL beaker, cover the beaker with a watch glass, and boil. Immediately add 50.0 mL of the sample solution, boil the mixture exactly for 5 minutes, add at once 50 mL of freshly boiled and cooled water, dip it in a water bath of a temperature below 109 for C 5 minutes, and collect the precipitate in a tared glass lter (G4). Wash the residue on the lter with water until the last washing is neutral, then wash with 10 mL of ethanol (95), add 10 mL of diethyl ether, and dry at 1059 for 30 minutes: the C mass of the residual precipitate is not more than 0.120 g. Loss on drying <2.41> 2 hours). Not more than 1.30z (15 g, 1059 C, Not more than 0.1z (2 g).

pH <2.54> Dissolve 1.0 g of Sulbactam Sodium in 20 mL of water: the pH of the solution is between 5.2 and 7.2. Purity (1) Clarity and color of solutionDissolve 1.0 g of Sulbactam Sodium in 20 mL of water: the solution is clear, and colorless to pale yellow. (2) Heavy metals <1.07>Proceed with 1.0 g of Sulbactam Sodium according to Method 2, and perform the test. Prepare the control solution with 2.0 mL of Standard Lead Solution (not more than 20 ppm). (3) Arsenic <1.11>Prepare the test solution with 1.0 g of Sulbactam Sodium as directed in Method 3, and perform the test (not more than 2 ppm). (4) Sulbactam penicillamineWeigh accurately about 0.2 g of Sulbactam Sodium, dissolve in the mobile phase to make exactly 50 mL, and use this solution as the sample solution. Separately, weigh accurately about 40 mg of sulbactam sodium for sulbactam penicillamine, dissolve in 2 mL of water, add 0.5 mL of sodium hydroxide TS, allow to stand for 10 minutes at a room temperature, and add 0.5 mL of 1 mol W hydrochloric acid TS, then add the mobile phase to L make exactly 100 mL. Pipet 5 mL of this solution, add the mobile phase to make exactly 50 mL, and use this solution as the standard solution. Perform the test with exactly 10 mL 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, AT and AS, of sulbactam penicillamine by the automatic integration method: the amount of sulbactam penicillamine is not more than 1.0z. Amount (z) of sulbactam penicillamine ( W S / W T ) ( A T / A S ) 5

Residue on ignition <2.44> Containers and storage ers.

ContainersWell-closed contain-

Sulbactam Sodium

WS: Amount (mg) of sulbactam sodium for sulbactam penicillamine WT: Amount (mg) of the sample
C8H10NNaO5S: 255.22 Monosodium (2S,5R )-3,3-dimethyl-7-oxo-4-thia1-azabicyclo[3.2.0]heptane-2-carboxylate 4,4-dioxide [69388-84-7]

Sulbactam Sodium contains not less than 875 mg (potency) per mg, calculated on the anhydrous basis. The potency of Sulbactam Sodium is expressed as mass (potency) of sulbactam (C8H11NO5S: 233.24).
Description Sulbactam Sodium occurs as a white to yellowish white crystalline powder. It is freely soluble in water, sparingly soluble in methanol,

Operating conditions Column, column temperature, mobile phase, and ow rate: Proceed as directed in the operating conditions in the Assay. Detector: An ultraviolet absorption photometer (wavelength: 230 nm). System suitability System performance: Proceed as directed in the system suitability in the Assay. System repeatability: When the test is repeated 6 times with 10 mL of the standard solution under the above operating conditions, the relative standard deviation of the peak areas of sulbactam penicillamine is not more than 2.0z.

JP XV
Water <2.48> Not more than 1.0z (0.5 g, volumetric titration, direct titration). Assay Weigh accurately an amount of Sulbactam Sodium and Sulbactam Reference Standard, equivalent to about 0.1 g (potency), dissolve each in a suitable amount of the mobile phase, add exactly 10 mL of the internal standard solution, then add the mobile phase to make 100 mL, and use these solutions as the sample solution and standard solution. Perform the test with 10 mL each of the sample solution and standard solution as directed under Liquid Chromatography <2.01> according to the following conditions, and calculate the ratios, Q T and Q S, of the peak area of sulbactam to that of the internal standard. Amount [mg (potency)] of sulbactam (C8H11NO5S) WS(Q T/Q S) 1000

Ocial Monographs / Sulbenicillin Sodium

1123

Sulbenicillin Sodium contains not less than 900 mg (potency) and not more than 970 mg (potency) per mg, calculated on the anhydrous basis. The potency of Sulbenicillin Sodium is expressed as mass (potency) of sulbenicillin (C16H18N2O7S2: 414.45).
Description Sulbenicillin Sodium occurs as white to light yellowish white powder. It is very soluble in water, freely soluble in methanol, and slightly soluble in ethanol (99.5). It is hygroscopic. Identication (1) Determine the infrared absorption spectrum of Sulbenicillin Sodium as directed in the potassium bromide disk method under the Infrared Spectrophotometry <2.25>, and compare the spectrum with the Reference Spectrum or the spectrum of Sulbenicillin Sodium Reference Standard: both spectra exhibit similar intensities of absorption at the same wave numbers. (2) Sulbenicillin Sodium responds to the Qualitative Tests <1.09> (1) for sodium salt. (1 Optical rotation <2.49> [a]20: 167 1829 g calculated D on the anhydrous basis, water, 20 mL, 100 mm). pH <2.54> The pH of a solution obtained by dissolving 0.20 g of Sulbenicillin Sodium in 10 mL of water is between 4.5 and 7.0. Purity (1) Clarity and color of solutionDissolve 2.5 g of Sulbenicillin Sodium in 5 mL of water: the solution is clear and colorless to pale yellow. (2) Heavy metals <1.07>Proceed with 1.0 g of Sulbenicillin Sodium according to Method 1, and perform the test. Prepare the control solution with 2.0 mL of Standard Lead Solution (not more than 20 ppm). (3) Arsenic <1.11>Prepare the test solution with 1.0 g of Sulbenicillin Sodium according to Method 1, and perform the test (not more than 2 ppm). (4) Related substancesDissolve 0.10 g of Sulbenicillin Sodium in 15 mL of the mobile phase, and use this solution as the sample solution. Perform the test with 10 mL of the sample solution as directed under Liquid Chromatography <2.01> according to the following conditions, determine each peak area by the automatic integration method, and calculate the amount of these peaks by the area percentage method: the amount of the each peak other than the two peaks of sulbenicillin is not more than 2.0z, and the total amount of the peaks other than the two peaks of sulbenicillin is not more than 5.0z. Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 254 nm). Column: A stainless steel column 3.9 mm in inside diameter and 30 cm in length, packed with octadecylsilanized silica gel for liquid chromatography (5 mm in particle diameter). Column temperature: A constant temperature of about 259 C. Mobile phase: Dissolve 10 g of potassium dihydrogen phosphate in 750 mL of water, adjust the pH to 6.0 0.1 with sodium hydroxide TS, and add water to make 1000 mL. To 940 mL of this solution add 60 mL of acetonitrile. Flow rate: Adjust the ow rate so that the retention time of

WS: Amount [mg (potency)] of Sulbactam Reference Standard Internal standard solutionA solution of ethyl parahydroxybenzoate in the mobile phase (7 in 1000). Operating conditions Detector: An ultraviolet absorption photometer (wavelength: 220 nm). Column: A stainless steel column 3.9 mm in inside diameter and 30 cm in length, packed with octadecylsilanized silica gel for liquid chromatography (10 mm in particle diameter). Column temperature: A constant temperature of about 359 C. Mobile phase: To 750 mL of 0.005 mol W tetrabutylamL monium hydroxide TS add 250 mL of acetonitrile for liquid chromatography. Flow rate: Adjust the ow rate so that the retention time of sulbactam is about 6 minutes. System suitability System performance: When the procedure is run with 10 mL of the standard solution under the above operating conditions, sulbactam and the internal standard are eluted in this order with the resolution between these peaks being not less than 1.5. System repeatability: When the test is repeated 6 times with 10 mL of the standard solution under the above operating conditions, the relative standard deviation of the peak areas of sulbactam is not more than 1.0z.
Containers and storage ContainersTight containers.

Sulbenicillin Sodium

C16H16N2Na2O7S2: 458.42 Disodium (2 S,5 R,6 R )-3,3-dimethyl-7-oxo-6-[(2 R )-2-phenyl2-sulfonatoacetylamino]-4-thia-1azabicyclo[3.2.0]heptane-2-carboxylate [28002-18-8 ]