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11221122 JP XVSulbactam Sodium / Ocial Monographs

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 molWL hydrochloric acid VS (not more

than 0.005z).

(3) Sulfate To 40 mL of the sample solution ob-

tained in (2) add 1 mL of dilute hydrochloric acid and waterto make 50 mL. Perform the test using this solution as the

test solution. Propare the control solution with 0.50 mL of

0.005 molWL sulfuric acid VS (not more than 0.006z).

(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 Proceed with 5.0 g of White

Soft Sugar according to Method 1, and perform the test. Pre-

pare the control solution with 2.5 mL of Standard Lead Solu-

tion (not more than 5 ppm).

(6) Arsenic 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 solu-

tion as the sample solution. Separately place 100 mL of alka-

line 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 109C for

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 1059C for 30 minutes: the

mass of the residual precipitate is not more than 0.120 g.

Loss on drying Not more than 1.30z (15 g, 1059C,

2 hours).

Residue on ignition Not more than 0.1z (2 g).

Containers and storage ContainersWell-closed contain-

ers.

Sulbactam Sodium

C8H10NNaO5S: 255.22

Monosodium (2S,5R)-3,3-dimethyl-7-oxo-4-thia-

1-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 yellow-ish white crystalline powder.

It is freely soluble in water, sparingly soluble in methanol,

very slightly soluble in ethanol (99.5), and practically insolu-

ble in acetonitrile.

Identication (1) Determine the infrared absorption spec-

trum of Sulbactam Sodium as directed in the potassium

bromide disk method under the Infrared Spectrophotometry

, and compare the spectrum with the Reference Spec-trum: both spectra exhibit similar intensities of absorption at

the same wave numbers.

(2) Sulbactam Sodium responds to the Qualitative Tests

(1) for sodium salt.

Optical rotation [a]20

D : 219 2339(1 g, water,

100 mL, 100 mm).

pH 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 Proceed with 1.0 g of Sulbac-

tam 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).


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 solu-

tion. 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

molWL hydrochloric acid TS, then add the mobile phase tomake 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 according to the fol-

lowing 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

(WS/WT)(A T/A S) 5

WS: Amount (mg) of sulbactam sodium for sulbactam

penicillamine

WT: Amount (mg) of the sample

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.

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11231123JP XV Ocial Monographs / Sulbenicillin Sodium

Water Not more than 1.0z (0.5 g, volumetric titra-

tion, 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 so-

lutions as the sample solution and standard solution. Per-

form the test with 10 mL each of the sample solution and stan-

dard solution as directed under Liquid Chromatography

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/QS) 1000

WS: Amount [mg (potency)] of Sulbactam Reference

Standard

Internal standard solutionA solution of ethyl parahydrox-ybenzoate in the mobile phase (7 in 1000).




Column: A stainless steel column 3.9 mm in inside di-

ameter and 30 cm in length, packed with octadecylsilanized

silica gel for liquid chromatography (10 mm in particle di-

ameter).

Column temperature: A constant temperature of about

359C.

Mobile phase: To 750 mL of 0.005 molWL tetrabutylam-

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 condi-

tions, 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 (2S,5R,6R )-3,3-dimethyl-7-oxo-6-[(2R )-2-phenyl-

2-sulfonatoacetylamino]-4-thia-1-

azabicyclo[3.2.0]heptane-2-carboxylate [28002-18-8 ]

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 Sul-benicillin Sodium is expressed as mass (potency) of sul-benicillin (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 spec-

trum of Sulbenicillin Sodium as directed in the potassium

bromide disk method under the Infrared Spectrophotometry

, and compare the spectrum with the Reference Spec-

trum or the spectrum of Sulbenicillin Sodium Reference

Standard: both spectra exhibit similar intensities of absorp-

tion at the same wave numbers.

(2) Sulbenicillin Sodium responds to the Qualitative Tests

(1) for sodium salt.

Optical rotation [a]D20:167 1829(1 g calculated

on the anhydrous basis, water, 20 mL, 100 mm).

pH 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 Proceed with 1.0 g of Sul-

benicillin 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).


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

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 sul-

benicillin is not more than 2.0z, and the total amount of the

peaks other than the two peaks of sulbenicillin is not morethan 5.0z.




Column: A stainless steel column 3.9 mm in inside di-

ameter and 30 cm in length, packed with octadecylsilanized

silica gel for liquid chromatography (5 mm in particle di-

ameter).

Column temperature: A constant temperature of about

259C.

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

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