Citric Acid,Magnesium Oxide,and Sodium Carbonate Irrigation
»Citric Acid,Magnesium Oxide,and Sodium Carbonate Irrigation is a sterile solution of Citric Acid,Magnesium Oxide,and Sodium Carbonate in Water for Injection.It contains not less than 95.0percent and not more than 105.0percent of the labeled amounts of citric acid (C6H8O7·H2O),magnesium oxide (MgO),and sodium carbonate (Na2CO3).
Packaging and storage— Preserve in single-dose containers,preferably of Type Ior Type IIglass.
Identification—
A: It responds to the tests for Sodium á191ñand for Magnesium á191ñ.
B: To 10mLof the Irrigation add 1mLof mercuric sulfate TS,heat to boiling,and add a few drops of potassium permanganate TS:a white precipitate is formed.
Bacterial endotoxins á85ñ It contains not more than 2.80Endotoxin Unit per mL.
pHá791ñ: between 3.8and 4.2.
Other requirements— It meets the requirements under Injections á1ñ,except that the container may be designed to empty rapidly,and may exceed 1000mLin capacity.
Assay for citric acid—
Mobile phase— Add 2.0mLof sulfuric acid to 800mLof water,mix,and dilute with water to 1000mL.Filter through a membrane filter,heat to 40,and degas.Maintain the temperature of the Mobile phaseat 40throughout the analysis.
Standard preparation— Dissolve a suitable quantity of anhydrous citric acid,accurately weighed,in water to obtain a solution having a known concentration of about 1.2mg per mL.
Resolution solution— Prepare a solution in water containing about 1mg of citric acid and about 2mg of boric acid per mL.
Assay preparation— Transfer an accurately measured volume of Irrigation,equivalent to about 130mg of citric acid monohydrate,to a 100-mLvolumetric flask,dilute with water to volume,and mix.
Chromatographic system (see Chromatography á621ñ)—The liquid chromatograph is equipped with a refractive index detector and a 7.8-mm ×30-cm column that contains packing L17.The column temperature is maintained at 40.The flow rate is about 0.6mLper minute.Chromatograph the Standard preparationand the Resolution solution,and record the peak responses as directed under Procedure:the relative standard deviation for replicate injections of the Standard preparationis not more than 1.5%,and the resolution,R,between the citric acid and boric acid peaks is not less than 4.0.
Procedure— Separately inject equal volumes (about 50µL)of the Standard preparationand the Assay preparationinto the chromatograph,record the chromatograms,and measure the responses for the major peaks.Calculate the quantity,in mg,of C6H8O7·H2Oin each mLof the Irrigation taken by the formula:
(210.14/192.12)(100C/V)(rU/rS),
in which 210.14and 192.12are the molecular weights of citric acid monohydrate and anhydrous citric acid,respectively,Cis the concentration,in mg per mL,of anhydrous citric acid in the Standard preparation,Vis the volume,in mL,of Irrigation taken,and rUand rSare the peak responses for citric acid obtained from the Assay preparationand the Standard preparation,respectively.
Assay for magnesium oxide— Transfer an accurately measured volume of Irrigation,equivalent to about 40mg of magnesium oxide,to a beaker containing 130mLof water heated to 75±5,and add 4mLof ammonium chloride TSand then 5mLof ammonium hydroxide.Mix,and add slowly,with stirring,8mLof 8-hydroxyquinoline TS.After allowing to stand for 30minutes at 75,filter through a sintered-glass crucible,previously dried and weighed,and wash the precipitate with 50mLof a warm mixture of water and 6Nammonium hydroxide (45:5),followed by 50mLof cool water.Dry the crucible and contents at 105for 3hours,cool,and weigh.Determine the equivalent of MgOin the portion of Irrigation taken by multiplying the weight of C18H12MgN2O2·2H2Oso obtained by 0.1156.
Assay for sodium carbonate—
Sodium chloride stock solution— Transfer 475mg of sodium chloride,previously dried at 105for 2hours and accurately weighed,to a 100-mLvolumetric flask.Dissolve in water,dilute with water to volume,and mix.
Internal standard solution— Transfer 636mg of lithium chloride to a 1000-mLvolumetric flask,dissolve in water,dilute with water to volume,and mix.
Standard preparation— Quantitatively prepare a mixture of Internal standard solutionand Sodium chloride stock solution(99:1).
Assay preparation— Dilute an accurately measured volume of Irrigation quantitatively with water to obtain a stock solution containing about 4.4mg of sodium carbonate per mL.Quantitatively prepare a mixture of Internal standard solutionand this stock solution (99:1).
Procedure— Concomitantly determine the emittances of the Standard preparationand the Assay preparationat 591nm and 671nm with a suitable flame photometer,adjusting the instrument to zero emittance with Internal standard solution.Calculate the quantity,in mg,of Na2CO3in each mLof the Irrigation taken by the formula:
(105.99/116.88)(C)(L/D)(RU,591/RU,671)(RS,671/RS,591),
in which 105.99is the molecular weight of sodium carbonate,116.88is two times the molecular weight of sodium chloride,Cis the concentration,in mg per mL,of sodium chloride in the Sodium chloride stock solution,Lis the labeled quantity,in mg per mL,of sodium carbonate in the Irrigation,Dis the concentration,in mg per mL,of sodium carbonate in the stock solution used to prepare the Assay preparation,on the basis of the labeled quantity in each mL,and the extent of dilution,RU,591and RU,671are the emittance readings obtained from the Assay preparationat the wavelengths indicated by the subscripts,and RS,671and RS,591are the emittance readings obtained from the Standard preparationat the wavelengths indicated by the subscripts.
Auxiliary Information— Staff Liaison:Behnam Davani,Ph.D.,MBA,Senior Scientist
Expert Committee:(PA7)Pharmaceutical Analysis 7
USP28–NF23Page 486
Phone Number:1-301-816-8394