» Ioxilan Injection is a sterile solution of Ioxilan in Water for Injection. It contains not less than 95.0 percent and not more than 105.0 percent of the labeled amount of ioxilan (C18H24I3N3O8) as organically bound iodine. It may contain small amounts of suitable buffers and of Edetate Calcium Disodium as a stabilizer. Ioxilan Injection contains no antimicrobial agents.
Packaging and storage Preserve injection in single-dose containers of Type I glass, protected from light.
Labeling Label containers of the Injection to direct the user to discard any unused portion. The label states that it is not to be used if it is discolored or contains a precipitate and states also that it is not for intrathecal use.
USP Reference standards 11
USP Endotoxin RS
A: Evaporate a volume of Injection, equivalent to about 500 mg of ioxilan, to dryness. Char the residue so obtained in a suitable crucible: violet vapors are evolved (presence of iodine).
B: The retention times of the major peaks in the chromatogram of the Assay preparation correspond to those of the major peaks in the chromatogram of the Standard preparation, as obtained in the Assay.
Bacterial endotoxins 85 It contains not more than 0.2 USP Endotoxin Unit per 50 mg of iodine.
Heavy metals, Method II 231: not more than 0.002%.
pH 791: between 6.0 and 7.5.
Free iodine Transfer an accurately measured volume of Injection, equivalent to about 1 g of Ioxilan, to a tared 25-mL volumetric flask, add 13 mL of water, and swirl to dissolve. Add 2.5 mL of 2 N sulfuric acid and 4 mL of toluene. Stopper the flask, and shake vigorously for 1 minute. Allow layers to separate: the toluene layer shows no red color. Reserve the contents of the flask for use as the test solution in the test for Free iodide.
Free iodide Proceed as directed in the test for Free iodide under Ioxilan. The limit is 200 µg of iodide per mL.
Standard stock solution, Internal standard solution, Standard solutions A, B, C, D, and Chromatographic system Proceed as directed in the test for Residual methanol under Ioxilan.
Test solution Transfer an accurately measured volume of Injection, equivalent to about 1 g of ioxilan, to a 10-mL volumetric flask. Add 1.0 mL of Internal standard solution, dilute with water to volume, and mix.
Other requirements It meets the requirements under Injections 1.
Mobile phase Prepare a filtered and degassed mixture of acetonitrile and water (87:13). Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard preparation A Transfer about 60 mg of USP Ioxilan RS, to a 10-mL volumetric flask, and add 1 mL of water. [noteHeat gently, if necessary, to effect dissolution. Cool to room temperature before proceeding. ] Dilute with acetonitrile to volume, and mix.
Standard preparation B Prepare a 1 in 10 dilution of Standard preparation A in Mobile phase.
Assay preparation A Transfer an accurately measured volume of Injection, equivalent to about 60 mg of ioxilan, to a 10-mL volumetric flask, add 1 mL of water, and swirl to mix. Dilute with acetonitrile to volume, and mix.
Assay preparation B Prepare a 1 in 10 dilution of Assay preparation A in Mobile phase.
Chromatographic system (see Chromatography 621)The liquid chromatograph is equipped with a 245-nm detector and a 25-cm × 4.6-mm stainless steel column that contains packing L8. The column is maintained at 30, and the flow rate is about 1 mL per minute. Chromatograph Standard preparation A, and record the peak responses as directed under Procedure: the resolution, R, between the two largest impurity peaks eluting immediately after the second ioxilan isomer peak is not less than 0.3. Chromatograph Standard preparation B, and record the peak responses as directed under Procedure: the resolution, R, between the two ioxilan isomer peaks is not less than 2.2, the column efficiency, based on the larger ioxilan isomer peak, is not less than 4000 theoretical plates, and the relative standard deviation of the sums of the responses of the two ioxilan isomer peaks from replicate injections is not less than 2.0%.
Procedure Separately inject equal volumes (about 10 µL) of Assay preparation A, Assay preparation B, Standard preparation A, and Standard preparation B into the chromatograph, record the chromatograms, and measure the areas of the responses for the major peaks. Record the integrated results, summing the areas of the two ioxilan peaks. From the chromatogram of Assay preparation A in comparison to that of Standard preparation B, determine the quantity of ioxilan in the Injection taken. Determine the percentage of impurities (excluding the serinol impurity with a relative retention time of 0.9 relative to the larger ioxilan isomer peak) by area percent, using the chromatogram of Assay preparation A. Not more than 0.5% of any individual impurity is found, and the total of all impurities is not more than 1.5%. [noteThe impurities eluting on the tail of the second ioxilan isomer peak should be integrated by skimming the peaks. ]
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USP35NF30 Page 3551