Printed on: Fri Jan 05 2024, 09:53:25 PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-54F0F942-3711-4D1F-BA1D-2A33481C799A_3_en-US
Printed by: USP NF Official Date: Official as of 01-May-2018 Document Type: USP @2024 USPC
Do Not Distribute DOI Ref: j666t DOI: [Link]
1
the solvent front has moved about 15 cm above the line of
Digoxin Injection application. Remove the plate, and allow the solvent to
evaporate. Spray the plate with Chloramine T–trichloroacetic
» Digoxin Injection is a sterile solution of Digoxin acid reagent, freshly mixed, and heat in an oven at 110° for 10
minutes. Examine the plate under long-wavelength UV
in Water for Injection and Alcohol or other suitable light: the R F value of the principal spot in the chromatogram
solvents. It contains not less than 90.0 percent and of the Test solution corresponds to that of the Standard
not more than 105.0 percent of the labeled solution.
amount of C41H64O14. Bacterial Endotoxins Test á85ñ—It contains not more than
200.0 USP Endotoxin Units per mg of digoxin.
Packaging and storage—Preserve in single-dose Alcohol Determination á611ñ: between 9.0% and 11.0%
containers, preferably of Type I glass. Avoid exposure to of C2H5OH.
excessive heat. Other requirements—It meets the requirements
USP Reference standards á11ñ— underInjections and Implanted Drug Products á1ñ.
USP Digoxin RS Assay—
Identification— Mobile phase—Proceed as directed in the Assay under
A: Injection meets the requirements for Identification test A Digoxin.
under Digoxin Oral Solution. Standard preparation—Dissolve an accurately weighed
B: Chloramine T–trichloroacetic acid reagent, Spotting quantity of USP Digoxin RS in diluted alcohol, and dilute
solvent, and Standard solution—Proceed as directed for quantitatively with diluted alcohol to obtain a solution
Identification test B under Digoxin Oral Solution. having a known concentration of about 250 µg per mL. Use a
Test solution—Pipet a volume of Injection, equivalent to sonic bath to aid dissolution. If necessary, dilute quantitatively
al
0.5 mg of digoxin, into a separator, and add 5 mL of water. to match, approximately, the concentration of the Injection.
Extract with three 10-mL portions of chloroform, combining Chromatographic system and System suitability preparation
the extracts in a conical flask. Evaporate the combined —Proceed as directed in the Assay under Digoxin.
chloroform extracts on a steam bath with the aid of a current Procedure—Separately inject equal volumes (about 10 µL)
of air to dryness. (If traces of water or propylene glycol remain, of the Standard preparation and Injection into the
dry the flask in vacuum at 100° for 30 minutes.) Dissolve the
residue in 2 mL of Spotting solvent.
Procedure—Apply 10 µL of the Test solution and 10 µL of
ci chromatograph, record the chromatograms, and measure the
responses for the major peaks. Calculate the quantity, in µg,
of C41H64O14 in each mL of the Injection taken by the formula:
the Standard solution on a line parallel to and about 2.5 cm
from the bottom edge of a reversed-phase thin-layer C(r U/r S)
ffi
chromatographic plate coated with a 0.25-mm layer of
chromatographic silica gel mixture to which is permanently in which C is the concentration, in µg per mL, of USP
bonded octadecylsilane (C18). Allow the spots to dry, and Digoxin RS in the Standard preparation; and r U and r S are the
place the plates in a developing chamber containing a mixture responses for the digoxin peaks obtained from the Injection
of methanol and water (7:3). Develop the chromatogram until and the Standard preparation, respectively.
O
[Link] 1/1