Add the following:
» Piperazine Adipate contains not less than 98.0 percent and not more than 101.0 percent of C4H10N2·C6H10O4, calculated on the anhydrous basis.
Packaging and storage Preserve in well-closed containers, and store at room temperature.
Labeling Label it to indicate that it is for veterinary use only.
USP Reference standards 11
USP Piperazine Adipate RS.
B: In the test for Chromatographic purity, the principal spot in the chromatogram obtained from Test solution 2 observed after spraying with the ninhydrin solutions corresponds in RF value, color, and size to that in the chromatogram obtained from Standard solution 1.
C: To 10 mL of a 1 in 20 solution of it add 5 mL of hydrochloric acid, and extract with three 10-mL portions of ether. Evaporate the combined ether extracts to dryness, wash the residue with water, and dry at 105: the residue of adipic acid so obtained melts at between 150 and 154.
Water, Method I 921: not more than 0.5%.
Residue on ignition 281: not more than 0.1%.
Solvent Prepare a mixture of 13.5 N ammonium hydroxide and dehydrated alcohol (3:2).
Test solution 1 Prepare a solution of Piperazine Adipate in Solvent containing 100 mg per mL.
Test solution 2 Mix 1 mL of Test solution 1 and 9 mL of Solvent.
Standard solution 1 Prepare a solution of USP Piperazine Adipate RS in Solvent containing 10 mg per mL.
Standard solution 2 Prepare a solution of ethylenediamine in Solvent containing 0.25 mg per mL.
Standard solution 3 Prepare a solution of triethylenediamine in Solvent containing 0.25 mg per mL.
Resolution solution Prepare a solution in Solvent containing 0.25 mg of triethylenediamine and 10 mg of Piperazine Adipate per mL.
Procedure Separately apply 5-µL portions of Test solution 1, Test solution 2, Standard solution 1, Standard solution 2, Standard solution 3, and the Resolution solution to a suitable thin-layer chromatographic plate (see Chromatography 621), coated with a 0.25-mm layer of chromatographic silica gel. Allow the spots to dry, and develop the chromatograms in a solvent system consisting of a freshly prepared mixture of acetone and 13.5 N ammonium hydroxide (80:20) until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the developing chamber, mark the solvent front, and dry the plate at 105. Spray the plate with a 0.3% solution of ninhydrin in a mixture of butyl alcohol and glacial acetic acid (100:3). Spray the plate again with a 0.15% solution of ninhydrin in dehydrated alcohol, dry the plate at 105 for 10 minutes, and examine the plate: any secondary spot in the chromatogram obtained from Test solution 1 is not more intense than the principal spot in the chromatogram obtained from Standard solution 2 (0.25%). Spray the plate with 0.1 N iodine TS, allow to stand for 10 minutes, and examine the plate: any spot corresponding to triethylenediamine in the chromatogram obtained from Test solution 1 is not more intense than the principal spot in the chromatogram obtained from Standard solution 3 (0.25%). In a valid test, the chromatogram obtained from the Resolution solution shows a spot due to triethylenediamine clearly separated from the principal spot. Disregard any spot at the origin of any chromatogram.
Assay Dissolve about 100 mg of Piperazine Adipate, accurately weighed, in 10 mL of glacial acetic acid, heating gently if necessary. Add 60 mL of glacial acetic acid and 0.25 mL of p-naphtholbenzein TS, and titrate with 0.1 N perchloric acid until the brownish-yellow color of the solution turns green. Each mL of 0.1 N perchloric acid is equivalent to 11.61 mg of C4H10N2·C6H10O4.USP32
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USP32NF27 Page 3314Pharmacopeial Forum: Volume No. 33(6) Page 1201