Pergolide Oral Suspension, Veterinary
» Pergolide Oral Suspension, Veterinary contains not less than 90.0 percent and not more than 110.0 percent of the labeled amount of pergolide mesylate (C19H26N2S·CH4O3S). Prepare Pergolide Oral Suspension, Veterinary, 1 mg per mL, using one of the following procedures (see Pharmaceutical CompoundingNonsterile Preparations 795):
Method IConnect an empty calibrated 35-cc Luer lock injection syringe to the port of a fluid-dispensing connector. Remove the plunger of another 35-cc Luer lock syringe, and set the plunger aside. Lock the barrel of this syringe onto the open port of the connector. Set this connected syringe apparatus in an upright, vertical position that is perpendicular to the work surface with the open syringe on top. Add 10 mL of Vehicle for Oral Suspension directly into the open barrel. Transfer 20 mg of Pergolide Mesylate into the open syringe barrel. Replace the plunger on the open syringe, and invert the apparatus 180. Apply 50 depressions to each syringe to mix. Consolidate the mixture into a single syringe. Disconnect the empty syringe. Add, via another 35-cc Luer lock injection syringe connected to the open port of the fluid-dispensing connector, a quantity of Vehicle for Oral Solution sufficient to make the total volume of the mixture 20 mL. Reattach the empty 35-cc syringe to the fluid-dispensing connector. Apply 50 depressions to each syringe to formulate a uniform suspension.
Method IIAdd 20 mg of Pergolide Mesylate to the mortar. Add 10 mL of Vehicle for Oral Suspension, and mix to a uniform paste. Add Vehicle for Oral Solution in small portions almost to final volume [noteThe final volume is 20 mL. ] , and mix thoroughly after each addition. Transfer the contents of the mortar, stepwise and quantitatively, to a calibrated bottle. Add sufficient Vehicle for Oral Solution to a final volume of 20 mL, and mix well.
Packaging and storage Preserve in tight, light-resistant containers, and store in a refrigerator.
Labeling Label to state that it is to be well-shaken, protected from light, and kept out of the reach of children; the beyond-use date; the nominal content of pergolide mesylate in the Oral Suspension, Veterinary; and that it is for veterinary use only.
USP Reference standards 11
Identification The retention time of the pergolide peak in the chromatogram of the Assay preparation corresponds to those in the chromatograms of the Standard preparations, as obtained in the Assay.
pH 791: between 4.0 and 4.2.
Beyond-use-date Fourteen days after the day on which it was compounded.
Octanesulfonate buffer Mix 10 mL of a 0.5 M sodium octanesulfonate solution with 490 mL of water and adjust with glacial acetic acid to a pH of 2.2.
Mobile phase Mix equal volumes of Octanesulfonate buffer and acetonitrile.
Pergolide standard stock preparation [noteUse low-actinic glassware. ] Dissolve an accurately weighed quantity of USP Pergolide Mesylate RS in methanol and dilute quantitatively, and stepwise if necessary, with methanol to obtain a solution having a known concentration of about 1.0 mg of pergolide mesylate per mL.
Standard preparations [noteUse low-actinic glassware. ] Prepare five Standard preparation solutions of known concentrations of about 20 µg, 10 µg, 5 µg, 2 µg, and 1 µg of pergolide mesylate per mL by quantitatively diluting the Pergolide standard stock solution with Mobile phase.
Diluent Mix equal volumes of methanol and 0.01 N hydrochloric acid.
Assay preparation [noteUse low-actinic glassware. ] Transfer 500 µL of Pergolide Oral Suspension, Veterinary to a 5-mL volumetric flask; dilute with Diluent to volume. Dilute with Mobile phase an accurately measured aliquot of the resulting solution to prepare a solution containing 10 µg of pergolide mesylate per mL.
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 223-nm detector and a 4.6-mm × 15-cm column that contains 5-µm packing L1. The column is maintained at 40. The flow rate is about 1 mL per minute. Chromatograph the Standard preparations and the Assay preparation, and record the peak responses as directed for Procedure: as determined from the pergolide peak of the 20 µg per mL Standard preparation, the tailing factor is not more than 2.0 and the relative standard deviation for replicate injections is not more than 2.0; a regression curve calculated from the five Standard preparations has a square of the correlation coefficient (r2) not less than 0.995; and the resolution of the pergolide peak from its nearest neighbor, as determined from the Assay preparation, is not less than 2.0.
Procedure Separately inject equal volumes (about 25 µL) of the Standard preparations and the Assay preparation into the chromatograph, record the chromatograms, and measure the heights for the major peaks. Generate a regression curve of peak height versus pergolide mesylate concentration, and calculate the equation for the regression line. Calculate the concentration, in mg per mL, of pergolide mesylate (C19H26N2S·CH4O3S) in the portion of Pergolide Mesylate Oral Suspension, Veterinary taken directly from the regression equation, correcting for dilution.
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USP35NF30 Page 4272Pharmacopeial Forum: Volume No. 34(2) Page 289