Standard preparation— Dissolve an accurately weighed quantity of USP Ergotamine Tartrate RSin a tartaric acid solution (1in 500),and dilute quantitatively and stepwise with the same tartaric acid solution as necessary to obtain a solution having a known concentration of about 18µg per mL.

Test preparation— Discharge the minimum recommended dose into the sampling apparatus and detach the inhaler as directed.Rinse the apparatus (filter and interior)with four 5.0-mLportions of a tartaric acid solution (1in 500),and transfer the resulting solutions quantitatively to a 50-mLcentrifuge tube.Add 10mLof trichlorotrifluoroethane,insert the stopper,shake vigorously for 1minute and centrifuge for 5minutes.Use the clear supernatant as the Test preparation.

Procedure— Into three separate flasks transfer 6.0mLeach of the Test preparation,the Standard preparation,and a tartaric acid solution (1in 500)to provide the blank.To each flask add 10.0mLof p-dimethylaminobenzaldehyde TS,mix,and allow to stand for 30minutes.Concomitantly determine the absorbances with a suitable spectrophotometer,in 5-cm cells,of the solutions from the Test preparationand the Standard preparation,at the wavelength of maximum absorbance at about 546nm,against the blank.Calculate the quantity,in µg,of (C33H35N5O5)2.C4H6O6contained in the minimum dose taken by the formula: in which Cis the concentration,in µg per mL,of USP Ergotamine Tartrate RSin the Standard preparation;Nis the number of sprays discharged to obtain the minimum recommended dose;and AUand ASare the absorbances of the solutions from the Test preparationand the Standard preparation,respectively.

Standard preparation— Prepare as directed under Unit spray content.

Assay preparation— [NOTE—Asuitable specimen beaker is one having a small indentation formed on its inside bottom surface having dimensions adequate to accept the aerosol valve stem during actuation,thereby preventing particle entrapment and side-of-stem leakage during the delivery of the specimen.]Place 10mLof trichlorotrifluoroethane in a suitable 100-mLbeaker.Prime the valve of Ergotamine Tartrate Inhalation Aerosol by alternately shaking and firing it 10times through its oral inhalation actuator.Accurately weigh the Aerosol,shake it,and immediately deliver a single spray under the surface of the trichlorotrifluoroethane,actuating the valve by pressing the tip into the indentation in the bottom of the beaker.Raise the Aerosol above the surface of the trichlorotrifluoroethane,and shake it gently preparatory to delivering another spray similarly under the surface of the trichlorotrifluoroethane.Deliver a total of 2sprays in this manner.Rinse the valve stem and ferrule with about 2mLof trichlorotrifluoroethane,collecting the rinsing with the specimen in the beaker.Allow the Aerosol to dry,weigh it,and determine the total weight of the 2sprays.Transfer the solution to a centrifuge tube with the aid of two 3-mLportions of trichlorotrifluoroethane,and add 10.0mLof tartaric acid solution (1in 500).Insert the stopper,shake vigorously for 15minutes,centrifuge for 5minutes,and use the clear supernatant as the Assay preparation.

Procedure— Transfer 5.0mLeach of the Standard preparation,the Assay preparation,and a blank consisting of tartaric acid solution (1in 500)to separate test tubes.To each tube add 10.0mLof p-dimethylaminobenzaldehyde TS,mix,and allow to stand for 30minutes.Concomitantly determine the absorbances of the solutions against the blank in 1-cm cells at the wavelength of maximum absorbance at about 546nm,with a suitable spectrophotometer.Calculate the quantity,in mg,of (C33H35N5O5)2·C4H6O6in each mLof the Aerosol taken by the formula: in which Cis the concentration,in µg per mL,of USP Ergotamine Tartrate RSin the Standard preparation;dis the density,in g per mL,of Aerosol determined as directed for din the Procedurein the Assayunder Isoproterenol Sulfate Inhalation Aerosol;Wis the weight,in g,of the specimen taken;and AUand ASare the absorbances of the solutions from the Assay preparationand the Standard preparation,respectively.