Ergotamine Tartrate Injection
» Ergotamine Tartrate Injection is a sterile solution of Ergotamine Tartrate and the tartrates of its epimer, ergotaminine, and of other related alkaloids, in Water for Injection to which Tartaric Acid or suitable stabilizers have been added. The total alkaloid content, in each mL, is not less than 450 µg and not more than 550 µg. The content of ergotamine tartrate [(C33H35N5O5)2·C4H6O6] is not less than 52.0 percent and not more than 74.0 percent of the content of total alkaloid; the content of ergotaminine tartrate is not more than 45.0 percent of the content of total alkaloid.
Packaging and storage Preserve in single-dose, light-resistant containers, preferably of Type I glass.
Bacterial endotoxins 85 It contains not more than 357.0 USP Endotoxin Units per mg of ergotamine tartrate.
pH 791: between 3.5 and 4.0.
Other requirements It meets the requirements under Injections 1.
Chloroform Use chloroform that recently has been saturated with water.
Standard preparation Dissolve about 10 mg of USP Ergotamine Tartrate RS, accurately weighed, with warming if necessary, in 50 mL of diluted alcohol and sufficient water to give a concentration of 50.0 µg per mL.
Ergotamine preparation Pipet a volume of Injection, equivalent to about 5 mg of ergotamine tartrate, into a beaker. Add 5 mL of Chloroform and a portion of sodium bicarbonate approximately equivalent in weight to one-tenth that of the portion of Injection taken. Mix, and add sufficient chromatographic siliceous earth to make a fluffy mixture (about 1 g for each mL of the Injection taken plus 3 g in addition). Pack the mixture in a chromatographic tube about 2.5 cm in diameter and about 30 cm in length. Rinse the sides of the beaker with 2 mL of Chloroform. Add sufficient chromatographic siliceous earth to make a fluffy mixture, and transfer it to the column.
Prepare a second column using a mixture of 9 g of the siliceous earth with 7 mL of citric acid solution (1 in 4). Place a mixture of 2 g of the siliceous earth and 2 mL of water on top of the second column. Insert a pledget of glass wool, and mount the tube containing the specimen so that the eluate from it will drain into the tube containing the citric acid solution. Add a total of 90 mL of Chloroform to the upper tube, and receive the eluate from the lower tube in a 200-mL volumetric flask. Rinse the tip of the upper tube with Chloroform. Pass sufficient Chloroform through the lower tube to dilute the eluate to volume. This eluate is the Ergotamine preparation.
Extrude the adsorbent from the second column by means of slight air pressure into a 600-mL beaker containing 10 g of sodium bicarbonate, and mix. Cautiously add 50 mL of water, with continuous stirring. Wash the mixture with water into a 250-mL separator, and extract the ergotamine with four 15-mL portions of Chloroform. Pass the extracts through a glass wool filter, combining them in a 100-mL volumetric flask, wash the filter, and dilute with Chloroform to volume. This is the Ergotamine preparation.
Pipet 10 mL of the Ergotamine preparation and 20 mL of the Ergotamine preparation into separate, small conical flasks, and evaporate with the aid of a current of air to dryness.
Total alkaloid preparation Pipet a volume of Injection, equivalent to about 2.5 mg of ergotamine tartrate, into a 50-mL volumetric flask, add 25 mL of alcohol, then add tartaric acid solution (1 in 100) to volume.
Procedure Pipet 5 mL each of the Standard preparation and the Total alkaloid preparation into separate, small conical flasks. To the dried residues of Ergotamine preparation and Ergotamine preparation add 5.0 mL of a freshly prepared solution of equal volumes of alcohol and tartaric acid solution (1 in 100). In turn, place each flask in an ice bath, and swirl continuously while adding, dropwise, 10.0 mL of p-dimethylaminobenzaldehyde TS. Allow to stand in subdued light at room temperature for not less than 90 minutes and not more than 2 hours. Concomitantly determine the absorbances of the four solutions at the wavelength of maximum absorbance at about 545 nm, with a suitable spectrophotometer, against a reagent blank.
Calculation Calculate the quantity of total alkaloids in terms of mg of (C33H35N5O5)2·C4H6O6 in the volume of Injection taken by the formula:
0.05C(AU / AS)in which C is the concentration, in µg per mL, of USP Ergotamine Tartrate RS in the Standard preparation, and AU and AS are the absorbances of the solutions from the Total alkaloid preparation and the Standard preparation, respectively.
Calculate the percentage of ergotamine tartrate taken by the formula:
(A¢ / AU)50
in which A¢ represents the absorbance of the solution from the Ergotamine preparation and AU is as defined in the preceding paragraph. Calculate the percentage of ergotaminine tartrate taken by the formula:
(A¢¢ / AU)50
in which A¢¢ represents the absorbance of the solution from the Ergotamine preparation.
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USP32NF27 Page 2279