If the dosage form is a tablet, weigh and finely powder not less than 20 tablets, weigh accurately a portion of the powder, equivalent to about 25 mg of the active ingredient, and transfer to a 125-mL separator; or, if the dosage form is a liquid, transfer a volume of it, equivalent to about 25 mg of the active ingredient and accurately measured, to a 125-mL separator. Then to the separator add 20 mL of dilute sulfuric acid (1 in 350), and shake vigorously for 5 minutes. Add 20 mL of ether, shake carefully, and filter the acid phase into a second 125-mL separator. Shake the ether phase with two 10-mL portions of dilute sulfuric acid (1 in 350), filter each portion of acid into the second separator, and discard the ether. To the acid extract add 10 mL of sodium hydroxide TS
and 50 mL of ether, shake carefully, and transfer the aqueous phase to a third 125-mL separator containing 50 mL of ether. Shake the third separator carefully, and discard the aqueous phase. Wash the two ether solutions, in succession, with a single 20-mL portion of water, and discard the water. Extract each of the two ether solutions with 20-, 20-, and 5-mL portions of dilute sulfuric acid (1 in 70), in the order listed, but each time extract first the ether solution in the third separator and then that in the second separator. Combine the acid extracts in a 50-mL volumetric flask, dilute with the acid to volume, and mix.
NOTEHexane or heptane may be substituted for ether if the distribution ratio of the nitrogenous base between water and hexane, or between water and heptane, favors complete extraction by the organic phase.