Abstract

Abstract Unsaponifiable residues are determined in milk samples by the following procedure: oily drug bases and fats are extracted with iso-octane (rather than the usual mixed ether solvents) in an alkaline alcohol-acetone mixture; this extract is concentrated and the fatty constituents are saponified with KOH. The unsaponifiable matter is then re-extracted with iso-octane and the residual soaps and extraneous constituents are removed by water washing and column chromatography. Mineral oil added at levels of 12–404 ppm to milk samples was quantitatively recovered, with an average value of 98%. Unsaponifiable matter in market milk was also determined; results demonstrated good precision between duplicate analyses. Milk-out studies were performed to determine the rate of diffusion and dissipation of infused formulations.

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