Mannitol, solution preparation

Prepare vials containing an inert material (e.g., 5% w/v mannitol solution) and run the freeze drying process after the actual product run. Analyze the vials with inert material for the active content of the previous product. 

Preparatively the last method is carried out by shaking the powdered solid pyridine compound with an aqueous-alcoholic solution of mannitol (2 moles of KOH and 2 moles of mannitol per atom of osmium) until there is complete dissolution or the pyridine compound is first dissolved in methylene dichloride (or chloroform) and then shaken with the alkaline mannitol solution until the methylene chloride solution is completely decolorized. Yields of diol are usually excellent. Since warming is not involved, side reactions rarely occur. The method is particularly important in the steroid field.125... 

Figure 5 X-ray powder diffraction patterns of (1) a freeze-dried mannitol solution and (2) the same preparation after heating at 70°C for 30 min. Peaks marked with asterisks do not appear in the diffractograms of any known mannitol polymorphs. All peaks in pattern (2) are attributable to (3- or -mannitol. Reproduced with permission from Yu et al. ...

Anesthetized rats were prepared for micropuncture as previously reported (2). Osmotic diuresis was induced by infusion of a 5 % mannitol solution in isotonic saline to permit rapid serial collections of urine necessary to determine fractional recoveries of the isotopes. Prior to abdominal surgery some rats were slowly infused i.v. with benzbromarone or benziodarone at a dose of 10 mg/kg/BW. 

Cobalt-on-alumina catalysts with increased dispersion and catalytic activity are prepared by addition of mannitol to the cobalt nitrate solution prior to impregnation. Thermogravimetric analysis (TGA) and in situ visible microscopy of the impregnation solution show that the organic compound reacts with cobalt nitrate, forming a foam. The foam forms because significant amounts of gas are released through a viscous liquid. The structure of the foam is retained in the final calcined product. It is this effect that is responsible for the increased dispersion. 

The unmodified catalyst was prepared by dissolving cobalt nitrate hexahydrate (19.76g, 68 mmol) in water (9 ml) and impregnating the solution into alumina (16.0 g). The catalyst was dried at 105°C in static air for 3 h and calcined at 400°C for 1 h. The mannitol-containing catalyst was prepared as described above, except that mannitol (2 g, 11 mmol) was dissolved in the cobalt nitrate solution prior to impregnation. The Co/mannitol ratio was 6.2. 

Tonicity agents are added to injectable preparations to prevent osmotic shock at the site of injection upon administration, and thereby reduce local irritation. Typical excipients used for tonicity adjustment include saline, glycerin, mannitol, dextrose, and trehalose. Tonicity is a colligative property that depends primarily on the number of dissolved particles in solution. Hence, the amount of tonicity agent to be added depends on the specific formulation. Typically, osmolality of 280 to 320mOsm is considered iso-osmotic. 

Example.—Mannitol.—The hexa-acetyl derivative (p. 259) is prepared and purified, and a quantity of it—about 0-2 gm.—along with 100 c.cs. of 10% benzene sulphonic acid solution placed in a steam distillation flask. The flask is connected to a condenser on one side and to an apparatus for the generation of pure steam on the other. A suction flask to serve as receiver is attached by a cork to the condenser, and to the side tube of the suction flask a soda-lime tube to prevent the entrance of carbon dioxide is attached. Steam is blown through the flask until (1-5—3 hours) the distillate passing over is neutral. The whole distillate is then titrated with standard baryta, using phenolphthalein as indicator. 

For both of these syntheses 2,3-isopropylidene-D-glyceraldehyde is readily accessible as an initial material since it can be prepared by oxidation of l,2 5,6-diisopropylidene-D-mannitol with lead tetraacetate in solution in dry benzene.188... 

Cognate preparation. (R)-2,3-0-Isopropylideneglyceraldehyde. To a solution of l,2 5,6-di-0-isopropylidene-D-mannitol (50 g, 0.19mol, Expt 5.114) in dry benzene (500 ml) (CAUTION) is slowly added lead tetra-acetate (90 g, 0.2 mol) with stirring. After 3 hours the mixture is filtered, and the filtrate concentrated below 25 °C to a syrup from which four 30-ml portions of carbon tetrachloride are evaporated at a temperature maintained below 25 °C. The syrup is distilled in vacuo. The first few millilitres are discarded and the main fraction is collected, 34 g (68%), b.p. 31 °C/5mmHg (1). 

---