Precipitation of calcium gluceptate from aqueous solutions

Suryanarayanan, R; Mitchell, AG

HERO ID

4837150

Reference Type

Journal Article

Year

1984

Language

English

PMID

6694089

HERO ID 4837150
In Press No
Year 1984
Title Precipitation of calcium gluceptate from aqueous solutions
Authors Suryanarayanan, R; Mitchell, AG
Journal Journal of Pharmaceutical Sciences
Volume 73
Issue 1
Page Numbers 78-82
Abstract A precipitate encountered in solutions of calcium gluceptate was identified as hydrated calcium gluceptate. Precipitation was associated with a change from a very soluble amorphous anhydrous form to a sparingly soluble crystalline hydrate, the presence of seed crystals inducing crystallization, and unsuitable proportions of the alpha- and beta-epimers of calcium gluceptate. Various commercial samples and the corresponding precipitates were examined by elemental analysis, thermal analysis, X-ray diffraction, IR spectroscopy, and GC-MS. The proportion of the alpha- and beta-epimers in commercial samples was quantitated by GC. In this method, an aqueous solution of calcium gluceptate was converted into a mixture of glucoheptonic acids and their corresponding lactones by passage through a cation-exchange resin. The solution was freeze-dried, the acid-lactone mixture converted to the gamma-lactones using concentrated hydrochloric acid, and the resulting material trimethylsilylated with trimethylsilylimidazole. Stability studies of solutions prepared from calcium gluceptate obtained from various commercial sources indicate that above approximately 50% alpha-epimer, stability decreased with an increase in the relative proportion of the alpha-epimer. Material complying with USP specifications (pure alpha-epimer) is the least stable in solution. It is suggested that calcium gluceptate containing approximately equal proportions of the alpha- and beta-epimers be introduced in the USP monograph together with a method for estimating the proportions of the epimers.
Doi 10.1002/jps.2600730121
Pmid 6694089
Wosid WOS:A1984SA06500020
Is Certified Translation No
Dupe Override No
Is Public Yes
Language Text English