Separation of hydrocortisone and epi-hydrocortisone by solvent extraction

✍ Scribed by Zhigang Tang; Xien Hu; Yongjun Zhu

• Publisher: Wiley (John Wiley & Sons)
• Year: 1997
• Tongue: English
• Weight: 319 KB
• Volume: 70
• Category: Article
• ISSN: 0268-2575
• DOI: 10.1002/(sici)1097-4660(199711)70:3<287::aid-jctb761>3.0.co;2-2

✦ Synopsis

Solvent extraction, instead of traditional crystallization, is suggested as a new method for separation of hydrocortisone and its optical isomer, epihydrocortisone. The extraction behavior of alcohols, ketones, esters, ethers and chlorinated hydrocarbons was studied experimentally. For the industrial separation process it was found that the best solvents are n-butyl acetate or chloroform. The distribution coefficients of hydrocortisone and epi-hydrocortisone in an n-butyl acetate/water system at 17¡C were found to be 9É98 and 2É62, respectively, and 5É57 and 1É93, respectively, in a chloroform/water system at 17¡C. When n-butyl acetate or chloroform solution of crude hydrocortisone (the mixture of hydrocortisone, epi-hydrocortisone and other steroid impurities) was scrubbed by deionized water in a nine-stage cross-current at 25¡C, the organic phase hydrocortisone purity increased from 78É10% to 98É22% (wt%) for the n-butyl acetate case and from 78É10% to 98É02% (wt%) for the chloroform case. The medicinal standard for hydrocortisone was attained. The e †ects of alcohol concentration, temperature, salting-out and pH on extraction are also discussed.