Comparison of the performance of chiral stationary phase for separation of fluoxetine enantiomers.

Separation of fluoxetine enantiomers on five chiral stationary phases (chiralcel OD-H, chiralcel OJ-H, chiralpak AD-H, cyclobond capital I, Ukrainian 2000 DM and kromasil CHI-TBB) was investigated. The optimal mobile phase compositions of fluoxetine separation on each column were hexane/isopropanol/diethyl amine (98/2/0.2, v/v/v), hexane/isopropanol/diethyl amine (99/1/0.1, v/v/v), hexane/isopropanol/diethyl amine (98/2/0.2, v/v/v), methanol/0.2% triethylamine acetic acid (TEAA) (25/75, v/v; pH 3.8) and hexane/isopropanol/diethyl amine (98/2/0.2, v/v/v), respectively. Experimental results demonstrated that baseline separation (R(S)>1.5) of fluoxetine enantiomers was obtained on chiralcel OD-H, chiralpak AD-H, and cyclobond capital I, Ukrainian 2000 DM while the best separation was obtained on the last one. The eluate orders of fluoxetine enantiomers on the columns were determined. The first eluate by chiralcel OJ-H and kromasil CHI-TBB is the S-enantiomer, while by chiralpak AD-H and cyclobond I 2000 DM is the R-enantiomer.

Separation of phosphatidylcholine from soybean phospholipids by simulated moving bed.

A simulated moving bed (SMB), equipped with eight silica-gel columns, was used to separate phosphatidylcholine (PC) from soybean phospholipids. The effects of flow rate in Sections 2 (Q(2)) and 3 (Q(3)), switching time, feed flow rate and feed concentration on the operating performance parameters: purity, recovery, productivity and desorbent consumption were studied. Operating conditions leading to more than 90% purity in both outlet streams have been identified, together with those achieving optimal performance. Regions leading to complete separation are observed and explained theoretically. As the mass-transfer effect was not considered, the triangle theory only gives initial guesses for the optimal operating conditions.

Study on retention factor and resolution of tocopherols by supercritical fluid chromatography.

To develop a process for separation of natural alpha-tocopherol from gamma- and delta-tocopherols by supercritical fluid chromatography, the effects of pressure, temperature and the ethanol concentration in the mobile phase on the retention factor and resolution of tocopherols were studied comprehensively. The ranges of the studied pressure, temperature and ethanol concentration were 12 to 20 MPa, 30 to 90 degrees C and 0 to 6.54 wt% respectively. It was found that the retention factors of the tocopherols decrease as the ethanol concentration in the mobile phase increases. The resolution of tocopherols increases as the temperature increases and as the pressure decreases, and there is a maximum of the ethanol concentration curve at a definite temperature and pressure. A simplified model of the retention factor ln k' = A + B/T + C rho - D(rho/T) + E(rho2/T) based on the unified molecular theory was proposed. The experimental data were correlated by the model with the AARD% less than 14.70%.

Preparation of natural alpha-tocopherol from non-alpha-tocopherols.

Non-alpha-tocopherols are hydroxymethylated and hydrogenated to produce alpha-tocopherol in one pot process by simultaneously reacting with paraformaldehyde and hydrogen in the presence of catalysts of benzenesulfonic acid and 5% Pd/C in an autoclave. Effects of various operation conditions have been studied. The preferable reaction conditions are: temperature 180 degrees C to 200 degrees C, pressure 5.0 MPa, acid concentration 0.5 g/100 ml ethanol, mass ratio of Pd/C to tocopherols 7.1 g/100 g, and reaction time 5.0 h. A product with alpha-tocopherol content of 80% was obtained by using a raw material with a total tocopherols content of 80.54%. The conversion of non-alpha-tocopherols is almost 100%, and the mole yield of alpha-tocopherol is more than 90%.

[Study on content variation of chemical constituents during combination of rhizoma coptidis alkaloids with fructus evodiae flavonoids by high performance liquid chromatography].

In order to study the compatibility of Chinese herbal drugs, a method was proposed by investigating chemical reactions with combination of chemical constituents or major groups of chemical compounds of Chinese herbal drugs. The content variation of chemical constituents during combination of rhizoma coptidis alkaloids with fructus evodiae flavonoids was analyzed by high performance liquid chromatography (HPLC). The experimental results showed that only small changes of the relative peak areas of different chemical constituents were observed and no new peaks were detected. No chemical reactions were observed during the compatibility test of rhizoma coptidis alkaloids with fructus evodiae flavonoids.