Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

Abstract

Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak's extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r 2 =0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak's extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

Regenerated Silica Gel for Isolation of Ethyl p-Methoxycinnamate from Kaempferia galanga rhizome

“…Method A: The procedure was followed lit. [3] with modification. The 8 g used silica gel was directly furnace the used silica gel at 600 ⁰C for 8 h. Method B: The procedure was followed lit.…”

“…The recycle approach for obtaining silica gel from glass waste, carried out with activation and purification method by using hydrochloride acid, is previously studied and reported to be used as stationary phase for papaya leave extract column chromatography [2]. The regeneration of silica gel, after the separation method with column chromatography of Curcuma xanthorrhiza Roxb (temulawak) extract, reported to be conducted with furnace at 600 o C and found the effectiveness of the regenerated silica gel for utilized as stationary phase in column chromatography [3]. The previous study of silica from rice husk extraction mentioned that the treatment of aqueous solution of sulfuric acid in prior of calcination can prevent the black particle formation due to the presence of impurities [4].…”