Statistical analysis of one-pot lipase-catalyzed esterification of ϵ-caprolactone with methyl- -glucopyranoside and its extension
One-pot synthesis of oligomeric sugar ester was carried out by lipase-catalyzed esterification of ε-caprolactone (ECL) with methyl-d-glucopyranoside (MGP) followed by the chain extension of ECL monomer/oligomer. Two-level half fractional factorial design was employed to analyse the effects of select...
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Format: | Article |
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Elsevier
2020
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Online Access: | http://eprints.um.edu.my/25207/ https://doi.org/10.1016/j.bcab.2019.101464 |
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Summary: | One-pot synthesis of oligomeric sugar ester was carried out by lipase-catalyzed esterification of ε-caprolactone (ECL) with methyl-d-glucopyranoside (MGP) followed by the chain extension of ECL monomer/oligomer. Two-level half fractional factorial design was employed to analyse the effects of selected operating variables namely lipase loading (1.2–2.8% w/v), initial ECL (3.8–11.5% w/v), initial MGP (0.04–0.14% w/v), temperature (40–60 °C) and agitation (90–180 rpm) as a function of maximum dry weight (% w/v) of MGP-6-O-oligo-ECL. It was found that individual variables viz. lipase loading, initial ECL and temperature affect the maximum product formation. The interaction effects between variables indicated the presence of relationship among them. Spectroscopic authentication showed the presence of covalent bond between the hydroxyl group of MGP with carboxylic acid end group of ECL monomer/oligomer. Thermal analysis indicated three degradation stages of functionalized oligomer. The molecular weight analysis of the functionalized oligomer was observed at 1655 g mol−1 with narrow PDI value of 1.36. Conversion of initial ECL was 90% compared to 14% of initial MGP. © 2019 Elsevier Ltd |
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