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Kinetics and Thermodynamics of Lactose Mutarotation through Chromatography.

ABSTRACT: The mutarotation kinetics and thermodynamics of the reaction α-lactose ⇌ β-lactose have been measured in dilute solutions using liquid chromatography without any derivatization step, using a C18 column and pure water as the mobile phase. The effect of temperature (0.5-45 °C) of the starting powder composition (α-lactose-rich or β-lactose-rich powder) and of the solvent composition (water with up to 35% weight fraction of seven organic solvents) has been experimentally investigated. Increasing the temperature leads to faster kinetics, following an Arrhenius model, and to slightly decreasing concentration-based equilibrium ratio. Conversely, increasing the weight fraction of organic solvent at 25 °C resulted in slower kinetics and smaller concentration-based equilibrium ratio. The starting powder composition is shown not to influence the kinetics or thermodynamics of the process. The corresponding parameter estimation problem is thoroughly discussed, taking into account the small difference in response factors of the lactose diastereomers.

SUBMITTER: Trespi S

PROVIDER: S-EPMC10979398 | biostudies-literature | 2024 Mar

REPOSITORIES: biostudies-literature

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Kinetics and Thermodynamics of Lactose Mutarotation through Chromatography.

Trespi Silvio S Mazzotti Marco M

Industrial & engineering chemistry research 20240318 12

The mutarotation kinetics and thermodynamics of the reaction α-lactose ⇌ β-lactose have been measured in dilute solutions using liquid chromatography without any derivatization step, using a C18 column and pure water as the mobile phase. The effect of temperature (0.5-45 °C) of the starting powder composition (α-lactose-rich or β-lactose-rich powder) and of the solvent composition (water with up to 35% weight fraction of seven organic solvents) has been experimentally investigated. Increasing th ...[more]

PMID: 38559666

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Project description:It is common to find that some of the lactose in dairy powders and pharmaceutical tablets is present in the unstable amorphous state. Therefore, their crystallization thermodynamics in different solvents are particularly important. In this paper, the solubility of α-lactose monohydrate (α-LM) in 15 mono-solvents such as ethanol, isopropanol, methanol, 1-propanol, 1-butanol, 2-butanol, isobutanol, 1-pentanol, isoamylol, 1-hexanol, 1-heptanol, 1-octanol, propanoic acid, acetonitrile, and cyclohexanone was evaluated by using the gravimetric method in the temperature ranges from 274.05 K to 323.05 K at constant pressure (1 atm). In the given temperature range, the solubility of α-LM in these solvents increased with the rising of temperature, the highest solubility of α-LM was found in methanol (2.37 × 104), and the lowest was found in 1-hexanol (0.80 × 105). In addition, the increase of α-LM solubility in isopropanol was the largest. The sequence at 298.15 K was: methanol > 1-butanol > isopropanol > ethanol > 1-propanol > 1-heptanol > isobutanol > propionic acid > 1-pentanol > 1-octanol > acetonitrile > isoamylol > 2-butanol > cyclohexanone > 1-hexanol. Solvent effect analysis shows that the properties of α-LM are more important than those of solvents. The Apelblat equation, λh equation, Wilson model, and NRTL model were used to correlate the experimental values. The root-mean-square deviation (RMSD) and relative average deviation (RAD) of all models were less than 2.68 × 10-2 and 1.41 × 10-6, respectively, implying that the fitted values of four thermodynamic models all agreed well with the experimental values. Moreover, the thermodynamic properties of the dissolution process (i.e., dissolution Gibbs free energy (ΔdisG), molar enthalpy (ΔdisH), and molar entropy (ΔdisS)) for α-LM in selected solvents were determined. The results indicate that ΔdisH/(J/mol) (from 0.2551 to 6.0575) and ΔdisS/(J/mol/K) (from 0.0010 to 0.0207) of α-LM in these solvents are all positive, and the values of ΔdisH and ΔdisS. ΔdisG/(J/mol) (from -0.0184 to -0.6380) are all negative. The values were observed to decrease with rising temperatures, implying that α-LM dissolution is an endothermic, entropy-driven, and spontaneous process. The solid-liquid equilibrium data and dissolution thermodynamics of α-LM were obtained, which provide a basis for industrial production.

Dataset Information

Kinetics and Thermodynamics of Lactose Mutarotation through Chromatography.

Publications

Kinetics and Thermodynamics of Lactose Mutarotation through Chromatography.

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