The Effect of Acids on Alkaloid Yield in Pressurized Water Extraction of Narcissus Pseudonarcissus

Pressurized water (PW) extraction of galanthamine from Narcissus pseudonarcissus bulbs was performed. The obtained yield was compared with the yield from conventional acidified water extraction and methanolic Soxhlet extraction. Both PW and conventional acidified water extraction were followed by a subsequent purification step for the alkaloids. The PW extraction (70 °C, 150 bar, 45 min) yielded as much galanthamine as methanolic-Soxhlet extraction (ca. 3.50 mg/g). Meanwhile, acid-base extraction with 1% of HBr (v/v) at 65 °C for 3 h gave a lower yield (ca. 2.65 mg/g). A higher PW temperature did not significantly increase the galanthamine yield. Pressure increase is not necessary since more water-soluble compounds such as proteins and polysaccharides are co-extracted, resulting in high viscosity of the water extract solution, which hampers the filtration process. Hence, the acidity of the solution is highly important both in the case of PW extraction and acidified water extraction. Besides galanthamine, the total alkaloid profile following Narcissus alkaloids was also obtained. Lycoramine, O-methyloduline, norgalanthamine, epi-norgalanthamine, narwedine, oduline, haemanthamine, O-methyllycorenine, and a haemanthamine derivate were identified. Although a high yield was obtained from PW extraction, the further purification needs to be improved to obtain an economically feasible industrial extraction process

Recovery of lactose from simulated delactosed whey permeate by a low-temperature crystallization process

ABSTRACT: Delactosed whey permeate is the mother liquor/by-product of lactose manufacture, but it still contains around 20 wt% lactose. The high mineral content, stickiness, and hygroscopic behavior prevent further recovery of lactose in the manufacturing process. Therefore, its use is currently limited to low-value applications such as cattle feed, and more often it is seen as waste. This study investigates a new separation technique operating at sub-zero conditions. At low temperature, precipitation of calcium phosphate is expected to be reduced and the lower solubility at sub-zero temperature makes it possible to recover a large portion of the lactose. We found that lactose could be crystallized at sub-zero conditions. The crystals had a tomahawk morphology and an average size of 23 and 31 µm. In the first 24 h, the amount of calcium phosphate precipitated was limited, whereas the lactose concentration was already close to saturation. The overall rate of crystallization was increased compared with the crystals recovered from a pure lactose solution. Mutarotation was rate limiting in the pure system but it did not limit the crystallization of lactose from delactosed whey permeate. This resulted in faster crystallization; after 24 h the yield was 85%

A sub-zero crystallization process for the recovery of lactose

In industry, lactose is generally produced by concentrating whey permeate by evaporation followed by a slow cooling process where lactose is crystallized. Here, an alternative method is presented whereby the concentration and crystallization steps are combined at sub-zero temperatures, so-called eutectic freeze crystallization. It was discovered that simultaneous crystallization of lactose and water (ice) is possible. The obtained lactose crystals had an average size of 10 μm and a thin triangular or tomahawk morphology. The process was analyzed in detail in two steps: freeze concentration and lactose crystallization at sub-zero temperatures. Freeze concentration experiments showed that concentrating to supersaturation was possible without excessive lactose crystallization. In the second step, lactose was crystallized at temperatures below zero from a 30 wt% lactose solution, without observation of significant primary or secondary nucleation. The amount of seed material had a large influence on the final yield, crystal size and morphology. The optimum seed amount was found to be at 0.08% of the total lactose; the resulting crystals had an average size of 26 μm and a tomahawk morphology. Although highly supersaturated conditions are present in the sub-zero crystallization of lactose, crystal growth is found to be the predominant process rather than nucleation

Crystallization kinetics of lactose recovered at sub-zero temperatures: A population balance model combining mutarotation, nucleation and crystal growth

Crystallization kinetics of lactose at sub-zero temperatures are modelled in this paper using a population balance model. There are two competing effects on the crystallization kinetics at low temperatures. On the one hand, mass transport and the rate of both mutarotation and nucleation are reduced, reducing the crystallization rate.On the other hand, supersaturation is increased, which increases nucleation and crystal growth and thereby increases the crystallization rate. To explore this phenomenon, the crystal growth of α-lactose monohydrate at sub-zero conditions was modelled, including the effects of mutarotation and nucleation. The model is compared with experiments. It was found that stirring did not have a significant influence, indicating that the process was not limited by mass transfer. Mutarotation had a significant effect; the model showed fast depletion of α-lactose; at high lactose concentrations, the mutarotation of β-lactose could not keep up with this depletion

Scaling up continuous eutectic freeze crystallization of lactose from whey permeate : A pilot plant study at sub-zero temperatures

Eutectic freeze crystallization is explored as an alternative to the state-of-the-art evaporation process for the recovery of lactose from whey permeate. At the so-called eutectic freezing point, both water (the solvent) and lactose (the solute) crystallize and can be removed continuously while continuously feeding whey permeate. This continuous process is demonstrated on a pilot scale at sub-zero temperatures. In the first instance, only freeze concentration of whey permeate took place at − 4 ◦C. It was possible to reach a lactose concentration of 30 wt% and hardly any nucleation was observed. The resulting ice had high purity, with a lactose concentration of ±2 wt %. Next, the eutectic phase was reached, and lactose and ice crystallized simultaneously and were continuously removed from the system, the resulting crystals had parallelogram morphology with an average size of 10 µm. Ice was recovered at a rate of 60 kg/h and lactose was recovered at a rate of 16 kg/h, yielding over 80% of the feed lactose. A conceptional design was proposed for an improved yield and reduction of energy. Yields of at least 80% and up till 95% could be achieved. Compared to the state-of-the-art mechanical vapor recompression (MVR), EFC is 80% more energy efficient

Oil-in-water emulsions based on hydrophobic eutectic systems

We demonstrate that oil-in-water emulsions can be prepared from hydrophobic eutectic systems (ES). Light microscopy and dynamic light scattering show that droplets are formed and zeta potential measurements indicate sufficient stability against coalescence. We investigate whether Ostwald ripening occurs in these ES-in-water emulsions by following the droplet growth over time and comparing it with an emulsion comprising decane in water. At first sight, the Ostwald ripening rate of the ES-in-water emulsion is expected to be orders of magnitude larger than the ripening of the decane-in-water emulsion due to a much higher solubility of the dispersed phase. However, experimentally we find that the ES-in-water emulsion actually grows a factor of two slower than the decane-in-water emulsion. We attribute this to the two-component nature of the ES, since the growth rate is mainly set by the least-soluble component of the ES. Thus, ESs offer the advantage of creating liquid emulsions of solid components, while setting the emulsion stability through their composition

Oil-in-water emulsions based on hydrophobic eutectic systems

We demonstrate that oil-in-water emulsions can be prepared from hydrophobic eutectic systems (ES). Light microscopy and dynamic light scattering show that droplets are formed and zeta potential measurements indicate sufficient stability against coalescence. We investigate whether Ostwald ripening occurs in these ES-in-water emulsions by following the droplet growth over time and comparing it with an emulsion comprising decane in water. At first sight, the Ostwald ripening rate of the ES-in-water emulsion is expected to be orders of magnitude larger than the ripening of the decane-in-water emulsion due to a much higher solubility of the dispersed phase. However, experimentally we find that the ES-in-water emulsion actually grows a factor of two slower than the decane-in-water emulsion. We attribute this to the two-component nature of the ES, since the growth rate is mainly set by the least-soluble component of the ES. Thus, ESs offer the advantage of creating liquid emulsions of solid components, while setting the emulsion stability through their composition

A search for natural hydrophobic deep eutectic solvents based on natural components

Deep eutectic solvents (DESs) based on terpenes are identified and characterized. 507 combinations of solid components are tested, which results in the identification of 17 new hydrophobic DESs. Four criteria are introduced to assess the sustainability of these hydrophobic DESs from a chemical engineering point of view. These criteria include a viscosity smaller than 100 mPa·s, a density difference between DES and water of at least 50 kg·m-3 upon mixing of the DES and water, low transfer of the DES to the water phase and minor to no pH change. The results show that five new hydrophobic DESs based on natural components satisfy these criteria; thymol and coumarin (2:1), thymol and menthol (1:1), thymol and coumarin (1:1), thymol and menthol (1:2) and 1-tetradecanol and menthol (1:2), and thus are promising DESs. These new DESs can be considered as natural deep eutectic solvents, which have the potential to be environmentally friendly. A selected group of the hydrophobic DESs were used for the extraction of riboflavin from water. They all show higher removal of riboflavin in comparison to decanoic acid:tetraoctylammonium bromide (2:1). The highest extraction efficiency of riboflavin from water, 81.1%, was achieved with the hydrophobic DES DecA:Lid (2:1)