| 1. |
- Ahuja, Dipali, et al.
(författare)
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Investigation of solid-liquid phase diagrams of the sulfamethazine-salicylic acid co-crystal
- 2019
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Ingår i: CrystEngComm. - : ROYAL SOC CHEMISTRY. - 1466-8033. ; 21:18, s. 2863-2874
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Tidskriftsartikel (refereegranskat)abstract
- The influence of temperature and solvent on the solid-liquid phase diagram of the 1 : 1 sulfamethazinesalicylic acid co-crystal has been investigated. Ternary phase diagrams of this co-crystal system have been constructed in three solvents: methanol, acetonitrile and a 7 : 3 (v/v) dimethylsulfoxide-methanol mixture, at three temperatures. The system exhibits congruent dissolution in acetonitrile and the co-crystal solubility has been determined by a gravimetric technique. The Gibbs energy of co-crystal formation from the respective solid components has been estimated from solubility data, together with the corresponding enthalpic and entropic component terms. The Gibbs energy of formation ranges from -5.7 to -7.7 kJ mol -1, with the stability increasing with temperature. In methanol and the DMSO-methanol mixture, the co-crystal dissolves incongruently. It is shown that the solubility ratio of the pure components cannot be used to predict with confidence whether the co-crystal will dissolve congruently or incongruently. The size of the region where the co-crystal is the only stable solid phase is inversely related to the pure component solubility ratio of salicylic acid and sulfamethazine.
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| 2. |
- Ahuja, Dipali, et al.
(författare)
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Solution and calorimetric thermodynamic study of a new 1:1 sulfamethazine-3-methylsalicylic acid co-crystal
- 2020
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Ingår i: CrystEngComm. - : Royal Society of Chemistry (RSC). - 1466-8033. ; 22:20, s. 3463-3473
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Tidskriftsartikel (refereegranskat)abstract
- A new 1:1 co-crystal of sulfamethazine (API, SMT) and 3-methylsalicylic acid (coformer, 3mSA) has been synthesized and its crystal structure solved by single crystal X-ray diffraction (XRD). The co-crystal has been thoroughly characterized by powder XRD, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The pure co-crystal could be synthesized by solvent drop grinding, cooling crystallization and slurry conversion co-crystallization. Ternary phase diagrams have been constructed in methanol and acetonitrile at 30 degrees C. The co-crystal exhibits incongruent dissolution in both solvents. The thermodynamics of co-crystal formation have been estimated from solubility data and calorimetric data, respectively, showing that formation of the SMT-3mSA co-crystal from its solid components is spontaneous and entropy-driven. The co-crystal formation is associated with a 5% increase in molecular volume. A relationship between the size of the region where the co-crystal is the most stable solid phase and the relative solubility of the co-crystal components has been uncovered. The co-crystal region becomes smaller as the solubility ratio increases.
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| 3. |
- Ashour, Radwa, et al.
(författare)
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DTPA-Functionalized Silica Nano- and Microparticles for Adsorption and Chromatographic Separation of Rare Earth Elements
- 2018
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Ingår i: ACS Sustainable Chemistry and Engineering. - : American Chemical Society (ACS). - 2168-0485. ; 6:5, s. 6889-6900
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Tidskriftsartikel (refereegranskat)abstract
- Silica nanoparticles and porous microparticles have been successfully functionalized with a monolayer of DTPA-derived ligands. The ligand grafting is chemically robust and does not appreciably influence the morphology or the structure of the material. The produced particles exhibit quick kinetics and high capacity for REE adsorption. The feasibility of using the DTPA-functionalized microparticles for chromatographic separation of rare earth elements has been investigated for different sample concentrations, elution modes, eluent concentrations, eluent flow rates, and column temperatures. Good separation of the La(III), Ce(III), Pr(III), Nd(III), and Dy(III) ions was achieved using HNO3 as eluent using a linear concentration gradient from 0 to 0.15 M over 55 min. The long-term performance of the functionalized column has been verified, with very little deterioration recorded over more than 50 experiments. The results of this study demonstrate the potential for using DTPA-functionalized silica particles in a chromatographic process for separating these valuable elements from waste sources, as an environmentally preferable alternative to standard solvent-intensive processes.
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| 4. |
- Cheuk, Dominic, et al.
(författare)
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Thermodynamics of the Enantiotropic Pharmaceutical Compound Benzocaine and Solubility in Pure Organic Solvents
- 2020
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Ingår i: Journal of Pharmaceutical Sciences. - : Elsevier BV. - 0022-3549 .- 1520-6017. ; 109:11, s. 3370-3377
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Tidskriftsartikel (refereegranskat)abstract
- The thermodynamic relationship between FI and FII of ethyl 4-aminobenzoate (benzocaine) has been investigated. Slurry conversion experiments show that the transition temperature below which FI is stable is located between 302 K-303 K (29 degrees C-30 degrees C). The polymorphs FI and FII have been characterised by infrared spectroscopy (IR), Raman spectroscopy, transmission powder X-ray diffraction (XRPD) and differential scanning calorimetry (DSC). The isobaric solid state heat capacities have been measured by DSC. The quantitative thermodynamic stability relationship has been determined in a comprehensive thermodynamic analysis of the calorimetric data. The solubility of both polymorphs has been determined in eight pure organic solvents over the temperature range 278 K-323 K by a gravimetric method. The mole fraction solubility of benzocaine decreases in the order: 1,4-dioxane, acetone, ethyl acetate, chloroform, acetonitrile, methanol, n-butanol and toluene. Comparison with the determined activity of solid benzocaine forms shows that negative deviation from Raoult's law ideality is found in dioxane, acetone and ethyl acetate solutions, and positive deviation in solutions of the other investigated solvents.
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| 5. |
- Crutzen, Jordan, et al.
(författare)
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Mesoscale clusters in multicomponent systems: the effect of solution preparation and pre-treatment on primary nucleation of a carbamazepine-saccharin cocrystal
- 2023
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Ingår i: CrystEngComm. - : Royal Society of Chemistry. - 1466-8033. ; 25:28, s. 4048-4057
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Tidskriftsartikel (refereegranskat)abstract
- In this work, direct investigation of mesoscale clusters in solution using dynamic light scattering is combined with an indirect method based on the study of primary crystal nucleation and its dependence on the conditions of solution preparation and pre-treatment. In a novel approach we have studied how the nucleation induction time of a pharmaceutical cocrystal, a 1 : 1 saccharin-carbamazepine cocrystal, depends on different preparation and pre-treatment conditions, in particular whether solutions are prepared by dissolving the cocrystal solids or the two coformers separately. Nucleation is clearly affected by some pre-treatment conditions, with longer induction times obtained for a high pre-treatment temperature and when solutions are microfiltered after dissolution. The strongest effect was observed when comparing different starting materials, with solutions prepared using cocrystals leading to much shorter induction times than solutions based on the separate coformers. DLS shows that both types of solutions contain mesoscale clusters of the order of 100-300 nm in size, but that there are clear differences in the amount of scattering indicating a higher cluster concentration in the solutions based on cocrystal solids. The results suggest the possibility that mesoscale clusters can have a structural dimension, associated with slow kinetics, which can directly affect nucleation.
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| 7. |
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| 8. |
- Diniz, Mariana O., et al.
(författare)
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New Solid Forms of Griseofulvin : A Solvate and a Relict Polymorph Related to Reported Solvates
- 2023
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Ingår i: Crystal Growth & Design. - : American Chemical Society (ACS). - 1528-7483 .- 1528-7505. ; 23:12, s. 8953-8961
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Tidskriftsartikel (refereegranskat)abstract
- This work presents two new solid forms, a polymorph and a solvate, of the antifungal active pharmaceutical ingredient griseofulvin (GSF). The novel forms were characterized by powder X-ray diffraction, differential scanning calorimetry, and thermogravimetric analysis, and their crystal structures were determined by single-crystal X-ray diffraction. The new polymorphic form (GSF Form VI) was obtained upon drying at room temperature the GSF-acetonitrile solvate. GSF Form VI is a relict structure related to reported solvates of GSF. Thermal stability studies show that Form VI is metastable and monotropically related to the stable GSF Form I. The new GSF-n-butyl acetate solvate was obtained by crystallization from an n-butyl acetate solution. The stoichiometry of the n-butyl acetate solvate is 1:0.5. The solvate loses the solvent from the crystal lattice at a temperature between 363.15 and 374.15 K.
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