Simple multipurpose apparatus for solubility measurement of solid solutes in liquids

Malwade, Chandrakant Ramkrishna; Christensen, Lars Porskjær

doi:10.1016/j.ece.2016.06.003

Cited by 6 publications

(6 citation statements)

References 26 publications

(17 reference statements)

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“…A detailed description of the apparatus used for the measurements is provided by Malwade and Christensen. 24 At the end of the equilibration, the saturated solution was separated from the excess solid phase with a syringe and 0.2 μm PTFE filters, appropriately diluted, and analyzed by highperformance liquid chromatography (HPLC) to determine the concentration of IMC. The solid phase was analyzed by XRPD to ascertain any possible phase change during the solubility measurement.…”

Section: Methodsmentioning

confidence: 99%

“…Sealed vials were maintained at constant temperature under magnetic stirring for 24 h to attain equilibrium. A detailed description of the apparatus used for the measurements is provided by Malwade and Christensen . At the end of the equilibration, the saturated solution was separated from the excess solid phase with a syringe and 0.2 μm PTFE filters, appropriately diluted, and analyzed by high-performance liquid chromatography (HPLC) to determine the concentration of IMC.…”

Section: Materials and Methodsmentioning

confidence: 99%

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Cooling Crystallization of Indomethacin: Effect of Supersaturation, Temperature, and Seeding on Polymorphism and Crystal Size Distribution

Malwade

2018

Org. Process Res. Dev.

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In this work, the effect of crystallization parameters, i.e., supersaturation, seeding, and temperature, on the polymorphism and crystal size of a nonsteroidal anti-inflammatory drug, indomethacin (IMC), was investigated. First, several crystallization solvents (ethanol, methanol, ethyl acetate, acetone, acetonitrile, and dichloromethane) were screened through the measurement of IMC solubility at different temperatures. This was followed by the investigation of IMC nucleation through measurement of induction times in selected solvents at two supersaturations. Finally, seeded cooling crystallization of IMC in ethanol was performed with different process parameters to investigate the influence on the polymorphism and crystal size distribution. Remarkably long induction times were observed for IMC in ethanol and ethyl acetate solutions, while a shorter induction time was observed in acetone. Cooling crystallization of IMC from ethanol confirmed that supersaturation, operating temperature, and seeding do affect the polymorphism as well as crystal size distribution of IMC. Fine needle-shaped crystals of metastable α-IMC were obtained at 5 °C with high supersaturation even in the presence of γ-IMC seeds, while rhombic platelike crystals of thermodynamically stable γ-IMC were obtained in the remaining experiments. The seed loading only marginally influenced the crystal growth rate and median particle diameter. Particle size analysis of the crystals obtained showed a bimodal distribution in all experiments, and a larger median particle diameter was observed at 15 °C with high supersaturation.

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Section: Methodsmentioning

confidence: 99%

Section: Materials and Methodsmentioning

confidence: 99%

Cooling Crystallization of Indomethacin: Effect of Supersaturation, Temperature, and Seeding on Polymorphism and Crystal Size Distribution

Malwade

2018

Org. Process Res. Dev.

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show abstract

“…Sealed vials were maintained at constant temperature under magnetic stirring for 24 h to attain equilibrium. A detailed description of the apparatus used for the measurements is provided by Malwade and Christensen . At the end of the equilibrium, the saturated solution was separated from the excess solid phase with a syringe and 0.2 μm PTFE filters, appropriately diluted, and analyzed by high pressure liquid chromatography (HPLC) to determine the concentration of IMC.…”

Section: Materials and Methodsmentioning

confidence: 99%

“…A detailed description of the apparatus used for the measurements is provided by Malwade and Christensen. 25 At the end of the equilibrium, the saturated solution was separated from the excess solid phase with a syringe and 0.2 μm PTFE filters, appropriately diluted, and analyzed by high pressure liquid chromatography (HPLC) to determine the concentration of IMC. A Dionex UltiMate 3000 HPLC system equipped with a ZORBAX Eclipse XDB-C18 reverse-phase column (dimensions 150 × 4.6 mm 2 , particle size 5 μm, Phenomenex, Denmark) maintained at 35 °C and a diode array detector (DAD-3000) were used for the analysis of samples.…”

Section: Methodsmentioning

confidence: 99%

Antisolvent Crystallization of Indomethacin from a Ternary Solvent System with High Productivity, Better Polymorphism, and Particle Size Control

Malwade

2019

Org. Process Res. Dev.

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Antisolvent crystallization of Indomethacin (IMC), a nonsteroidal anti-inflammatory drug, from a ternary solvent system (acetone-methanol-water) has been investigated in this work. Acetonemethanol (66.5-33.5 wt%) binary mixture was selected as a solvent based on the solubility of IMC reported earlier. Water was selected as an antisolvent based on the solubility of IMC measured in acetone-methanol-water mixtures at 25 °C. Unseeded and seeded antisolvent crystallization was carried out for two initial concentrations of IMC (and) with stepwise addition of 0, 1 0, 2 antisolvent. The acetone solvate of IMC was crystallized during the unseeded experiments, while the desired γ-IMC was obtained with a bimodal particle size distribution (PSD) during the experiments seeded with γ-IMC. A significant increase in the productivity was observed because of increased crystal yield and faster crystallization kinetics as compared to the crystallization processes reported earlier for the production of γ-IMC. Finally, the feasibility of IMC particle size tuning through the solvent-antisolvent (dissolution-growth) addition cycles was demonstrated successfully.

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“…Sample solubility measurement of phenyliodonium diacetate (1) in diethyl ether. Following the procedure and set up from Malwade et al, 35 110 mg of 1 was weighed into an 8 mL vial equipped with a Teflon coated stir bar. Diethyl ether (5.0 mL) was transferred to the vials via a syringe to form a saturated solution of 1 (21 mg/mL) in diethyl ether.…”

Section: General Procedures Amentioning

confidence: 99%

Ligand exchange of aryl iodine dicarboxylates to form reagents with differing solubilities

Seecharan¹,

Armand²,

Noorollah³

et al. 2021

Arkivoc

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Hypervalent iodine (HVI) reagents are employed in organic synthesis as versatile, proficient, and environmentally friendly reagents. Despite the utility of such reagents, the application of HVI reagents, especially phenyliodonium diacetate (PIDA), has been limited due to its poor solubility in a myriad of solvents. The aggregated and polymeric structures of many HVI reagents account for their poor solubility, thus limiting the reactivity and use of HVI reagents in reactions in non-polar solvents. The research presented herein outlines ligand exchange reactions of universal carboxylic acids promoted by phenyliodonium diacetate (PIDA) reagents, in which the acetate moiety of PIDA is modified, ultimately enhancing the solubility and reactivity of HVI reagents.

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Simple multipurpose apparatus for solubility measurement of solid solutes in liquids

Cited by 6 publications

References 26 publications

Cooling Crystallization of Indomethacin: Effect of Supersaturation, Temperature, and Seeding on Polymorphism and Crystal Size Distribution

Cooling Crystallization of Indomethacin: Effect of Supersaturation, Temperature, and Seeding on Polymorphism and Crystal Size Distribution

Antisolvent Crystallization of Indomethacin from a Ternary Solvent System with High Productivity, Better Polymorphism, and Particle Size Control

Ligand exchange of aryl iodine dicarboxylates to form reagents with differing solubilities

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