JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2017
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IF 3.255
Wen-Peng Zhang,Dong-Ying Chen
The purpose of this work was to investigate the crystal structures and physicochemical properties of amisulpride polymorphs. Except of the previously reported polymorph (named as Form I), a new polymorphic form (named as Form II) was discovered through comprehensive solid-state screening experiments. Both polymorphic forms were characterized by single crystal X-ray structure analysis (SXRD), powder X-ray diffraction (PXRD), dynamic vapor sorption (DVS) and thermal analysis (TGA and DSC) as well. It has been found that the Forms I and II are of conformational polymorph with the main conformational difference around ethylsulfonyl group. Form II possesses lower hygroscopicity and better solubility compared with that of Form I, indicating Form II could be an alternate solid form for formulation development.
研究领域:
药学
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材料科学
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药物化学
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产品关联
DOI
PubMed
高影响因子
PHYSICS LETTERS A
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2024
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IF 2.3
Ting-ting Yan,Ran Jiang,Dong-yang Xi,Long Ma,Dan-dan Zhang,Yi-fei Xu
This study investigated the structural stability of 1-methylhydantoin (1-MH, C 4 H 6 N 2 O 2 ) Form-I at room temperature using Raman spectroscopy and a diamond anvil cell (DAC) for high-pressure experiments. Two phase transitions were identified at pressures of 0.6–1.7 GPa and 3.4–6.7 GPa. After complete release of pressure, the spectrum aligned with the Raman spectrum at ambient pressure, indicating reversibility of the phase transition. Analysis of Hirshfeld surface energy and fingerprints was conducted to assess changes in intermolecular interactions, revealing that the phase transitions are associated with rearrangements in the hydrogen-bonded network.
研究领域:
物理化学
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材料科学
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DOI
高影响因子
CRYSTAL GROWTH & DESIGN
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2024
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IF 3.2
Shuhong Song,Lei Wang,Yaqian Qu,Huimin Li,Hongshuai Wang,Peizhuo Han,Zeliang Gao,Xutang Tao
The crystal growth mechanism of form I (AZ-I) of the antihypertensive drug azilsartan is revealed by in situ atomic force microscopy (AFM). On the dominant (100) face, AZ-I grows by a classical spiral growth mechanism. The growth spiral is asymmetric due to the different step kinetics in different crystallographic directions. The normal growth rate of the (100) face is inferred to be much lower than the step velocity within this face according to the step geometry, resulting in the plate-like crystal morphology. The dependence of step velocity on terrace width indicates that molecules incorporate into steps primarily by a surface diffusion mechanism involving molecular adsorption on terraces at first and then diffusion into steps. Within the (100) face, steps in different directions exhibit different step edge free energies and total minimal energies for step advancement. The step kinetics depends on the step length within a certain range. These findings provide a fundamental understanding of drug crystal growth at the microscale.
研究领域:
药物结晶学
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材料科学
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纳米成像
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药物研发
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物理化学
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DOI
高影响因子
JOURNAL OF CHEMICAL THERMODYNAMICS
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2021
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IF 3.178
Rongguan Lv,Xuehua Zhang,Rong Xing,Weizhong Shi,Hongkun Zhao,Wanxin Li,Abolghasem Jouyban,William E. Acree
The intermolecular interactions and overall charge distribution of curcumin were respectively investigated by using Hirshfeld surface analysis and molecular electrostatic potential surface. The mole fraction solubility magnitudes of curcumin (I) in aprotic co-solvent blends of DMSO + water, acetone + water and acetonitrile + water ranging from 278.15 to 318.15 (333.15) K under 101.1 kPa was obtained by means of shake-flask method. Under the same conditions, e.g. identical temperature and mass fraction of DMSO (acetone or acetonitrile), the equilibrium solubility of curcumin was greater in DMSO + water blends than in acetone/acetonitrile + water blends. The lowest solubility magnitude was found in neat water at 278.15 K; and the highest one, in acetone/acetonitrile at temperature of T = 318.15 K (aqueous solutions of acetone or acetonitrile) or 333.15 K (aqueous solutions of DMSO). No crystal transition and solvate formation occurred in experimental processes as documented through X-ray power diffraction analysis. The acquired data were correlated by means of the Jouyban-Acree model, Apelblat model and modified van’t Hoff-Jouyban–Acree model. The preferential solvation at 298.15 K was investigated by the approach of inverse Kirkwood–Buff integrals. The parameters of preferential solvation for DMSO, acetone or acetonitrile were positive in the above three blends with middle and DMSO/acetone/acetonitrile-rich composition ranges, which specified that preferential solvation of curcumin was made by co-solvent. The extended Hildebrand solubility approach was further employed to describe the mole fraction solubility at 298.15 K in DMSO/acetone/acetonitrile + water blends studied in the current work and in ethanol/ n -propanol/isopropanol/PG + water blends reported previous by us, obtaining average relative deviations < 5.21%.
研究领域:
药理学
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化学
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药物化学
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产品关联
DOI
高影响因子
JOURNAL OF CHEMICAL AND ENGINEERING DATA
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2022
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IF 3.119
Li Chen,Lingbin Shen,Yuhang Chen,Zhengyang Luo,Zexin Ren,Rongrong Li,Cunbin Du
The solubility data of nimesulide (form I) in different mono- and mixed solvents over the temperature range from 273.15 to 318.15 K are determined. In this work, it is further studied to improve the solubility data of nimesulide (form I) and analyze the intermolecular force. The solubility profiles in mono- and mixed solvents are correlated by some thermodynamic models. The results of statistical analysis show that all selected models could provide a good correlation of the dissolution profile for nimesulide in selected solvents at all investigated temperatures. At 318.15 K, the largest solubility in mole fraction is obtained in acetone (7.812 × 10–2), followed by 2-butanone (6.334 × 10–2), cyclohexanone (4.977 × 10–2), ethyl acetate (3.803 × 10–2), tetrahydrofuran (3.651 × 10–2), acetonitrile (2.975 × 10–2), ethanol (2.169 × 10–3), toluene (1.788 × 10–3), isobutanol (1.348 × 10–3), isopropanol (1.201 × 10–3), and propylene glycol (PG, 6.764 × 10–4). However, in mixtures of (ethyl acetate + isopropanol), the solubility data increase with the increase of the mass fraction of ethyl acetate at a given temperature. The effect of solute–solvent interactions on the solid–liquid phase equilibrium of the solute is discussed with the solvent properties. The calculation of preferential solvation parameters shows that solute molecules are preferentially solvated by isopropanol in isopropanol-rich regions and as the mass fraction of ethyl acetate increases, nimesulide is preferentially solvated by ethyl acetate. Studying the dissolution process of nimesulide is of great practical significance for its purification.
研究领域:
药学
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物理化学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHEMICAL AND ENGINEERING DATA
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2026
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IF 2.4
Lihong Jia,Zixiang He,Hanchang Huang,Xing Fan,Yuan Sui,Yongping Han
The solubility of meglumine Form I was systematically determined in 12 pure solvents (methanol, ethanol, n-propanol, isopropanol, n-butanol, ethyl formate, methyl acetate, ethyl acetate, tetrahydrofuran, 1,4-dioxane, N,N-dimethylformamide (DMF), and acetonitrile) using a gravimetric method over the temperature range of 288.15 to 328.15 K. Solubility increased with temperature in all systems, with DMF exhibiting the highest solubility and acetonitrile the lowest. Three thermodynamic models (the modified Apelblat, λh, and van’t Hoff) were employed to correlate the solubility data, among which the modified Apelblat model provided the best fit. The solubility behavior of meglumine Form I was further analyzed using Hirshfeld surface analysis, the Kamlet–Abboud–Taft linear solvation energy relationship (KAT-LSER) model. The results demonstrate that the solvent’s hydrogen-bond acceptor capability is the key determinant of solubility, as it generates sufficiently strong solute–solvent interactions to overcome the robust hydrogen-bond network within the crystal lattice. These findings provide essential thermodynamic data and mechanistic insights for the optimization of meglumine crystallization and formulation processes.
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DOI
高影响因子
JOURNAL OF CHEMICAL AND ENGINEERING DATA
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2024
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IF 2
Xiaofang Luo,Yuntian Xiao,Linlin Shi,Lingli Hou,Yongkang Liu,Ling Zhou,Qiuxiang Yin
Prednisolone (PDL), a corticosteroid extensively used in the treatment of allergic and autoimmune inflammatory diseases, faces limitations in clinical application due to its poor water solubility. Consequently, grasping the solid–liquid equilibrium behavior across diverse solvents is imperative for advancing the development of solid formulations with improved bioavailability. This study measured the solubility of PDL Form I in 13 pure solvents using gravimetric analysis and employed molecular dynamics, including molecular electrostatic potential surface analysis, Hirshfeld surface analysis, the independent gradient model based on Hirshfeld partitioning, radial distribution function, and solute–solvent interaction energy calculations, to explore the solid–liquid equilibrium behavior. The solubility of PDL Form I across various solvents exhibited a temperature-dependent increase, showing the largest variation in acetone. Radial distribution function analysis indicated multiple hydrogen-bonding interactions between the PDL molecule and the solvents tested. The calculations of solute–solvent interaction energy revealed that ethanol had the highest interaction energy with PDL, correlating with its the highest solubility. The validity of the solid–liquid equilibrium data was confirmed by fitting to the Apelblat equation, λh model, van’t Hoff equation, and NRTL equation, with an average relative deviation below 2.5, indicating good correlation.
研究领域:
药学
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生物物理学
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化学工程
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产品关联
DOI
高影响因子
JOURNAL OF MOLECULAR LIQUIDS
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2022
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IF 6.633
Pengshuai Zhang,Haiyan Luo,Lan Cui,Jixiu Deng,Shiyu Xie,Danfeng Liu,Shuqi Wang,Xiaoying Si,Zichao Wang,Yameng Wan,En Zhang,Xing Li,Lu Zhang
Solid-liquid equilibrium solubility of artemisinin (ART) Form I in twelve mono-solvents namely N, N-dimethylformamide (DMF), oxolane (THF), n -propanol (NPA), 4-methylpentan-2-one (MIBK), ethyl formate (EF), butyl acetate (BAC), 2-ethoxyethanol (EGEE), 1,4-Dioxane, 2-methoxyethanol (EGME), 2-propoxyethanol (EGPE), propyl acetate (NPAC) and 2-butoxyethanol (EGBE) from 283.15 K to 323.15 K were determined by a laser dynamic method under 0.1 MPa. The minimum solubility of ART (Form I) was found in NPA at 283.15 K (0.004541), the maximum mole fraction solubility of ART (Form I) was observed as 0.2523 in DMF at 323.15 K. At the temperature of 298.15 K, the experimental mole fraction solubility order of ART Form I in the tested solvents was DMF (0.1559) > 1,4-Dioxane (0.09117) > THF (0.08301) > MIBK (0.05054) > EF (0.04902) > NPAC (0.03860) > BAC (0.03658) > EGME (0.02031) > EGEE (0.01859) > EGPE (0.01817) > EGBE (0.01689) > NPA (0.007185). The solubility behavior was computationally correlated by Margules model, Wilson model, NRTL model, NRTL-SAC model, Buchowski-Ksiazczak λh model and UNIQUAC model, the total RMSD was no>0.025 in the selected models. With the help of Hansen solubility parameters (HSPs) analysis, molecular similarities of ART (Form I) in twelve mono-solvents were investigated. Besides, Hirschfeld surface analysis (HSs) was considered to evaluate the intermolecular interaction of artemisinin. Moreover, thermodynamic properties including Δ mix H , Δ mix G , Δ mix S , lnγ 1 , l n γ 1 ∞ of ART (Form I) in the selected solvents were estimated. All the negative Δ mix G and positive Δ mix S values indicated that the mixing process were spontaneous and entropy-increasing.
研究领域:
药学
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物理化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF MOLECULAR LIQUIDS
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2021
·
IF 6.165
Fengxin Guo,Qiong Liu,Jiao Sha,Zidan Cao,Yuanhui Chong,Yu Li,Tao Li,Baozeng Ren
The solubility of amitriptyline hydrochloride (AMT) (Form I) in fourteen mono-solvents, including {methanol, 2-methoxyethanol, ethanol, 2-ethoxyethanol, n-propanol, 2-propoxyethanol, n-butanol, 2-butoxyethanol, n-octanol, n-hexanol, n-heptanol, n-pentanol, N-Methyl pyrrolidone (NMP), N,N-Dimethylformamide (DMF)} was determined under 0.1 MPa from 278.15 K to 323.15 K by laser detection method. The experimental results showed that as the temperature increasing, the solubility of AMT (Form I) gradually increased. The order of solubility of AMT (Form I) in fourteen mono-solvents at 298.15 K was: methanol (0.1753) > 2-methoxyethanol (0.1488) > 2-ethoxyethanol (0.1082) > 2-propoxyethanol (0.08140) > ethanol (0.07940) > 2-butoxyethanol (0.06600) > n-propanol (0.05720) > NMP (0.04480) > DMF (0.04230) > n-butanol (0.04050) > n-pentanol (0.03210) > n-hexanol (0.02700) > n-heptanol (0.02250) > n-octanol (0.004700). In addition, the Hansen solubility parameter (HSP) was applied to further discuss the miscibility of AMT (Form I) in the studied solvents. Molecular dynamics simulation explored the intermolecular interaction between solute and solvents. And the solvent effect of AMT (Form I) in the tested pure solvents was explained by the KAT-LSER model. The basic data of experimental solubility of AMT (Form I) were correlated with five thermodynamic models, including NRTL, λh, modified Apelblat, NRTL-SAC and two-Suffix Margules. Furthermore, the van't Hoff equation was applied to calculate the dissolution thermodynamic properties of AMT (Form I) in all tested solvents, including Δ dis H o , Δ dis S o and Δ dis G o .
研究领域:
药学
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物理化学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHEMICAL AND ENGINEERING DATA
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2020
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IF 2.369
Yanbo Liu,Mingyang Chen,Jiawei Lin,Maolin Li,Kang Li,Zhenguo Gao
Experimental solubility data of clopidogrel hydrogen sulfate (form I) in four binary solvents (1-propanol + isopropyl acetate, 2-propanol + isopropyl acetate, 1-butanol + isopropyl acetate, and 2-butanol + isopropyl acetate) was measured by using the laser dynamic method at the temperature ranging from 278.15 to 318.15 K. The experimental results showed that the solubility of clopidogrel hydrogen sulfate (form I) increased with the increasing temperature of all four binary solvent systems at the constant solvent composition, and the isopropyl acetate had a negative effect on the solubilities. The solubilities of clopidogrel hydrogen sulfate (form I) were correlated by the modified Apelblat, λh, and NRTL equations. The results indicated that the three models can predict the experimental values satisfactorily. Moreover, the modified Apelblat equation achieves the best fitting performance compared with other two models through calculating the value of average relative deviation.
研究领域:
药物化学
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物理化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF MOLECULAR LIQUIDS
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2021
·
IF 6.165
Jiao Sha,Di Fan,Jingyi Zhang,Zidan Cao,Yameng Wan,Renren Sun,Haixia He,Gaoliang Jiang,Yu Li,Tao Li,Baozeng Ren
The equilibrium solubility of nimesulide (NIMS) in twelve single solvents was accurately measured by a laser monitoring method. It was indicated that the positive impact of experimental temperature on the solubility data of NIMS (Form I) in twelve mono-solvents within the investigated temperature range of 278.15–323.15 K under 101.3 KPa. The solubility shows a clear non-linear trend and decreased in the order methyl acetate > ethyl acetate >2-methoxyethanol > n-propyl acetate > n-butyl acetate >2-ethoxyethanol >2-propoxyethanol >2-butoxyethanol > methanol > ethanol > n-propanol > n-butanol. NIMS (Form I) has the highest solubility ( x 1 = 5.223e-2) in methyl acetate at 323.15 K and the smallest solubility ( x 1 = 6.800e-6) in n-butanol at 278.15 K. And then, the solvent polarity, radial distribution function obtained from molecular dynamic simulation and solvent effect (KAT-LSER model) were implemented to investigate the effect of solute-solvent interactions on solid-liquid phase equilibrium of NIMS (Form I). The results demonstrated that the whole dissolution behavior of NIMS (Form I) in organic solvents was a complicated process, and the solvent-solute interactions are mainly affected by the dipolarity/polarizability. Moreover, five widely used activity coefficient models including NRTL, NRTL-SAC, Wilson, Two-Suffix Margules, and UNIQUAC models had been fitted to experimental solubility data. Deviation analysis reveals that the UNIQUAC model reflects the best agreement between the measured data and calculated values, with the minimum mean values of 100ARD (0.89) and RMSD (1.22e-4). Finally, the thermodynamic parameters (Δ dis G o , Δ dis H o , Δ dis S o , ζ H and ζ TS ) of NIMS (Form I) dissolution process in investigated 12 single solvents were evaluated based on the van't Hoff equation. The positive Δ dis G o , Δ dis H o and Δ dis S o indicate that the dissolution process of NIMS (Form I) is an entropy-driven non-spontaneous endothermic process in all chosen single solvents, and the ζ H is the main contributor of Δ dis G o .
研究领域:
药学
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物理化学
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热力学
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分子动力学
✓ 已验证
DOI
高影响因子
JOURNAL OF MOLECULAR LIQUIDS
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2022
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IF 6.633
Yuanhui Chong,Qiong Liu,Zeqi Wang,Liukai Zhu,Fengxin Guo,Yu Li,Tao Li,Baozeng Ren
Perphenazine has rather effective in the treatment of mental illness. In this work, the solid-liquid equilibrium data of perphenazine in eleven organic neat solvents were determined by laser dynamic method under the atmospheric pressure and temperature range of 278.15 K ∼ 318.15 K. The selected solvents were n-propanol, n-butyl alcohol, methyl acetate, ethyl acetate, n-propyl acetate, n-amyl acetate, N, N-dimethylformamide (DMF), N, N-dimethylacetamide (DMAC), acetone, 2-methoxyethanol, glycol ether, respectively. From the results, the solubility of perphenazine is all positively correlated with temperature. Separately, we have adopted the KAT-LSER model and molecular dynamics simulation to investigate the influence of solvent effects and solute-solvent interaction on solute solubility. Meanwhile, there were four activity coefficient models being used to correlate the solubility data and Average relative deviation of models are 4.13% (Margules model), 3.94% (NRTL model), 4.49% (NRTL-SAC model) and 3.06% (UNIQUAC model), respectively, all of which do not exceed 5%. It manifests that the four activity coefficient models can fit the experimental values well, in which the UNIQUAC model gives the best regression effect. Moreover, the apparent thermodynamic properties( △ sol G° , △ sol H° and △ sol S° ) of perphenazine in various solvents were calculated by Van’t Hoff equation. In accordance with the analysis and calculation of dissolution, the dissolution process is an endothermic entropy-driven process. This research can provide basic data for the crystallization process of perphenazine.
研究领域:
药学
·
物理化学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）