Screening For Solid Forms By Ultrasound Crystallization And Cocrystallization Using Ultrasound

a technology of cocrystallization and ultrasound, which is applied in the direction of glucose production, separation processes, instruments, etc., can solve the problems of reducing or eliminating the utility or beneficial purpose, reducing or eliminating the utility of the effect, and pharmaceutical industry spending a great deal of time, effort and expense on the identification of particular compounds

Inactive Publication Date: 2007-12-13
AMRI SSCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0045] The present methods may be used to form at least one new solid state phase of an active agent, including new solid state phase

Problems solved by technology

Chemical substances (compounds, elements, and mixtures) have properties which tend to be unpredictable and variable.
Certain chemical substances may have utility for numerous different applications, including vital biological applications, yet a slight change may reduce or eliminate the utility or benef

Method used

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  • Screening For Solid Forms By Ultrasound Crystallization And Cocrystallization Using Ultrasound
  • Screening For Solid Forms By Ultrasound Crystallization And Cocrystallization Using Ultrasound
  • Screening For Solid Forms By Ultrasound Crystallization And Cocrystallization Using Ultrasound

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0324] In this Example, a new solid form of sulfathiazole was prepared from solution in acetonitrile using sonication. This form was not seen without sonication under the same conditions. Form II of sulfathiazole was generated without sonication.

[0325] A saturated solution of sulfathiazole in acetonitrile at 45° C. was prepared, filtered hot and split between two pre-heated 1-dram vials (about 1 ml each). The samples were left to slowly cool to room temperature. One sample was then nucleated by ultrasound treatment using 5 pulses of one second each at 20 kHz, amplitude control set at 40, using a Cole Palmer ultrasonic processor CP130 fitted with a 6 mm tip stainless steel probe, while the other sample was left undisturbed (unsonicated). Both samples were then left to evaporate slowly to dryness. XRPD patterns of the sonicated and unsonicated samples showed that the sonicated sample gave an unknown pattern (FIG. 1) whereas the unsonicated sample yielded the known Form II of sulfathi...

example 2

[0326] In this Example, an unusual solid form of an acetone solvate of sulfathiazole was prepared. Without sonication, this form was only seen in a mixture with the known form of an acetone solvate of sulfathiazole.

[0327] A saturated solution of sulfathiazole in acetone at 45° C. was prepared, filtered hot and split between two pre-heated 1-dram vials (about 1 ml each). The samples were left to slowly cool to room temperature. One sample was then nucleated by ultrasound treatment using 5 pulses of one second each at 20 kHz, amplitude control set at 40, using a Cole Palmer ultrasonic processor CP130 fitted with a 6 mm tip stainless steel probe, while the other sample was left undisturbed (unsonicated). Both samples were then left to evaporate slowly to dryness. XRPD patterns of the sonicated and unsonicated patterns showed that the sonicated sample gave an unknown pattern (FIG. 3) whereas the unsonicated sample yielded a mixture of this same form with the known acetone solvate of su...

example 3

[0328] In this Example, a new DMSO solvate of carbamazepine was prepared.

[0329] Three 100 μl samples of a saturated solution of carbamazepine in DMSO at 50° C. were placed in 3 pre-heated HPLC vials. The samples were allowed to cool to ambient temperature. One sample was nucleated by ultrasound treatment (5 one-second pulses, 20 kHz, amplitude control set at 40, using the Cole Palmer ultrasonic processor with a 3 mm tip stainless steel probe), while another was stirred using a stir bar and the other was left undisturbed (unsonicated). While the sonicated sample yielded a new DMSO solvate, the other samples remained as solutions indefinitely. The XRPD pattern of the new DMSO solvate is shown in FIG. 5.

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Abstract

The present disclosure relates to crystallizing a chemical substance(s) using ultrasound. Methods are provided for screening a chemical substance according to its solid forms by using ultrasound to generate new or unusual solid forms. Methods are also provided for crystallizing a chemical substance by novel techniques that include sonication. The present disclosure also relates to cocrystallization using ultrasound. Methods are provided for preparing cocrystals of an active agent and a guest by sonicating and crystallizing. Methods are also provided for screening a sample according to solid state phases (such as cocrystals and salts) and include generating a cocrystal from the sample using ultrasound.

Description

FIELD OF THE INVENTION [0001] The present disclosure relates to crystallizing a chemical substance using ultrasound. Methods are provided for screening a chemical substance according to its solid forms by using ultrasound to generate new or unusual solid forms. Methods are also provided for crystallizing a chemical substance by novel techniques that include sonication. The present disclosure also relates to cocrystallization using ultrasound. Methods are provided for preparing cocrystals of an active agent and a guest by sonicating and crystallizing. Methods are also provided for screening a sample according to solid state phases (such as cocrystals and salts) and include generating a cocrystal from the sample using ultrasound. BACKGROUND OF THE INVENTION [0002] Chemical substances (compounds, elements, and mixtures) have properties which tend to be unpredictable and variable. Certain chemical substances may have utility for numerous different applications, including vital biologica...

Claims

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Application Information

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IPC IPC(8): G01N1/00B01D9/00C30B7/00
CPCB01D9/00B01D9/0077Y10T436/25875C30B7/00C07C217/72
Inventor CHILDS, SCOTT L.MOUGIN-ANDRES, PATRICIA M.STAHLY, BARBARA C.
Owner AMRI SSCI
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