Methods of screening for possible solid forms

• US 6,750,064 B2
• Filed: 12/28/2000
• Issued: 06/15/2004
• Est. Priority Date: 12/28/2000
• Status: Expired due to Term

• Current Assignee: AMRI Americium, LLC, Purdue Research Foundation (The Trustees of Purdue University (d/b/a Purdue University))
• Original Assignee: SSCI, Inc., Purdue Research Foundation (The Trustees of Purdue University (d/b/a Purdue University))
• Inventors: Coates, David, Morris, Kenneth R., Stahly, G. Patrick, Stahly, Barbara C.
• Primary Examiner(s): Gakh, Yelena G.
• Application Number:
  US09/752,857
• Publication Number:
  US 20030190758A1
• Time in Patent Office: 1,265 Days
• Field of Search: 436/180, 436/181, 436/174, 422/243, 422/245.1, 422/255, 422/258, 422/260
• US Class Current: 436/181
• CPC Class Codes: B01J 2219/00522 in a multiple parallel arrangement
• CPC Class Codes: B01J 2219/00585 Parallel processes
• CPC Class Codes: B01J 2219/00599 Solution-phase processes
• CPC Class Codes: B01J 2219/00702 Processes involving means for analysing and characterising the products
• CPC Class Codes: B01J 2219/00725 Peptides
• CPC Class Codes: B01J 2219/00756 Compositions, e.g. coatings, crystals, formulations
• CPC Class Codes: B01L 3/06 Crystallising dishes
• CPC Class Codes: C30B 7/00 Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions from molten solvents C30B9/00; by normal or gradient freezing C30B11/00; under a protective fluid C30B27/00
• CPC Class Codes: C40B 40/10 Libraries containing peptides or polypeptides, or derivatives thereof
• CPC Class Codes: C40B 50/08 Liquid phase synthesis, i.e. wherein all library building blocks are in liquid phase or in solution during library creation; Particular methods of cleavage from the liquid support
• CPC Class Codes: G01N 25/147 by cristallisation
• CPC Class Codes: Y10T 436/25 including sample preparation
• CPC Class Codes: Y10T 436/2575 Volumetric liquid transfer
• CPC Class Codes: Y10T 436/25875 Gaseous sample or with change of physical state

Abstract

Methods for searching for possible forms of a sample and methods of screening a sample according to its form comprise disposing the sample in at least one receptacle that defines a capillary space, such as a capillary tube. The sample is solidified to generate at least one solid form or semisolid form, and the generated form is analyzed and classified. The analysis may determine differences in molecular arrangement of the various forms or characteristics that reflect the form. The methods may employ a plurality of samples, conditions, or receptacles in an effort to generate a variety of forms, so that all or a high percentage of possible forms are obtained.

Claims

1. A method of screening for a new crystal form of a substance, which comprises

solidifying the substance in one or more capillary spaces each independently having an inside diameter from about 0.1 mm to about 5 mm to produce at least one crystal form of the substance;

analyzing the crystal form of the substance in at least one of the capillary spaces while the substance remains in the capillary space, using at least one technique chosen from microscopic analysis, thermal analysis, diffraction analysis, and spectroscopic analysis; and

classifying the crystal form by comparing the analytical results of the crystal form of the substance to those of a know crystal form or forms of the substance and determining if the crystal form of the substance produced is new.

2. The method of claim 1, wherein the capillary spaces each independently have an inside diameter from about 0.5 mm to about 2.5 mm.

3. The method of claim 1, wherein the one or more capillary spaces form a well plate and wherein the crystal form of the substance is analyzed by transmission X-ray diffraction.

4. The method of claim 3, wherein the capillary spaces each independently have an inside diameter from about 0.5 mm to about 2.5 mm.

5. The method as claimed in claim 1, wherein the substance is solidified by solvent evaporation, cooling, heating, anti-solvent addition, gel diffusion or thin-layer deposition.

6. A method of screening for a new crystal form of a substance, which comprises

solidifying the substance in one or more capillary tubes each independently having an inside diameter from about 0.1 mm to about 5 mm to produce at least one crystal form of the substance,

analyzing the crystal form of the substance in a least one of the capillary tubes using at least one technique chosen from microscopic analysis, thermal analysis, diffraction analysis, and spectroscopic analysis;

and

classifying the crystal form by comparing the analytical results of the crystal form of the substance to those of a known crystal form or forms of the substance and determining if the crystal form of the substance produced is new.

7. The method as claimed in claim 6, wherein the capillary tubes each independently gave an inside diameter from about 0.5 mm to about 2.5 mm.

8. The method as claimed in claim 6, wherein the crystal form of the substance is analyzed by transmission X-ray diffraction.

9. The method as claimed in claim 8, wherein the capillary tubes each independently have an inside diameter from about 0.5 mm to about 2.5 mm.

10. The method as claimed in claim 6, wherein the substance is solidified by solvent evaporation, cooling, heating, anti-solvent addition, gel diffusion or thin layer deposition.