PPXRD-14 Program - Program PDF

 

MONDAY OPTIONAL WORKSHOP
Caloosa Room

Quantitative Phase Analysis by XRPD
9:00 -5:30
Organizer & Instructors: A. Kern, Bruker AXS GmbH, Karlsruhe, Germany, arnt.kern@bruker.com
F. Gozzo, Excelsus Structural Solutions SPRL, Brussels, Belgium, fabia.gozzo@excels.us
M. Reinle-Schmitt, Paul Scherrer Institut, Swiss Light Source, Villigen, Switzerland, mathilde.reinle-schmitt@psi.ch

This workshop will discuss the basis of quantitative phase analysis (QPA) for both single peak and whole pattern approaches. The focus will be on how to select and apply these methods, particularly in the context of the derivation of absolute phase abundances. The presence of poorly crystalline or amorphous content requires extension of the basic methods, but once these are established, they can be shown to produce QPA to the similar lower limits of detection and accuracy as for crystalline phases.

 

Time

Activity

Speaker

Quantitative Phase Analysis by XRPD
Methodology

9:00 - 10:30

QPA of crystalline and amorphous phase abundance: Basis and methods

F. Gozzo

10:30 - 11:00

Coffee Break

 

11:00 - 12:30

Practical assessment of merits of methods for QPA

A. Kern

12:30 - 2:00

Lunch

 

Quantitative Phase Analysis by XRPD
Towards one weight percent accuracy

2:00 - 2:45

Issues in QPA - minimising systematic errors

A. Kern

2:45 - 3:30

Challenges of absolute quantification of pharmaceuticals by the internal standard methods

M. Reinle-Schmitt

3:30 - 4:00

Coffee Break

 

4:00 - 5:00

Instrumentation and sample presentation:

  • Laboratory

  • Synchrotron

A. Kern
F. Gozzo

5:00 - 5:30

Discussion

 

 

TUESDAY SESSIONS
Caloosa Room

*Indicates Presenter

8:30   Welcoming Remarks from PPXRD-14 Organizing Committee Chairman
T. Blanton, International Centre for Diffraction Data, Newtown Square, PA, USA
 
New Frontiers in XRD for Pharmaceutical R&D
Chair: D. Beckers, PANalytical, Almelo, The Netherlands, detlef.beckers@panalytical.com
9:00  P34 Invited - Characterization of Spatial Phase Heterogeneity in Tablets by X-ray Diffractometry
R. Suryanarayanan*, S. Koranne, University of Minnesota, Minneapolis, MN, USA
9:45 P4 Invited - Instrumentation and Applications of 2D XRD for Pharmaceutics
B.B. He*, Bruker AXS, Madison, WI, USA
10:30    Break
11:00 P6 Large-Area CdTe Pixel Detectors for High-Energy X-ray Diffraction Applications
D. Sisak Jung*, T. Donath, DECTRIS Ltd., Switzerland
J. Bednarcik, Deutsches Elektronen-Synchrotron, Germany
M. Di Michiel, European Synchrotron Radiation Facility, France
S. Jacques, School of Materials, University of Manchester, UK
11:30 P52 Crystal Structure Determination from Beam Sensitive Organic Materials using Electron Diffraction
P.P. Das*, S. Nikolopoulos, NanoMEGAS SPRL, Brussels, Belgium
12:00   Lunch (attendees are on their own for lunch)
 
Patent Issues
Chair: T. Blanton, International Centre for Diffraction Data, Newtown Square, PA, USA, tblanton@icdd.com
1:30  P22 Invited – Using X-ray Powder Diffraction and Other Solid-State Data to Protect Pharmaceutical Inventions
E.H. Barash*, Barash Law LLC, Lafayette, IN, USA
 
PXRD Techniques/Rietveld Refinement/Crystal Structure Prediction/Crystal Structure Verification
Chair: R. Suryanarayanan, University of Minnesota, Minneapolis, MN, USA
2:30 P7 Invited - Crystal Structures of Large-Volume Commercial Pharmaceuticals
J. Kaduk*, Illinois Institute of Technology, Chicago, IL and North Central College, Naperville IL, USA
3:15   Break
3:45 P14 Invited – Transmission Non-ambient X-ray Powder Diffraction as a Means to Study Liquid-solid Transformations
S. Bates*, Triclinic Labs, Lafayette, IN, USA
4:30 P15 Humidity Induced Phase Transitions in HEWLYSOZYME Investigated By Microcrystalline Powder Diffraction
D. Beckers*, T. Degen, G. Nénert, PANalytical B.V., Almelo, The Netherlands
S. Saslis, S. Logotheti, F. Karavassili, A. Valmas, I. Margiolaki, University of Patras, Greece
S. Trampari, Kapodistrian University of Athens, Greece
5:00     Ends

 

TUESDAY EVENING POSTER SESSION
Caloosa Room - 5:30-7pm

*Indicates Presenter

P8 Unraveling the Solid State of MK-8970: A Racemic Acetal Carbonate Prodrug of Altegravir
N. Tsou*, C. Scott Shultz, R.J. Varsolona, Department of Process & Analytical Chemistry, Merck Research Laboratories, Rahway, NJ, USA
P9 WITHDRAWN - Monitoring Solid Forms and Solid-State Transformations of Drugs by X-ray Powder Diffraction
K. Xu*, X. Xiong, H. Li, Sichuan University, Chengdu, Sichuan, China
P10 Evaluation of Dehydration Mechanism of Ondansetron Hydrochloride with Crystal Structure Analysis
R. Mizoguchi*, H. Uekusa, Department of Chemistry and Materials Science, Tokyo Institute of Technology, Tokyo, Japan
P12 STOE InSitu HT2 – A New In-situ Reaction Chamber in Debye-Scherrer Geometry
J. Richter*, S. Correll, T. Hartmann, Stoe & Cie GmbH, Darmstadt, Germany
P13   Estimation of Grain Size by Two-Dimensional X-ray Diffractometry: Applications to Powders and After Compression into Tablets
S. Thakral*, R. Suryanarayanan, Department of Pharmaceutics, University of Minnesota, Minneapolis, MN, USA
N.K. Thakral, Eli Lilly and Company, Indianapolis, IN, USA
P27 ICDD Full Diffraction Pattern Polymer Project – New Entries for PDF-4+ 2016 and PDF-4 Organics 2017
T. Blanton*, S. Gates-Rector, ICDD, Newtown Square, PA, USA
S. Misture, Kazuo Inamori School of Engineering, Alfred University, Alfred, NY, USA
P29 Incorporation of Pharmaceutical API's into the PDF® Databases
A. Gindhart, T. Blanton*, International Centre for Diffraction Data, Newtown Square, PA, USA
J. Kaduk, Illinois Institute of Technology, Chicago, IL, USA
P30 Crystal Structures of New Group 2 Citrate Salts
J.A. Kaduk, Illinois Institute of Technology, Chicago IL and North Central College, Naperville, IL, USA
A. Rammohan, Atlantic International University, Honolulu, HI, USA
P31 Crystal Structures of Large-Volume Commercial Pharmaceuticals
J.A. Kaduk, Illinois Institute of Technology, Chicago, IL and North Central College, Naperville, IL, USA
R.J. Papoular, IRAMIS/CEA-Saclay, Leon Brillouin Laboratory, Gif-sur-Yvette Cedes, France
A.M. Gindhart, T.N. Blanton, International Centre for Diffraction Data, Newtown Square, PA, USA
P33  The Powder Diffraction File™ for Materials Research
T.G. Fawcett, S.N. Kabekkodu, S. Gates-Rector, A.M. Gindhart, J. Blanton, T. Blanton, International Centre for Diffraction Data, Newtown Square, PA, USA

 

WEDNESDAY SESSIONS
Caloosa Room

*Indicates Presenter

Formulation & Product Development/Polymorph, Salt & Co-crystal Screening
Chairs: T.G. Fawcett, International Centre for Diffraction Data, Newtown Square, PA, USA, fawcett@icdd.com
K. Saito, Rigaku Europe SE, Ettlingen, Germany, Keisuke.Saito@rigaku.com
9:00 P24 Invited – Strategies to Expand Solid-state Landscapes of Drugs to Enable Successful Tablet Formulation Development
C. Sun*, Department of Pharmaceutics, University of Minnesota, Minneapolis, MN, USA
9:45 P5 Invited - Two-Dimensional X-ray Diffractometry in Pharmaceutical Product and Process Development
N.K. Thakral*, Amgen Inc., Thousand Oaks, CA, USA
10:30    Break
11:00 P32 Invited – Capturing the Significance of X-ray Crystallography in Pharmaceutical Field: The Application to Characterize New Salt, Co-Crystal and Co-Amorphous
E. Yonemochi*, Hoshi University, Tokyo, Japan
11:45 P20  Which Form? Which Formulation? A Case Study on the Impact of Form to Bioavailability and Formulation Development
A. Patel*, Bristol-Myers Squibb, New Brunswick, NJ, USA
12:15    Lunch (attendees are on their own for lunch)
 
Amorphous, Activated and Nanomaterials
Chair: F. Gozzo, Excelsus Structural Solutions SPRL, Brussels, Belgium, fabia.gozzo@excels.us
1:45  P19 Invited - Total Scattering Characterization of Amorphous and Nanostructured Pharmaceuticals
A. Prodi*, Excelsus Structural Solutions sprl, Brussels, Belgium
P.M. Mazzeo, Excelsus Structural Solutions (Swiss) AG
A. Cervellino, SLS, Paul Scherrer Institut (CH)
F. Gozzo, Excelsus Structural Solutions sprl, Brussels, Belgium and Excelsus Structural Solutions (Swiss) AG
2:30  P18 The Analysis of Non-Crystalline Materials in Pharmaceutical Formulations
T.G. Fawcett*, S.N. Kabekkodu, S. Gates-Rector, A.M. Gindhart, J.R. Blanton, T.N. Blanton, International Centre for Diffraction Data, Newtown Square, PA, USA
3:00    Break
3:30 P53 X-ray Scattering Studies on Nano Crystalline and Amorphous Materials
D. Beckers*, M. Gateshki, PANalytical B.V., Almelo, The Netherlands
A. Adibhatla, PANalytical Inc., Westborough MA, USA
4:00 P26 Quantification of Multiple Amorphous Phases  
A. Adibhatla*, PANalytical Inc., Westborough MA, USA
T. Degen, D. Beckers, PANalytical B.V., Almelo, The Netherlands
4:30    Ends

 

 

THURSDAY SESSIONS
Caloosa Room

*Indicates Presenter

Qualitative and Quantitative Analysis
Chair: T. Blanton, International Centre for Diffraction Data, Newtown Square, PA, USA, tblanton@icdd.com
8:30 P28 Invited - Characterization of Active Pharmaceutical Ingredients and Excipients in Commercial Formulations and Preparation of New Forms by Crystallization and Heat Treatment
G. Díaz De Delgado*, R.A. Toro, A.J. Dugarte, Y.W. Escalante, R.C. López, J.A. Trejo, J.E. Contreras, J.M. Delgado, Laboratorio de Cristalografía-LNDRX, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida, Venezuela
9:15 P11 Absolute Quantification of Pharmaceuticals: The Search of Suitable Internal Standards
M.L. Reinle-Schmitt*, Swiss Light Source, Paul Scherrer Institute, Villigen, Switzerland
P.P. Mazzeo, Excelsus Structural Solutions (Swiss) AG, Switzerland
A. Prodi, Excelsus Structural Solutions SPRL, Belgium
F. Gozzo , Excelsus Structural Solutions (Swiss) AG, Switzerland and Excelsus Structural Solutions SPRL, Belgium
9:45    Break
10:00 P25 Excipient Reference Data in the Powder Diffraction File™ (PDF®) for Phase Identification in Pharmaceutical Formulations
J. Quagliarello, K. Krishnan, S. Gates-Rector, T.G. Fawcett, T.N. Blanton*, International Centre for Diffraction Data, Newtown Square, PA, USA
10:30 P21 Recent Developments in the Powder Diffraction File™
S. Kabekkodu*, S. Gates-Rector, A. Gindhart, J.R. Blanton, T.N. Blanton, T.G. Fawcett, International Centre for Diffraction Data, Newtown Square, PA, USA
11:00     Closing comments
11:15    Symposium ends