DOSAGE FORM DESIGN PARAMETERS

SOLID-STATE CHARACTERIZATION AND PHYSICAL BEHAVIOR

Prof Nalini Shastri SVCP,HYD

DIFFRACTION METHODS
Single crystal XRD Powder XRD

XRD-THEORY
Crystals Atoms and molecules are arranged in a regular pattern which follows certain law of geometry. Seven crystal systems Crystal systems are shape of unit cell which is basic repetitive unit in a crystal lattice

XRD-THEORY
Sample crystal is mounted Narrow beam of Xray passed through it l of Xray is in the order of distance between the molecules in crystal lattice and sample Acts like a diffraction grating Diffraction occurs at angle corresponding to Braggs equation nl = 2dsin d = distance between the successive planes in the crystal lattice, n = order of reflection

BRAGGS EQUATION

IDENTIFICATION BY XRD
Qualitative analysis Comparison with ICDD cards Quantitative analysis Peak intensity method height or AUC Internal standard method

OUTPUT INFORMATION FROM XRD DATA

Braggs angles
(q)

Intensity (I)

Line profile

d-values Identification Particle size Lattice parameters Crystal structure Degree of crystallinity Phase identification Polymer characterization Mixture composition Crystalline defects

PHASE STUDY BY XRD

Phase Identification
Different crystalline structures Solvates and hydrates Crystalline vs amorphous Polymorphism

Phase transitions
During processing Heating, milling, crystallization

PXRD
Sample preparation Preferred orientation Amorphous powders Broad and featureless Particle size <0.1m

ICDD card pattern for Ibuprofen

Identification of crystal impurities

a=KCl, b=NaCl, c=Physical mixture d=mixed crystal

PHASE IDENTIFICATION
a=anhydrous carbamazepine b form b=anhydrous carbamazepine a form c=carbamazepine dihydrate

Tween 80

SOLVATES

PEG400

PVPk30

PXRD-PHASE TRANSITIONS

Nifedipine xerogels

PHASE TRANSITIONS

XRD of Oxycarbamazapiene and Microcrystalline cellulose

PXRD-PROCESSING

Powder X-ray diffraction patterns of lyophilized DL-proline

DEGREE OF CRYSTALLINITY

c=crystalline a=amorphous

PXRD - QUANTITATIVE ANALYSIS

Quantitative analysis of Prazosin HCl by calibration curve method using AUC

PXRD - QUANTITATIVE ANALYSIS

XRD of 60% crystalline Indomethacin With Lithium fluoride as internal standard

XRD-ADVANCED TECHNIQUES
MICRODIFFRACTOMETRY Xray beam focused on a small area of sample 2D area detector for fast data acquisitions Detection of counterfeit drugs in tablets SYNCHROTRON RADIATION Increased sensitivity, Rapid data acquisition rapid detection of onset of crystallization High resolution data VARIABLE TEMPERATURE XRD Thermal analysis

PXRD OF CLARITHROMYCIN

VARIABLE TEMPERATURE PXRD