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Related Concept Videos

X-ray Diffraction of Biological Samples01:10

X-ray Diffraction of Biological Samples

X-ray diffraction or XRD is an analytical tool that utilizes X-rays to study ordered structures such as crystalline organic and inorganic samples, polycrystalline materials, proteins, carbohydrates, and drugs.
According to Bragg's law, when X-rays strike the sample positioned on a stage, the rays are  scattered by the electron clouds around the sample atoms. The  X-ray diffraction or scattering is caused by constructive interference of the X-ray waves that reflect off the internal crystal...
Determination of Crystal Structures01:29

Determination of Crystal Structures

In the late 1800s, the revelation that light extended beyond visible wavelengths led to the discovery of X-rays by Wilhelm Roentgen. Recognized as high-energy electromagnetic radiation with short wavelengths, X-rays prompted exploration into their interaction with crystals. Max von Laue proposed in 1912 that the periodic arrangement of atoms, ions, or molecules in crystals would cause them to diffract X-rays, a hypothesis confirmed through experiments with copper sulfate and zinc sulfide...
X-ray Crystallography02:18

X-ray Crystallography

The size of the unit cell and the arrangement of atoms in a crystal may be determined from measurements of the diffraction of X-rays by the crystal, termed X-ray crystallography.
Diffraction
Diffraction is the change in the direction of travel experienced by an electromagnetic wave when it encounters a physical barrier whose dimensions are comparable to those of the wavelength of the light. X-rays are electromagnetic radiation with wavelengths about as long as the distance between neighboring...
Quantitative Analysis01:12

Quantitative Analysis

Quantitative analysis is a technique for measuring the amount of specific constituents in a sample. When the sample's composition is unknown, qualitative analysis is performed first to identify its components, which ensures that the correct substances are measured during the quantitative phase.
In quantitative analysis, two key measurements are made: the sample quantity and a property proportional to the amount of the analyte (the substance being analyzed). This forms the basis of the method...

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Synthesis and Microdiffraction at Extreme Pressures and Temperatures
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Published on: October 7, 2013

A quick method for the quantitative analysis of mixtures. 1. Powder X-ray diffraction.

Wei Dong1, Christopher Gilmore, Gordon Barr

  • 1WestCHEM, Department of Chemistry, University of Glasgow, Glasgow G12 8QQ, UK.

Journal of Pharmaceutical Sciences
|September 19, 2007
PubMed
Summary

This study introduces a new X-ray powder diffraction method for analyzing API-excipient mixtures. The technique accurately quantifies components with minimal data processing and computer time.

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Area of Science:

  • Analytical Chemistry
  • Materials Science
  • Pharmaceutical Analysis

Background:

  • Accurate quantification of active pharmaceutical ingredients (APIs) and excipients in mixtures is crucial for drug development and quality control.
  • Traditional methods for analyzing mixtures using X-ray powder diffraction (XRPD) can be complex and computationally intensive.
  • Existing techniques often rely solely on peak analysis, potentially overlooking valuable information within the diffraction pattern.

Purpose of the Study:

  • To develop and validate a novel, simplified method for analyzing mixtures of APIs and excipients using XRPD.
  • To assess the accuracy and efficiency of the new method compared to established techniques like Rietveld refinement.
  • To demonstrate the applicability of the method across different diffractometer systems, including high-throughput instruments.

Main Methods:

  • A linear regression algorithm was employed to fit pure component phases to the mixture's XRPD pattern using linear least squares.
  • The method utilizes all measured data points across the 2theta scan, minimizing data processing.
  • The PolySNAP computer program implements the developed analytical techniques.

Main Results:

  • The method accurately analyzed mixtures with up to three components, achieving mean errors of 1.7–3.9% for two-phase and 4.0–8.6% for three-phase mixtures.
  • Results demonstrated comparable accuracy to traditional Rietveld refinement.
  • The Bruker GADDS system, designed for high-throughput, yielded results of similar accuracy to single-sample diffractometers.
  • Detection limits around 10% were achieved for mixtures lacking pure phase patterns.

Conclusions:

  • The described XRPD method offers a robust, efficient, and accurate approach for analyzing API-excipient mixtures.
  • The technique requires minimal computer time and user interaction, making it practical for routine analysis.
  • The method's versatility extends to high-throughput screening and situations with incomplete reference data.