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Applications of XRD – Foods

Applications of XRD

The growth of our civilization has seen a parallel growth in the food industry. In pre-historic ages humanity was dependent mainly on vegetables, fruits and meat for its daily food intake. However, over the years there has been an increasing demand for processed synthetic foods to cater to the needs of a growing population and to meet scarcities in different regions having harsh climatic conditions.

Processed foods need to have some basic characteristic properties which make them acceptable to the consumer. Some of these features are:

Colour which can be introduced with a blend of natural and artificial colouring agents

Flavours need to be added to make foods appealing or suppress some inherent bad odours

Preservatives are needed to improve the shelf life for long time storage and use

Stabilisers are added to improve their texture. This means modification of the crystalline behaviour and characteristics of the phases of different constituents

Anti- oxidants are added to prevent decay of food by oxidation

Emulsifying agents help in facilitating uniform distribution of fats and oils in aqueous media

Buffering agents control the acidity or pH of the food over storage period

The number of additives added to foods are growing by the day to match consumer tastes and lead to a corresponding increase in  market potential.

Several analytical techniques are routinely used to monitor the d presence of such food additives in manufacturing processes. The role played by XRD cannot be overlooked. X-ray diffraction provides us information on polymorphism, degree of crystallinity and amorphism. Such parameters help control the texture and stability of foods under different storage conditions.

X-ray diffraction has helped conduct studies on following common food ingredients such as

Starches

Fats

Candies

Starches

X-ray diffraction complements the DSC studies in starch gelatinization in foods. Gelatinization results when starch crystals melt with increasing temperature. It has been observed that the melting temperature increases with the decrease in moisture content. Gelatinization decreases the degree of crystallinity of starch granules and increases the non-crystalline amorphous content. This results in apparent changes in optical and rheological flow properties of foods.

Fats

X-ray diffraction has been extensively used in studying the polymorphism (different molecular packing arrangements in crystals) of fats such as margarines. The three common polymorphs of fats are α, ß and ß’. Packing arrangement in α form is hexagonal, triclinic in ß and orthorhombic in ß’. The ß form is the most stable form whereas α form is the least stable of the three. Polymorphic differences are of significance in food industry as such differences bring about changes in physical properties such as texture. Such inter- conversions can result from transitions from ß’ to the more stable ß form under different processing conditions.

Candies

Candies and chocolates are very popular among children. X-ray diffraction plays a useful role in manufacturing products of consistent quality in terms of sweetness, texture and flavor. Such characteristics depend on the balance between crystalline and amorphous proportions of constituents which can be easily monitored with the help of the X-ray diffraction technique.

The scope of X-ray diffraction in the food industry is increasing as consumers demand consistency of quality and new ingredients are finding their way into new products which are developed at an amazing pace.

Applications of XRD – Pharmaceuticals

Applications of XRD

Pharmaceutical formulations are available as tablets, capsules, ointments, pills, oral liquids, aerosol sprays, etc. Even a single drug can be found in several different formulations which impart   it different characteristics as per administration requirements .In case of solid formulations X-ray diffraction has been used as a non-destructive technique for testing of inconsistencies in manufactured batches, new drug development, and detection of impurities, degree of crystallinity and presence of polymorphism. In other words XRD serves as a fingerprinting technique for pharmaceutical formulations. It helps in optimization of manufacturing parameters, compatibility of excipients with active ingredients and controlling properties of dosage forms such as dissolutuion rate of active ingredients and stability behaviour under different environmental conditions.

The article discusses some common applications of the technique in drug manufacture and quality control .It is important to mention that XRD is a sensitive technique and errors in sample preparation can lead to wrong inferences. The sample collected should be representative of the material and with uniform distribution of particles. During sample collection and preparation the material should not be subjected to unwanted stress or other environmental conditions as such factors can result in adverse effect on the material characteristics.

Identification

Conventionally the analysis is carried out by crushing the tablet or capsule gently in a mortar and pestle or a grinding mill. Vigorous grinding can introduce mechanical stress leading to phase transitions. For small sample quantities capillary mounts can be used. Today modern diffractometers have provision to correct for the curvature when examining tablets or capsules with curved surfaces.  XRD analysis can help determine the uniform distribution of tablet ingredients. Such distribution can establish the preferential treatment of surface modifying agents such as pigments or lubricants which can influence shelf life of a formulation, its dissolution rate and disintegration behaviour. Accessories are also available to conduct studies under variable temperature and humidity.

Degree of hydration or solvation

Hydrated or solvated molecules have different characteristics. Thermal techniques such as TGA and DSC are being used to determine the number of molecules of hydration or solvation but XRD helps easy correlation of such states with crystal structure. Variable temperature accessories further provide an idea of temperature or humidity on associated properties of such materials.

Amorphous content

A drug substance can contain excipients which are amorphous in nature. In comparison with crystalline materials an amorphous material shows instability and transforms to crystalline phase over time due to environmental conditions during storage. Solubility of a drug increases with increasing amorphous content so it becomes necessary to quantify the amorphous content. X-ray diffraction offers a useful tool for quantifying the amorphous content. This is achieved by comparison of the intensity ratio between the peak of crystalline component with the hollow intensity of the amorphous content.

Polymorphic impurity profiling

A formulation can contain polymorphic impurities, products of degradation and excipients which can have a bearing on the functionality, stability and effectiveness of the active ingredient. Different polymorphs of the same compound exhibit different properties. Compression forces during tablet production can cause changes in composition of such compounds. X-ray diffraction is an established method for estimation of such substances

Pharmaceutical analysis poses quite a few challenges due to presence of a broad range of materials, their orientations and mixed crystallinity. However, XRD provides useful information and in combination with other contemporary techniques such as TGA, FT-IR, DSC, NMR,etc can provide useful details on pharmaceutical formulations.

 

Material Characterization by X-ray Diffraction Studies

Symmetric Faced Crystal

X-ray diffraction is a valuable tool in the hands of the analytical chemist for material characterization which is based on arrangement of atoms in the crystal lattices. The biggest advantage is that it is a non-destructive technique and the sample can be reused for further investigations by other means. Samples can range from symmetrically ordered atomic arrangements to random arrangements as in amorphous substances. The common applications of x-ray diffraction studies include crystal lattice dimensional analysis, grain size, crystal defects and residual strain.

X-rays interact with solid materials to generate diffraction patterns. Data on diffraction patterns resulting from interaction of x-rays with inorganic and organic solids shows definite patterns which can be used as fingerprints in identification of such materials. Diffraction data base is maintained by the International Centre of Diffraction data (ICDD) which was formerly known as Joint Committee on Powder Diffraction Standards (JCPDS). Such reference data can be purchased direct from ICDD or through

x-ray diffraction instrument suppliers.

X-ray diffraction studies easily distinguish between single crystal orderly arrangements of atoms to polycrystalline arrangements. The atomic planes of crystal lattices responsible for scattering of x-rays are their reflective surfaces. Scattered beams when in phase interact constructively and intensities are maximum at particular angles. Such reflecting patterns on reaching the detector will generate a response which can be matched with the pattern from standard materials.

It is interesting to note that under the influence of heat small particles anneal to form larger aggregates. This becomes apparent as peak intensities get enlarged and help distinguish nano-particles from larger aggregates of particles.

Applications of XRD

X-ray diffraction is a powerful tool for characterization of

nano- materials, bulk materials and thin polymeric films.

Phase studies

Powder crystallographic studies help characterization on the basis of chemical composition of materials. Such studies provide valuable details on phase transformations resulting from subjecting materials to extremes of temperatures.

Degree of crystallization

Polymeric materials often exhibit mixed behaviour as they can be partially crystalline and partially amorphous. The degree of amorphous content can vary with the conditions used during their processing. The more the amorphous content the greater will be the peak broadening so the ratio between the peaks of pure crystalline standards and polymeric materials will give an idea on the degree of crystallinity in the polymeric sample.

Residual stress

Stress is defined as force acting on a material per unit area and any deformation per unit length is referred to as strain. Residual stress is the stress that remains in the material when the force responsible for it is removed. In synthetic materials residual stress results from material treatment processes such as machining, welding, heat quenching, etc. On the other hand in geological samples such stress could be the result from natural rock dynamics under the earth’s surface. X-ray diffraction is helpful in studies on residual stress introduced in materials through artificial or natural processes.

X-ray diffraction also helps study the dominant or preferred orientation of polycrystalline aggregates. Such information is beneficial in relating orientations of aggregates or texture to the desirable properties of materials.

In conclusion it can be said that x-ray diffraction studies provide valuable information which can help characterize both manufactured as well as naturally occurring materials.

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Recent Posts

  • Applications of XRD– Forensics
  • Applications of XRD – Geology and Mining
  • Applications of XRD – Cosmetics
  • Applications of XRD – Foods
  • Applications of XRD – Pharmaceuticals

Applications of XRD – Pharmaceuticals

Pharmaceutical formulations are available as tablets, capsules, ointments, pills, oral liquids, aerosol sprays, etc. Even a single drug can be found in several different formulations which impart   it different characteristics as per administration requirements .In case of solid formulations X-ray diffraction has been used as a non-destructive technique for testing of inconsistencies in manufactured batches, […]

Applications of XRD– Forensics

Forensic analysis is a scientific study which assists criminal investigations. Whenever any crime takes place there is exchange of material between the accused and the victim such as textile fibers, blood stains, gunshot residues, broken glass, saliva, semen, etc. Chemical and biological tests on such materials can provide undisputed evidence to nail down the suspect. […]

Copper bearing ore on mine conveyor

Applications of XRD – Geology and Mining

X-ray diffraction or XRD has made valuable contributions in the field of geology and mining. Geology is the scientific study on structure of planet earth, formation of rocks, sediments and minerals. Mining is an applied science which concerns with extraction of ores, fossil fuels for energy needs and minerals for commercial processing. Minerals are inorganic […]

Applications of XRD – Cosmetics

Cosmetics have been in use since time immemorial. In earlier ages several potentially toxic inorganic pigments such as malachite, mercuric sulphide or white lead were used in cosmetic preparations. In contemporary products several organic components such as parabens, alkylphenols, etc have also been included. It was a common concept that cosmetic products were only meant […]

Applications of XRD – Foods

The growth of our civilization has seen a parallel growth in the food industry. In pre-historic ages humanity was dependent mainly on vegetables, fruits and meat for its daily food intake. However, over the years there has been an increasing demand for processed synthetic foods to cater to the needs of a growing population and […]

  • Applications of XRD – Pharmaceuticals
  • Material Characterization by X-ray Diffraction Studies
  • Component parts of an X-ray Diffractometer
  • Crystal Geometries – Lattices and Miller Indices
  • Role of Bragg’s law in X-Ray Diffraction studies

Applications of XRD– Forensics

Copper bearing ore on mine conveyor

Applications of XRD – Geology and Mining

Applications of XRD – Cosmetics

Applications of XRD – Foods

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