TABLET EVALUTION BY NEAR

INFRARED SPECTROSCOPY
It is a rapid, nondestructive method of
quantitative and qualititative evaluation of tablet.
It has been used in food and agriculture
industries for many years to determine moisture,
protein and starch.
In Pharmaceutical application, NIR is used as a
secondary analytical tool.
The NIR region of the electro spectrum is from
800 to 2500 nm.
In the NIR region, the radiation can penetrate
compressed materials such as tablets, providing a
vast amount of the information about the sample

 The NIR region of the spectrum contain

overtone and combination bands that are
primarily attributed to hydrogen vibration.
This overtone and combination bands are
much weaker than the fundamental
vibration thus the absorptivity are much
smaller than corresponding IR bands.
NIR instruments are designed as
transmittance or reflectance.

Current method of tablets evaluation:

Official methods: weight uniformity,
content uniformity and
disintegration testing.
Unofficial methods: hardness,
crushing strength,
friability.
Time consuming and destructive in
nature.
Integrity is also loss.

Advantage of NIRs tablet evaluation:

Non destructive method
Noninvasive method
Can be used in the early stage of product
development
Rapid
Reducing environmental wastage
Reducing no. of the sample taken from the
batch
Reducing sampling error by directB
measurement form apparatus
Multiple components can be measured.

Limitation of NIRs tablet evaluation:

Initial calibration process for a
subs is quite difficult
Calibration equation is needed for
each constitutes
Calibration must be formulation
specific
Physical attributes of the tablets
can affect the calibration process

Application:
Raw material identification:
It is useful analysis of raw material and final product.
Measure large variation in moisture content and
particle size which is monitored by it.
Used as an identification method
Particle size
Convention methods are sieve method and laser
scattering.
NIR method is used to determine particle size of the
pure granules.
Based on that, the reflectance increase as the particle
size decease.
This method is accurate for larger size particles (above
85 mm).
Employed for MCC and lactose monohydrate.

 Polymorphism and recemization

Many drugs have ability to form polymorph.
Generally it is identified by DSC and X-ray
crystallography. But these are destructive.
Polymorph is chemically identical having
different arrangement of molecules. So
having different types of IR spectra.
E.g. Identification of the polymorphs of
caffeine.

 Moisture content:
Classical method for this is Karl Fischer titration,
gas chromatography, and loss on drying.
In this method presence of the water can be
identified by abs band at 1920-1950nm.
This band depend on the degree of the hydrogen
bond, so as the stronger the bond longer the wave
length of NIR absorption.
And the second band is appearing at 1450nm for
bound water.
This method is used for determination of content
of powder, bulk hard gelatin capsules, and tablets.

 Product evaluation:

Identification and potency:

Use to measurement of content in formulation. E.g. For
measurement of metaprolol in SR tablets.
Strength of tab also measured.
NIR can be distinguishing b/w three avicel products
owing to particle size.
Lubricant recognition can be done.
Uncoated and coated tablets produce different spectra
in reflectance mode, while minimum diff in
transmittance.
Quantitative determination of acetyl salicylic acid can
be done by NIR.
Also used fir identity of blister packaged tablets.
The problems of dissolution failure in the Erythromycin
tab can be identified.

 Quality control parameter:

Tablet hardness:
It shows variation in signal as change in the compression
force so it affects the tab hardness.
Increasing the compression force cause the harder the
tablet causing less light scattering leading to higher abs,

Tablet coating
Used to determine tablet coating and core thickness.
Used to monitor film coating.
Also used to predict coating thickness of coating
formulation at various intervals during the process and it is
less time consuming.

 Determination of degradation product:

Use for monitor the decomposition of aspirin.
Change in spectra can be correlated to mass of
water absorbed and mass of salicylic acid formed.
Characterization of powder blends and
homogeneity:
It is useful in evaluating the powder mixing process.
The apparatus consist of a diffuse reflectance
fibric optic probe interfaced online with a blender.
Spectra are collected at different time interval and
variability of spectra as a function of time is
measured and it has been shown that this variability
reached a minimum level when blend is homogenous