NIR SPECTROSCOP

Y & APPLICATION

A Seminar on..

Prepared by:Nikhil PrajapatiM.Pharm,1styear[Q.A]T1616QA001

Guided by:Dr. Falguni TandelHead of Dept. [Q.A]

PARUL INSTITUTE OF PHARMACY, LIMDA

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CONTENTS Introducttion Principle Instrumentation Adwanteges Dis-adwanteges Applicatons Refrences

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INTRODUCTION

Infra-red spectrum is an important record which gives sufficient information about the structure of a compound.

In recent years, NIR spectroscopy has become so widespread in process analysis and within pharmaceutical industry for raw material testing, pharmaceutical industry in biotechnology, genomics analysis, proteomic analysis ,textile monitoring, food analysis, plastics, textiles, insect detection forensic lab application, crime detection, various military applications,

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RANGE OF ELECTROMAGNETIC RADIATION

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NIR is comprised of combinations and overtones that is anharmonic oscillation.

Most molecules contain covalent bonds which

share electrons between atoms. Although bonds are elastic, they do not obey Hooke’s law exactly. The model of anharmonic oscillation is more precise.

Harmonic oscillator can not be retained at larger amplitudes of vibrations owing to repulsive forces between the vibrating atoms and possibility of dissociation..

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NIR VIBRATIONAL BANDS

From Metrohm “NIR Spectroscopy” monograph

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INSTUMENTATION

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BASIC CONFIGURATIONS OF NIR Conf. A is commonly preferred. In the case of

interference-filter spectroscopy, it is better because unnecessary components of the light are cut off before the sample position.

Conf. B has to be used for multichannel spectroscopy because a wide range spectrum is being simultaneously measured with a multichannel detector.

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1)LIGHT SOURCES1.LIGHT EMITTING DIODES(LED) Gallium arsenide Advantages:- they require low power have Long life expectancy.

2. TUNGSTEN LAMPS (incandescent bulbs) produce heat up to 1100k.Advantages cheap readily available

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2) MONOCHROMATOR:

Two types of monochromator used1. Prism2. Grating

Grating monochromator is used to measure the full visible and NIR spectrum may be in transmittance or reflectance

It is mainly used for research or when a wide range of different applications is required.

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3) SAMPLES PRESENTAION Transmittance: calculated by dividing the radiant power of

the light transmitted through the sample by the radiant power of the incident light

Reflectance: calculated using the ratio of the radiant power of reflected light to the radiant power of incident light

Transflectance: calculated by dividing the radiant power of light that has traversed a sample twice (once right after it was emitted, and once after if was reflected by a reflector) by the radiant power of the incident light

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4) DETECTORThe choice of detectors depends on Wavelength range, Spectrometer design characterstics detector characteristics such as photosensitivity

(responsivity),noise equivalent power (NEP),etc

Detectors using in NIR spectrometers are 1. Lead sulphide detectos (PbS), 2. Lead selenide detectors (PbSe), 3. Silicon detectors,4. Indium antimonide detectors,5. InGaAs, InSb, Common Charged Coupled Devices

(CCD).

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DETECTORS USED IN NIR SPECTROSCOPY

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CLASSIFICATION OF MODERN NIR INSTRUMENTS

Filter based instruments AOTF based instruments Scaning grating based instruments Fourier-transform based instruments Multichannel Fourier-transform (MCFT)

spectroscopy   Classification of Modern NIR Instruments

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FILTER-BASED INSTRUMENTS A filter allows a particular portion of the spectrum to pass

through or blocks all wavelengths below or above a certain frequency. An interference filter consists of a transparent dielectric spacing material separating two partially reflective windows, allowing a specific set of wavelengths to pass..

source Interference filter sample detector

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ACOUSTIC OPTICAL TUNEABLE FILTER In AOTF wavelength selectors light is directed into a crystal

of TeO2 . A high-frequency acoustic wave in the radio frequency range is coupled into the crystal by the use of a piezoelectric material bonded to the crystal. These acoustic waves quickly propagate through the crystal, interact with the broadband light and generate two monochromatic beams of light, each polarized in a different direction.

it has no

moving parts, adjustable

intensity and gives narrow

beams

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TILTING FILTER It’s first type of interference filter. The transmitted

energy at various wavelength depends on the incident angle of light passing through the filter. In this, the filters were mounted in an encoder wheel for greater accuracy i.e. wavelength reproducibility.

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FOURIER TRANSFORM -BASED INSTRUMENTS The interferometer works on the principle whereby light from the

source is split into two segments by the beam-splitter. One portion travels to a fixed mirror and is reflected back to the

splitter and The second portion strikes on a moving mirror and returns to be recombined with the first portion of light.

It’s pattern of peaks/troughs is called an interferogram and by applying mathematical calculations to these, a spectrum evolves. Interferometers are popular in both mid-range infrared and NIR.

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MULTICHANNEL FOURIER-TRANSFORM (MCFT) SPECTROSCOPY

This instrument utilizes a fixed monochromator, usually a holographic grating and an array of many small detectors. The light is collimated onto the grating and is thereafter dispersed into component wavelengths. The wavelengths are then directed to a series of photo-diodes. Photo-diode arrays are more commonly used for process control.

Fixed monochromator

source sample slit detector

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NIR APPLICATIONS

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Identification and qualification of raw materials and intermediates.

1. Library approach .2. Conformity approach3. Quantitative calibration models Analysis of intact dosage forms1. Tablets.2. Capsules3. Lyophilized products4. Polymeric implants and microspheres. Process monitoring and process control1. Powder blending2. Drying3. Granulation .4. Pelletization5. Tabletting and capsule-filling6. Film coating7. Packaging

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NIR AGRICULTURAL APPLICATIONS it is in commercial use in Japan, primarily for melons and citrus

fruit.  The technology may be used to exclude fruit with internal

defects. A portable unit would enable random checks of fruit in the field

or in the wholesale or retail store.  On-harvester estimation of grain protein content for precision

agriculture and estimation of the sugar content of fibrated sugar cane (beet) in sugar mills.

Sweet Corn - insect damage and insect detection Coal - moisture determination Citrus - quality attributes Pineapples, mango's, strawberries - quality attributes

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Stone fruit - quality attributes Melons - quality attributes

Determination of pharmaceutical dosage forms Monitoring of PVC industrial blending process Identification of inorganic preservative-treated Wood Analysis of polymorphs Determination of Adulteration of African Essential Oils Protein quantification within lipid implants

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LYOPHILIZED PRODUCTS Lyophilization is usually performed to increase the storage

stability of hydrolytically unstable drugs that are intended to be used as injectables or to achieve an instantly soluble oral dosage form.

Normally The moisture content of lyophilized products is determined by

time-consuming methods, such as Karl Fischer titration. In addition, the procedure requires the vial to be opened for analysis.

NIR Moisture determination with NIR diffuse reflectance techniques

can be performed in a fast and non invasive manner through the glass vials.

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MEASURE THE NIR SPECTRUM OF EACH LYO-PRODUCTa) The principal set up which

to achieve the NIR spectra in reflection mode

b) The illumination is realized through a 40 Watt tungsten halogen lamp which illuminates the vial

c) The NIR reflection is collected in a fibre optic cable which is connected to the NIR PDA spectrometer with 256 diodes and a wavelength range of 1000 nm to 2100 nm

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Packaging is the last step in the production line of a pharmaceutical product. To ensure the product safety of pharmaceuticals, a last identity check of the product on the packaging line would be highly desirable.

Such an inspection system based on the combination of a conventional high resolution camera with an on-line diode

NIR spectrometer ranging from 900 to 1700 nm at 6 nm resolution has been developed recently. The system is supposed to perform a 100% identity check at full line speed(i.e. 12,000 tablets per minute) before closing the blister. The potential of this type of equipment has been evaluated in a feasibility study .