m.pharm analysis, pharmaceutical analysis, food analysis, cosmetic analysis and evaluation, modern bio analytical techniques, advanced pharmaceutical analysis, phamaceutical validation

1. QUALIFICATION OF FTIR
SUBMITTED TO:
DR. C. SREEDHAR
PROFESSOR AND HOD
DEPT. OF PHARMACEUTICAL
ANALYSIS
KARNATAKA COLLEGE OF PHARMACY
BANGALORE
SUBMITTED BY:
S.GOKULRAJ
M PHARM 1ST SEMESTER (2022-2023)
DEPT.OF PHARMACEUTICAL ANALYSIS
KARNATAKA COLLEGE OF PHARMACY
BANGALORE
SUBJECT: PHARMACEUTICAL VALIDATION
1 KARNATAKA COLLEGE OF PHARMACY

2. FTIR
 Fourier transform infrared spectroscopy (FTIR) is a technique which is
used to obtain an infrared spectrum of absorption, emission,
photoconductivity or Raman scattering of a solid, liquid or gas.
 An FTIR spectrometer simultaneously collects spectral data in a wide
spectral range. This confers a significant advantage over a dispersive
spectrometer which measures intensity over a narrow range of
wavelengths at a time
2 KARNATAKA COLLEGE OF PHARMACY

3. QUALIFICATION
 Qualification is a part of validation.
 It is action of proving and documenting the equipment which
are properly installed.
 Qualification is 4 types they are,
1. Design qualification
2. Installation qualification
3. Performance qualification
4. Operational qualification
3 KARNATAKA COLLEGE OF PHARMACY

4. DESIGN QUALIFICATION
 Supplier must provide documented evidence that the product
has been designed, developed and manufactured in a quality
environment.
 ISO 9001:2000 certification.
 Supplier must provide phone and on-site support in case of
defects.
 Supplier must provide information through the internet on
availability of new firmware upgrades.
 The below is a sample of technical attributes that may be
considered in design qualification of an FT-IR spectrometer
and may be adapted if necessary.
4 KARNATAKA COLLEGE OF PHARMACY

5. INSTALLATION QUALIFICATION:
 Equipment is compared as received with purchase order,
including software, accessories, spare parts and consumables.
 Documentation checked for completeness of operating,
maintenance instructions, standard operating procedures for
testing and safety, validation certificates and health and safety
instruments.
 Equipment is checked for any damage.
 The supplier's instruction for installation is read.
 The supplier's safety instructions are read, if there are any
5 KARNATAKA COLLEGE OF PHARMACY

6.  Hardware (computer, equipment, fittings and tubing for fluid
connections, power cables, data flow and instrument control cables) is
installed following the manufacturer's recommendation.
 The instruments are switched on and ensured that all modules power
up and an electronic self test is performed. Any deviations are
recorded.
 Software is installed on computer following the manufacturer's
recommendation.
 Correct software installation is verified.
 A backup copy of software is made.
 Peripherals eg. printers and equipment modules are configured.
6 KARNATAKA COLLEGE OF PHARMACY

7.  A list with a description of all software installed on the computer
is made.
 A list with a description of all hardware are identified and made,
including drawings where appropriate.
 Equipment manuals and SOPs are listed.
 An installation report is prepared.
7 KARNATAKA COLLEGE OF PHARMACY

8. OPERATIONAL QUALIFICATION
 Wavelength accuracy
 Control of 0 and 100%
 Wavelength resolution
 Wave number scale
 Detector energy ratio
 Signal/noise ratio
 Zero test
 Contamination test
8 KARNATAKA COLLEGE OF PHARMACY

9. Wavelength accuracy
Test procedure Acceptance limits Test frequency Remarks
Measurements of
polystyrene spectrum at
1144,1680,2167 and
2307nm. The results
are compared with
reference values.
2nm daily Standard should be
traceable to national
standard.
Wavelength resolution
Test procedure Acceptence limits Test frequency
Resolution of polystyrene at
2870/2851 and at 1589/1883nm.
T (band 2870cm-1-band 2851 cm-1)18
T (band 1589cm-1-band 1583cm-1)12
daily
9 KARNATAKA COLLEGE OF PHARMACY

10. Test procedure Acceptance limits Test frequency
Control at 0 and 100% 1% transmission (measured at 4000cm-
1)
Daily and after changing
measurement
parameters
Control of 0 and
100%
Test procedure Acceptance limits
The minimum energy ratio value for at
least one of the following is measured
and it is compared to the vendors
specifications.
• Energy at 3990cm-1/energy at
2000cm-1
• Energy at 3400cm-1/energy at
Energy ratio test specifications vary for each
spectrometer configuration and must be referred to
the manufactures specifications.
Detector energy ratio
10 KARNATAKA COLLEGE OF PHARMACY

11. PERFORMANCE QUALIFICATION
 Power spectrum
 Wave number accuracy
 Wave number reproducibility
 Transmittance reproducibility
11 KARNATAKA COLLEGE OF PHARMACY

12. Power spectrum:
 Power spectrum gives the plot of portion of signal's power(energy per unit time) falling with
in the given frequency bins.
 This test estimates the intensity of power spectrum at a specified wave numbers.
 When the measured intensity is equal to or larger than the criterion value, the test is
passed.
Wave number (cm-1) Standard value FTIR-8400S
4600 10% or min of max
4000 25% or min of max
3000 50% or min of max
Power max value 50.0
700 10% or min of max
500 2% or min of max
403 0.5% or min of max
351 0.01% or min of max
12 KARNATAKA COLLEGE OF PHARMACY

13. WAVE NUMBER ACCURACY:
 The wave number scale is usually calibrated by the use of several characteristic wave
numbers of a polystyrene film.
 3060.0 (+/-1.5) cm-1
 2849.5 (+/-1.5) cm-1
 1942.9(+/-1.5) cm-1
 1601.2(+/-1.0) cm-1
 1583.0(+/-1.0) cm-1
 1154.5(+/-1.0) cm-1
 1028.3(+/-1.0) cm-1
 The software then judges whether the values are within the allowable range.
 The program labels the results "PASS" if all the peak numbers are within the range.
 In case of dispersive spectrophotometer the permissible level of frequency at 1601.2 cm-1 and at 1028.3 cm-
1 should be with in +/- 2.0 cm-1
13 KARNATAKA COLLEGE OF PHARMACY

14. WAVE NUMBER REPRODUCIBILITY
 This program specifies three points to measure the peak wave
numbers.
 Then it obtains the actual peak wave numbers at each point by
measuring the polystyrene film twice.
 It should satisfy 5 cm around 3000 cm-1 of polystyrene
absorption wave number, 1 cm around 1000 cm-1.
 The software determines whether the differences between each
of two measurements are within the allowable range and it
labels the result PASS if they are with in the range.
 EP 4.0 doesn't include this inspection.
14 KARNATAKA COLLEGE OF PHARMACY

15. TRANSMITTANCE REPRODUCIBILITY:
 This program specifies peak wave number at three points and the transmittance at each
point is measured is twice.
 The transmittance reproducibility should satisfy 0.5%T when the several points of
polystyrene absorption from 3000 cm to 1000 cm-1 are measured twice.
 Then it is determined whether the differences between the two data are within the
allowable range and it labels the result PASS if they are with in the range.
AS PER ASTM E1421-94 LEVEL ZERO:
 This software complies describes with in the description in the ASTM (American Society
for Testing and Materials).
 The FTIR abnormalities or large changes over short term and long term is assessed by
these tests.
 The three parameters checked by this program are:
1. Energy spectrum test.
2. 100% line test.
3. Polystyrene test.
15 KARNATAKA COLLEGE OF PHARMACY

16. 1. ENERGY SPECTRUM TEST:
 Power spectra obtained in the inspection are compared with reference
data and the spectra are checked for changes over long periods.
2. ONE HUNDRED PERCENT LINE TEST:
 100% T line spectra are calculated for power spectra & are measured
continuously in inspection and the spectra are checked for changes over
short periods.
3. POLYSTYRENE TEST:
 Evaluation is performed using differences between spectra obtained for
polystyrene film in inspection and the stored reference data.
 When the differences are within the standard, "pass" results.
 All of the above furnished data should be represented in Validation Report.
16 KARNATAKA COLLEGE OF PHARMACY

17. THANK YOU
17 KARNATAKA COLLEGE OF PHARMACY