1. GPAT
COURSE: B.PHARM VII SEM
SUBJECT: PHARMACEUTICAL QA
Date: 01.02.2024 11AM -12 NOON
ANALYTICAL METHOD VALIDATION
PARAMETERS
Dr. C. Vinodhini, M.Pharm, Ph.D
Associate Professor
Sri Ramachandra Faculty of Pharmacy
SRIHER, DU.
Venue: Lecture hall IV, III Floor SRFOP
Number of students enrolled: 31
07/02/2025
1
2. LECTURE – 11
PROGRAM: PHARM.D –III YEAR
COURSE : PHARMACEUTICAL
ANALYSIS
Date: 28. 10.2024, 8-9am & 29.10.2024, 11-12noon
ANALYTICAL METHOD VALIDATION
PARAMETERS
Dr.C.Vinodhini, M.Pharm, Ph.D
Associate Professor
Sri Ramachandra Faculty of
Pharmacy
SRIHER, DU.
07/02/2025 1
Number of stduents enrolled: 31
Venue: Lecture hall –IV, II Floor
3. 3
o Learning objectives
o At the end of the session student will be able to
o Define Analytical method validation
o Discuss the characteristics of Analytical method validation as
below:
a) ACCURACY
b) PRECISION
c) REPEATABILITY
d) REPRODUCIBILITY
e) LIMIT OF DETECTION (LOD)
f) LIMIT OF QUANTIFICATION (LOQ)
g) LINEARITY
h) RANGE
i) SELECTIVITY
j) SENSITIVITY
k) ROBUSTNESS
l) RUGGEDNESS
4. 4
ANALYTICAL METHOD VALIDATION
(Q2R1)
It is defined as the process by which it is established by
laboratory studies, that the performance characterstics of the
method meets the requirement for intended analytical
application.
Purpose:
• To ensure the selected analytical procedure will give reproducible
& reliable results.
• To validate an analytical procedure certain characterstics are
studied.
• If satisfactory results are obtained for the following
characterstics, then the method may be considered as validated.
5. 5
oa) ACCURACY:
It is defined as closeness of the test values obtained by
the method to the true (standard) value.
• It is determined by assay method used on a highly pure
substances like reference/standard & compared it with same
material with a known and established method.
ob) PRECISION:
It is degree of agreement among individual test results
when the method is applied repeatedly to multiple sampling
of a homogenous sample.
• It refers to degree of reproducibility of results
6. 6
• It is determined by assessing sufficient number of dilutions of
a homogenous samples to be able to calculate statistically
valid estimates of std deviation or relative S.D
oc) REPEATABILITY:
It is a precision of the procedure when repeated by
the same analyst under the same set of conditions & with a
short interval of time.
• It is assessed by carrying out complete, separate
determinations on separate, identical samples of the same
homogenous batch of materials.
7. 7
od) REPRODUCIBILITY:
It is a precision of the procedure when it is carried out
under different conditions usually in different laboratories
on separate identical samples from same homogenous batch
oe) LIMIT OF DETECTION (LOD):
It is the lowest amount of analyte in a sample that
can be detected, but not necessarily quantitated under
stated experimental conditions.
LOD = 3.3 X σ
S
σ - Standard deviation
S - Slope
8. 8
o f) LIMIT OF QUANTITATION (LOQ):
It is the lowest concentration of the analyte in a sample
that may be determined & quantitated with acceptable accuracy
& precision when the required procedure is applied
LOQ = 10 X σ
S
σ - Standard deviation
S - Slope
o g) LINEARITY:
The linearity of an analytical procedure is its ability to
produce results that are directly proportional to concentration of
analyte in the sample
9. 9
oh) RANGE:
Range is defined as the interval between the upper
& lower levels of analyte that have been demonstrated to be
determined with a suitable level of precision, accuracy &
linearity
oi) SELECTIVITY:
Selectivity or specificity of a procedure is its ability
to measure the analyte in a manner that is free from
interference from other components in the sample being
examined
10. 10
o j) SENSITIVITY:
It is the capacity of test procedure to record small variations in the
concentration.
• It is the slope of the calibration curve.
o k) ROBUSTNESS:
It is defined as a measure of its capacity to remain unaffected by
small (but deliberate) variations in method parameters & provides an
indication of its reliability during normal usage.
Eg: In HPLC analysis
Change in flow rate ± 0.1 ml
Change wavelength ± 2 nm
11. 11
ol) RUGGEDNESS:
It is defined as a degree of reproducibility of test
results obtained by the analysis of same sample under a
variety of conditions such as different laboratories, analysts,
different instruments, reagents, assay time intervals, assay
temperature at different days
• It is a measure of the reproducibility of test results under
variations in specific conditions
• POSSIBLE QUESTION
• ANALYTICAL VALIDATION PARAMETERS
