PRECISION

th
By : 8 Group

NAMA ANGGOTA
1. Sugi Hartono
(132210101062)
2. Intan Nur Saadah
(132210101065)
3. Fathimatuzzahrah
(132210101074)
4. Nina Amalia
(132210101076)
5. Friska Wira Sabrina
(132210101095)
6. Dita Isnaini
(132210101108)

Definition of precision
ICH
The precision of an analytical procedure expresses the closeness
of agreement (degree of scatter) between a series of
measurements obtained from multiple sampling of the same
homogeneous sample under the prescribed conditions. Precision
may be considered at three levels; repeatability, intermediate
precision and reproducibility.

Precision should be obtained preferably using authentic

samples. As parameters, the standard deviation, the relative
standard deviation (coefficient of variation) and the confidence
interval should be calculated for each level of precision

 Precision system is obtained by repeated analysis of the same sample

(solution) and can be calculated using for a larger number of analyses (at
least five).
Precision system provides valuable information about the variability of the
analytical system, mainly the instrument and the analyte concentration
needs to be sufficiently above the quantitation limit (at least 100 times),
otherwise the contributions of the detection/integration errors will
increase

Parameters Describing the Distribution of

Analytical Data

Normal Distribution
Confidence
Standard Deviations
Intervals

Normal distribution

The distribution of data can

be visualised by histograms,
i.e., plotting the frequency of
the data within constant
intervals (classes)
throughout the whole data
range observed

The normal distribution or

Gaussian curve is bellshaped and symmetrically
centred around the mean
(true value) for which the
highest frequency is
expected

The probability of measured data decreases with the

distance from the true value and can be calculated with the
probability density function :

Standard Deviations
The
standard
deviation
is
an
important
parameter
used
to
describe the width of the normal
distribution, i.e., the degree of
dispersion of the data. It corresponds
to the horizontal distance between
the apex and the inflection point of
the Gaussian curve

Confidence intervals
The (arithmetic) mean of the measurements is an estimate of the
true value of a normal distribution and interval around the sample
mean, so called confidence interval
Because of the infinity of the normal distribution, data far away from
the true value are theoretically possible (although with a very small
probability, but this cannot predict when such an event will happen),
the expectation needs to be restricted to a practical range

Measurement of standard deviation

Reproducibility
Intermediet
precision
Repeatability

Repeatability
Repeatability is the variation experienced by a single
analyst on a single instrument.

Repeatability does not distinguish between variation from

the instrument or system alone and from the sample
preparation process.

Repeatability is performed by analyzing multiple replicates

of an assay composite sample by using the analytical
method.

The recovery value is calculated and reported for each

value.

Intermediate precision
Intermediate precision refers to a precision estimate
obtained from replicate measurements in a single laboratory
under more variable conditions than repeatability conditions.

Ideally, intermediate precision conditions should mirror, as far

as possible, the conditions of routine use of the method (i.e,
measurements made on different days by different analysts
using different sets of equipment within the same laboratory).

Intermediate precision (also called withinlaboratory or within-device precision) is a measure

of precision under a defined set of conditions:
same measurement procedure,

same measuring system,

same location, and

replicate measurements on the same or similar

objects over an extended period of time.
It may include changes to other conditions
such as new calibrations, operators, or
reagent lots.

Experimental Determination of
Intermediate Precision for Assay
Perform the repeatability analysis on different days.

Perform the repeatability analysis using different operating conditions and

different instruments when possible (e.g., column, apparatus, reagents)

If possible use a different manufacturers instrument.

Prepare the six replicate samples solutions from the same assay composite
sample according to the analytical method.
Analyze the samples according to the analytical method make two
injections of each sample.
Calculate the assay results (% recovery) for each sample.

Acceptance criteria
The
%
RSD
of
the
assay/recovery
values
generated by a single
analyst should not be
greater than 2.0%.
The
%
RSD
of
the
combined assay/recovery
values generated by both
analysts, over both days
should not be greater
than 3.0%.
Notes : A chromatogram
of a typical standard, a
typical system suitability
standard, and a typical
sample
should
be
included in the validation
report.

acceptance criteria from

related 2 sample:

The
%
RSD
of
the
impurities/degradants
generated on the second
day
should
not
be
greater than 15%.
The
%
RSD
of
the
combined assay/recovery
values generated by both
over both days should
not be greater than 15%.
Notes : A chromatogram
of an impurity typical
standard,
a
typical
system
suitability
standard,
a
typical
sample, and a sample
spiked with impurities
should be included in the

Reproducibility

Reproducibility as defined by ISO 35346 refers to a precision

estimate obtained from replicate measurements carried out in
different laboratories by different analysts using different pieces of
equipment. It therefore has to be evaluated by carrying out an
interlaboratory study. Note that the term reproducibility has also
been used more generally to describe any conditions of
measurement other than repeatability; it is therefore often useful to
qualify the term (for example, interlaboratory reproducibility).

The Precision of the method was demonstrated by system precision,

method precision studies and intermediate precision. In system
precision, the standard solution injected five times as per procedure.
In method precision six replicate injections of the standard solution
and sample solution prepared as per the proposed method and
chromatograms were recorded. In Intermediate precision was
performed on different day by using different make column of same
dimensions.

The precision is done to check for the consistent results and which
are in the limits. The method and intermediate precisions are showing
the results within the limits

Acceptance criteria:
The %RSD of areas from six preparations precision level
should not be more than 2.0%.

 System precision of the method assessed by repeatability;

determined by analyzing 10 g /ml of RIS for six times;
Method precision was studied as intra-day and inter-day
variations. Intra-day precision was determined by analyzing the
6, 8 and 10 g/ml of RIS for three times in the same day.

Precision studies were performed by preparing the standards three

times and measuring the absorbances of drugs at 235 nm and 376 nm.
Low %RSD (< 2%) shows that the method has good precision (Table
No. 7)

Interday and intraday studies showed repeatability of an analytical

method under normal operating conditions. Results of tablet analysis
showed deviation in the range of 99.78 to 101.57 % and from 98.62 to
99.84 % for PARA and LOR respectively, which indicated repeatability
of the method

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