GROUP LOD LOQ

YASMIN
122210101032
NANDA SURYANING R122210101034
MIA RISWANI
122210101042
GALUH SINOARSIH 122210101050

Method Validation- LOD and

LOQ
Sensitivity
Limit of detection (LOD) the lowest
content that can
be measured with reasonable statistical
certainty.
Limit of quantitative measurement (LOQ)
the lowest
concentration of an analyte that can be
determined with
acceptable precision (repeatability) and
accuracy under
the stated conditions of the test.

Limit of Detection (LOD)

Typically 3 times the signal-to-noise
(based on standard deviation of the noise)

Validation-LOD
Various methods
possible
visual evaluation
minimum level at which the analyte can
be detected reliably

signal-to noise
3:1 ratio is
acceptable

standard deviation of the slope and

response
LOD = 3.3 / S
= standard deviation of the
response

Based on signal-to noise

Reliable quantification is a 10:1 ratio

Based on SD of the response and the

slope
LOQ = 10 / S
= standard deviation of the response
S = slope of the calibration curve

LOQ (Limit of Quantitation)

QL / LOQ is the lowest amount of analyte in a

sample that can be quantitatively determined
with suitable precision and accuracy
QL is a parameter of quantitative assays for low
concentration of compounds in sample matrices
and is used particularry for the determination of
impurities an/or degradation products.

THE FORMULA OF LOQ

Limit of detection (LOD) and Limit of Quantification

(LOQ) were found to be 0.5892g/ml and 1.785g/ml
respectively by simple UV Spectrophotometric.

Preparation of standard stock solution

Stock solution I: Accurately weighed quantity (10

mg) of bivalirudin was dissolved separately in small
quantity of distilled water and volume was made up to
10ml with distilled water to get a solution containing
1000g/ml.
Stock solution II: From the stock solution, 1ml
solution was taken and then diluted up to 10ml with
same solvent in a volumetric flask and then
concentration of this stock solution was 100g/ml.

Determination of

max

Preparation of Calibration Curve

Next ...

Methods of Validation
Limit of detection (LOD) and
Limit of quantification (LOQ)

Determination of the detection and quantification

limits was performed based on the standard
deviations of y-intercept and the slope of the least
square line parameters as defined in the
International Conference on Harmonization (ICH)
Q2 guidelines.
The Limit of Detection (LOD) and Limit of
Quantification (LOQ) were 0.5892 g/ ml and
1.785 g/ml respectively and data (Table 5).

The limit of detection (LOD) is defied

as the lowest concentration of an analyte
that an analytical process can reliably
differentiate from back-ground levels.

The limit of
quantification
(LOQ) is
defined as the lo
west
concentration of
the
standard curve th
at can
be measured wit
h an
acceptable accu
racy,
precision, and va
riability

LOD and LOQ were based on the

standard deviation of the
response and the slope of the
corresponding curve using the
following equations :
LOD = 3s/m; LOQ = 10s/m
s, the noise of estimate, is the
standard deviation of the
absorbance of the sample and
m is the slope of the related
calibrations graphs

Limit of detection (LOD) and Limit of Quantification

(LOQ) were found to be 0.5892g/ml and 1.785g/ml
respectively by simple UV Spectrophotometric.

Sample preparation

Limits of detection (LOD) and

Limits of quantitation (LOQ)

LOD and LOQ were calculated from the data

obtained from the linearity studies. The slope
of the linearity plot was determined.
For each of the six replicate determinations, y
intercept was calculated and the standard
deviation of the y intercept was computed.
From these values, the parameters Limit of
detection (LOD) and Limit of quantitation LOD
and (LOQ) were determined on the basis of
response and slope of the regression
equation.

LOD and LOQ were calculated

using following equation as per
ICH guidelines.
LOD=3.3 /S
LOQ=10 /S

where :
is a standard deviation of
the y-intercept of the
regression line
s is slope of the calibration
curve.

LOD and LOQ for AMB was found to be 14.09 and

42.724 and for DOX the values of LOD and LOQ
found to be 8.9005 and 26.9713 respectively

THANKS FOR YOUR

ATTENTION