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Basics of Validation

This document discusses key concepts in analytical method validation including calibration, validation, accuracy, precision, specificity, linearity, range, limit of detection, limit of quantification, robustness, and ruggedness. It provides definitions and examples for each parameter to ensure methods consistently produce reliable results. Validation demonstrates a process can perform effectively and ensures analytical methods are suitable for their intended purpose.

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Dr Nilesh Patel
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Download as PDF, TXT or read online on Scribd
58 views

Basics of Validation

This document discusses key concepts in analytical method validation including calibration, validation, accuracy, precision, specificity, linearity, range, limit of detection, limit of quantification, robustness, and ruggedness. It provides definitions and examples for each parameter to ensure methods consistently produce reliable results. Validation demonstrates a process can perform effectively and ensures analytical methods are suitable for their intended purpose.

Uploaded by

Dr Nilesh Patel
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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Dr.

Nilesh Patel
Assistant Professor,
QA Department, BKMGPC, Rajkot
CALIBRATION VALIDATION
• Calibration is a • Validation is a
demonstration that, a documented program that
particular Instrument or provides assurance that a
device produces results specific process,
with in specified limits consistently produces a
comparing against a result as per acceptance
reference standard. criteria.
• Calibration ensures that • Validation provides
instrument or measuring documented evidence
devices producing that a process produces
accurate results. consistent results
• Shall be performed • Shall be performed when
periodically as per changes or modifications
calibration SOP happen
Validation Parameter
• Accuracy • Limit of detection
• Precision • Limit of Quantification
• Selectivity • Robustness
• Linearity • Ruggedness
• Range
Accuracy
• Closeness of the test
results and true value.
If actual Burette
Reading is 10.0 ml and
you get 9.9, 10.1 &
10.0 then all are
accurate results.
Accuracy express in %
Relative Standard
Deviation
Precision
• Closeness of the between test results.
you get Burette Reading 3.3, 3.2 & 3.4
ml then all are accurate results.
Precision express in % Relative Standard
Deviation
Neither Accurate Not Accurate
nor Precise But Precise

Near Accurate
But not Precise Accurate & Precise
Specificity
• Specificity is the ability of a method to
discriminate between the intended
analyte(s) and other components in the
sample.
Linearity
Linearity of a method is its ability to
obtain test results that are directly
proportional to the sample
concentration over a given range, using
the relationship between detector
response
Range
• The range of an analytical method is the
interval between the upper and lower
analytical concentration of a sample.
• Acceptable range having linearity,
accuracy, precision
Limit of Detection
• The detection limit of an individual analytical
procedure is the lowest amount of analyte in a
sample which can be detected but not
necessarily quantitated as an exact value.
• The detection limit (DL) may be expressed as:
DL = 3.3 σ/S
– σ = the standard deviation of the response
– S = the slope (Calculate the rise and run) of
the calibration curve
Limit of Quantification
• Limit of quantitation (LOQ) is the lowest level
that an analyte can be quantitated with some
degree of certainty (e.g., with a precision of
±5%).
• Standard Deviation of the Response and the
Slope
– quantitation limit (QL) may be expressed as:
QL = 10 σ/S
– σ = the standard deviation of the response
– S = the slope of the calibration curve
Y=bX+a

Statistical estimate of LOD & LOQ

LOD = 3.3 Sbl / b LOQ = 10 Sbl / b

Ybl

LOD LOQ
Robustness
The robustness of an analytical procedure is a
measure of its capacity to remain unaffected by
small, but deliberate variations in method
parameters and provides an indication of its
reliability during normal usage.
– stability of analytical solutions;
– extraction time.
– influence of variations of
pH in a mobile phase
– Temperature
Ruggedness
• Degree of reproducibility of test results
under a variety of conditions
• Different Laboratories
• Different Analysts
• Different Instruments
• Different Reagents
• Different Days
Method Life Cycle
Validation

Development Optimization

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