10 Method Validation Parameters in Pharma

Method Validation Parameters in Pharma

Analytical Method validation is an essential step in the development of reference methods and in the assessment of a lab’s ability to produce reliable analytical records. Validation is incorporated within the context of a procedure, generating chemical data.

Validation of analytical methods, taking the maximum possible steps to ensure that the best possible parameters are being used, using the numerous relevant performance metrics inclusive of selectivity, specificity, accuracy, precision, linearity, range, the limit of detection, the limit of quantification, ruggedness, and robustness are severely discussed in an effort to prevent misguided utilization and ensure scientific correctness and consistency among publications.

What are the analytical method validation parameters?

As per method validation guidelines, there are some parameters where the method can be established.

Here is the list of Analytical Method validation parameters.

  1. Accuracy
  2. Precision
  3. Specificity/Selectivity
  4. Robustness
  5. Linearity
  6. Range
  7. Limit of Detection
  8. Limit of Quantitation
  9. Ruggedness/Intermediate Precision
  10. Stability

Let’s understand the definition of all analytical method validation parameters in brief;

1. Definition of Accuracy:

The accuracy of an analytical procedure is the closeness of the test results obtained by that procedure to the true value.      Or

The accuracy of an analytical method is the degree of agreement of test results generated by the method to the true value.

2. Definition of Precision: 

The precision of an analytical procedure is the degree of agreement among individual test results when the procedure is applied repeatedly to multiple sampling of a homogeneous sample. Precision may be a measure of either the degree of reproducibility or of repeatability of the analytical procedure under normal operating conditions.

3. Definition of Specificity/Selectivity:

The ICH guideline defines specificity as the ability to access unequivocally the analyte in the presence of components that may be expected to be present, such as impurities, degradation products, and matrix components.

4. Definition of Robustness:

The robustness of an analytical procedure is a measure of its capacity to remain unaffected by small but deliberate variations in procedural parameters listed in the procedure documentation and provides an indication of its suitability during normal usage.

Robustness may be determined during the development of the analytical procedure.

Few examples of robustness:

  • pH
  • Temperature
  • Flow Rate
  • Different make of column
  • Stability of Analytical Solutions
  • Extraction time

5. Definition of Linearity:

The linearity of an analytical procedure is its ability to elicit test results that are directly or by a well-defined mathematical transformation, proportional to the concentration of analyte in a sample within a given range. Possible transformations may include log, square root, or reciprocal although other transformations are acceptable.

6. Definition of  Range:

The range of an analytical procedure is the interval between the upper and lower levels of analyte (Including these levels) that have been demonstrated to be determined with a suitable level of precision, accuracy, and linearity using the procedure as written.

The range is normally expressed in the same unit as obtained in the test results by the analytical procedure. (ex. Percent, parts per million)

7. Definition of Limit of Detection (LOD):

It is a characteristic of the limit test. It is the lowest amount of analyte in a sample that can be detected but not necessarily quantitated under the given set of conditions. The detection limit is usually expressed as the concentration of analyte (Ex. Percentage,  parts per billion) in the sample.

8. Definition of Limit of Quantitation (LOQ):

It is the lowest amount of analyte in the sample that can be determined with acceptable precision and accuracy under the stated experimental conditions. The quantitation limit is expressed as the concentration of an analyte. (Ex. Percentage, parts per billion) in the sample.

9. Definition of Ruggedness/Intermediate Precision:

A robust analytical method can achieve the same level of repeatability when processed in another lab, with new analysts, new equipment, different lots of reagents, new assay conditions, new days, and other factors.

10. Stability:

Several analytes readily decompose prior to chromatography investigations. For instance, when preparing the sample solution, removing the solvent, cleansing the sample, transferring the sample to a new vial, and during storage of the prepared vials.

During method development, the stability of the analyte should be investigated. The accuracy test takes care of stability. It should be mentioned in the method how long the sample can be stored before the final analysis, based on the duration of the accuracy test.

These are the 10 method validation parameters that are used to establish the method while method development study. Method validation parameters are very helpful to make the method rugged, robust, and more accurate.

Method Validation Parameters

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