SOP FOR VALIDATION OF ANALYTICAL TEST PROCEDURE

I.                   PURPOSE

To define the procedure for Validation of Analytical Test Procedure.

II.                SCOPE

This SOP is applicable for Validation of Analytical Test Procedure in Quality Control department at …

III.             RESPONSIBILITY

 Executive - Quality Control

             Head - Quality Control

IV.             ACCOUNTABILITY

Dy. Manager - Quality Assurance

V.                PROCEDURE

1.0    Analytical Method like Spectrophotometer, Chromatographic methods are shall be validated as follows.

2.0        In General assay, impurities determination methods shall taken for validation.

3.0        If any methods are not validated at R & D centre, the methods can be validated at QC Unit-V.

4.0        Pharmacopoeial & In-house Analytical methods shall validated for

4.1            Accuracy

4.2            Precision

4.3            Specificity

4.4            Limit of Detection

4.5            Limit of Quantitation

4.6            Linearity and Range

4.7            Ruggedness

4.8            Robustness (Pharmacopoeial and compended methods used in the cleaning

       procedure may not be considered.)

5.0        For any revised analytical method, a comparative evolution shall be made between existing and proposed analytical method. This evolution shall be made keeping minimum accuracy, specificity, and Precision in to consideration.

6.0        Whenever there is a need to change critical test parameters and conditions, the method shall revalidated with the revised parameters and conditions.

7.0        The separate protocol shall be prepared before validation.

8.0        Accuracy

8.1      The accuracy is the closeness of test results obtained by that method to the true value. Accuracy is a measure of exactness of analytical method.

                   8.2   This is done by adding known amount of drug substance to the previously assayed product. Then percentage recovery of added amount is calculated. (Follow guidelines Q2A and Q2B)

9.0        Precision

9.1      The precision of any analytical method is the degree of agreement among individual test results when the procedure is applied repeatedly to multiple sampling of a homogeneous sample. This is usually expressed as standard Deviation or Relative standard deviation.

9.2      For this aliquots of a homogeneous sample shall be assayed six times. Calculate the   Relative Standard Deviation. (Follow guideline Q2A and Q2B)

10.0    Specificity

10.1  The specificity of an analytical method is its ability to measure accurately and specifically the analyte in the presence of components that may be expected to be present in the sample matrix.

10.2  Alternatively, in HPLC method, PDA detector is used and peak purity and contour plot is compared. (Follow guideline Q2A and Q2B)

11.0    Limit of Detection

11.1        The Limit of detection is a parameter of limit tests. It is the lowest concentration of the analyte that can be detected but not necessarily quantitate. (Follow guideline Q2A and Q2B)

11.2        For instrumental methods, usually standard deviation multiplied by a factor 3 provides an estimate of limit of detection or signal to noise ratio of 3:1 is generally accepted in case of HPLC/GC analysis. This limit is subsequently validated by 5 samples prepared, to the calculated concentration. (Follow guidelines Q2A and Q2B)

12.0    Limit of Quantification

12.1        This is a parameter of quantitative assays for low levels of analyte in sample matrices. (Follow guidelines Q2A and Q2B)

12.2        For instrumental methods, standard deviation, multiplied by 10 provides an estimate of the limit of quantitation. This limit is subsequently validated by 6 samples prepared to the calculated concentration. (Follow guidelines Q2A and Q2B).

13.0    Linearity and Range

13.1        Linearity of an analytical method is its ability to elicit test results that are directly or by a mathematical transformation, proportional to concentration of analyze in a sample within a given range.

13.2        The range of an analytical method is the interval between the upper and lower levels of analyte that have been demonstrated to be determined with precision, accuracy and linearity using the method.

13.3        The linearity is determined by analyzing different concentration of analyze and establishing proportional ratio between two different concentrations of analyte.

13.4        The range is validated by verifying that the analytical method provides accuracy, precision and linearity when applied to samples containing analyze at the extremes of the range as well as within the range. (Follow guidelines Q2A and Q2B)

14.0    Ruggedness

14.1        The ruggedness of an analytical method is the degree of reproducibility of test obtained by the analysis of the same sample under the variety of normal test conditions, such as different analyst, different days, different work conditions. (Follow guidelines Q2A and Q2B)

14.2         The reproducibility of test is compared to the precision of test under normal conditions.

15.0    Robustness

15.1        The robustness of an analytical method 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 use. (Follow guidelines Q2A and Q2B) 

VI.       REVISION SUMMARY

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