by 1.0 OBJECTIVE
To lay down a procedure which describe the parameters to be followed by the analysts, in analytical method validation of equipment wash water.
2.0 SCOPE
This procedure is applicable to validation of analytical methods used for equipment wash water samples .
3.0 RESPONSIBILITIES
QC Executive/Officer/designee shall be responsible for Analytical Method Validation for Equipment Wash Water Samples.
Head-QC/Designee shall be responsible for the ensuring overall compliance of the Standard Operating Procedure.
4.0 DISTRIBUTION
Master copy : Quality Assurance Department
Controlled copy – 1 : Quality Control Department
5.0 PROCEDURE
The parameters that should be tested during validation of analytical methods used for equipment wash water samples are:
5.1 Precision
5.2 Linearity
5.3 Accuracy
5.4 Ruggedness
5.5 Limit of detection
5.6 Limit of quantiation
5.1 PRECISION:
SYSTEM PRECISION:
Definition: Degree of agreement among individual standard responses from multiple analysis (e.g. Absorbance reading) of a single standard preparation.
Determined by: Repeated analysis (e.g. Absorbance reading) of single standard preparation for 6 times.
Acceptance criteria: The relative standard deviation (RSD) of 6 Analysis responses should be not more than (NMT) 2.0 %.
METHOD PRECISION:
Definition: Degree of agreement among standard responses from single analysis (e.g. Absorbance reading) of a multiple standard preparations.
Determined by: Single analysis (e.g. Absorbance reading) of different six standards in different preparations.
Acceptance criteria: The relative standard deviation of 6 analysis should be NMT 2.0 %.
5.2 LINEARITY:
Definition: Ability of an assay to elicit a proportional response to changes in analyte concentration.
Determined by: Prepare 5 concentrations of standard solutions, over the range from LOQ to 150% of specimen level.
Plot of responses versus concentrations.
Calculate (R2), the regression factor.
Acceptance criteria: The regression factor should be between not less than 0.99
5.3 ACCURACY (as recovery):
Definition: Closeness of test results obtained by the method to the true value.
Determined by: Applying the analysis method 6 times for sample prepared by preparation of 6 different known concentration amount of the analyte is added in concentration of 10 ppm.
Acceptance criteria:
- % recovery should be not less than 80%.
- The relative standard deviation of the six samples should be NMT 2.0 %.
5.4 RUGGEDNESS:
Definition: It is the degree of reproducibility of the test results obtained by the analysis of the same samples under a variety of normal test conditions, different analysts different days and different instruments.
Determined by: Applying the analysis method 6 times for sample prepared by preparation of 6 different known concentration amount of the analyte is added in concentration of 10 ppm using different analysts.
Acceptance criteria:
- Between the averages of two sets NMT ± 2.0 %.
- RSD for each 6 samples NMT 2.0 %.
5.5 LIMIT OF DETECTION:
Definition: Smallest concentration of analyte sample that can be detected reliably.
Determined by: Comparing test results from samples with known concentration of analyte with that of blank sample and establish the minimum level at which the analyte can be reliably detected.
Acceptance criteria: Signal of analyte response to noise of blank response ratio should be NLT (3:1).
5.6 LIMIT OF QUANTITATION:
Definition: Smallest concentration that can be quantified with acceptable levels of accuracy and precision.
Determined by: Comparing test results from samples with known concentration of analyte with that of blank sample and establish the minimum level at which the analyte can be quantified with acceptable precision and accuracy.
Applying the analysis method 6 times for a sample known to be prepared near or at the limit of quantitation.
CONCLUSION: Method is considered valid if all the above mentioned tests are within acceptance criteria of each parameter.
DOCUMENTATION: Validation report per Wash water analytical method must be issued to demonstrate the validation parameter & results obtained.
ACCEPTANCE CRITERIA: The acceptance criteria for all equipment’s is not more than 10 PPM
TESTING OF SAMPLES (Validation & verification)
For testing of samples, the wavelength selection will be taken from the wavelength scanning at maximum absorbance for the 10 PPM standard.
For testing of the cleanses of coating machine , scanning will be done from wavelength 200- 600 due to direct contact of the coating solution to inside the coating machine which is directly contact with the Powder.
6.0 ABBREVIATIONS
QC : Quality Control.
PPM : Parts Per Million
NMT : Not More Than
NLT : Not less than
RSD : Relative Standard Deviation
ABS : Absorbance
% : Percentage
LOQ : Limit of Quantitation
