SPDS SET 2: ASH-01

Precision:

4.3)

4.3.1) Definition: The precision is a measure of the closeness of agreement between observed values obtained independently from multiple samplings of a homogenous sample and is expressed as the variance, standard deviation or relative standard deviation (coefficient of variation) of observed values.

4.3.2) Assessment for Area: Determined by injecting 5 different concentrations of standards 5 times each and 7 different samples 2 times each and calculating the relative standard deviation (RSD).

4.3.3) Assessment for Retention Time: Checking the relative standard deviation of retention time of the peaks obtained using the above solutions.

4.3.4) Assessment for reproducibility of result: By analyzing the same sample in duplicate and finding the relative standard deviation of the assay.

4.3.5) Acceptance Criteria: The Relative standard deviation to be less than 2.5% for all the above.

4.3.6) Precision for peak areas:

Experiment:

a) Standard preparation: Prepared as mentioned in linearity 4.2.4 (a). b) Sample preparation: The sample solution was prepared by weighing the quantity of the sample shown in the Table in a 250 ml beaker, extracted with 100ml of methanol, boiling on water bath for 10-15 minutes and repeated the procedure 3-4 times till the material is completely extracted or till the extracts turn colourless. Combined all the fractions, concentrated and made up the volume to 50ml with methanol. Filtered

through 0.45 microns membrane filter paper.

Table -17

Batch No.

Quantity (mg) 753.6

1503.2

WS/06Lot10

2096

1$785$/ 5(0(',(6

3DJH RI