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Dushyant Patel LC-MS/MS Method

S.K.P.C.P.E.R., Kherva 47 M .Pharm. Thesis

¾ At least 67% of total dilution samples at each dilution level should fall within above-

mentioned criteria.

I. Matrix effect:

Procedure:

¾ Calibration standards were processed and analyzed in the same matrix which was to be

used during validation experiment and three replicates from all lots described above each

at LQC and HQC levels were processed and analyzed as per the procedure described in

sample preparation section.

Acceptance criteria:

¾ The back calculated concentrations of LQC and HQC must be within 85- 115% of their

theoretical concentration.

¾ At least 67% of LQC and HQC samples must fall within above-mentioned criteria for

each lot of matrix.

¾ At least 75% of the buffered plasma should meet the acceptance criteria.

¾ Both lipemic and haemolysed plasma should meet the above criteria, if the experiment

fails repeat the experiment once or change the methodology.

J. Stability:

1. Stock solution stability:

Procedure:

¾ Fresh stock solution of an analyte and an internal standard were prepared as per the

procedure described in sample preparation section.

¾ Freshly prepared main stock solutions aliquots of analyte and internal standard solution

were stored at 2-8°C in refrigerator or in freezer if required for a relevant period for

short-term and long-term stability.

¾ Freshly prepared main stock solutions aliquots of analyte and internal standard solution

were stored at room temperature for at least 6 hrs or relevant short-term period.

¾ After relevant stability period fresh stock comparison solution of analyte and an internal

standard were prepared as per the procedure.

¾ The main stock aliquots were retrieved from refrigerator and from room temperature.

¾ Appropriately stock solution of analyte was diluted to get concentration equivalent to

ULOQ nominal concentration for both comparison and stability sample solution.

¾ Six injections of freshly prepared diluted analyte and internal standard comparison

solution and stability solutions were performed.

¾ The analytical area results of stability solutions were compared with those of freshly

prepared solutions area results.

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Samsung RT34M Manuale Utente Pagina 59