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Dushyant Patel LC-MS/MS Method

S.K.P.C.P.E.R., Kherva 50 M .Pharm. Thesis

¾ % Mean change must be within ± 15%.

4. Freeze and thaw stability of GBP (after 4

cycle at -20°C and -70°C):

¾ Freeze and thaw stability of analyte was determined after three freeze and thaw cycles at

LQC and HQC levels.

Procedure:

¾ Three sets (set-1, set-2 and set-3) each having six replicates each of LQC and HQC

sample of freeze and thaw stability by spiking with freshly prepared stock solutions or

stock solutions with proven stability were prepared.

¾ All the samples were stored at –20°C and/or –70°C for at least 24 hrs and after this period

all the three sets of samples were thawed unassisted at room temperature.

¾ When completely thawed, set-1, set-2 and set-3 were refrozen for at least 12 hrs under the

same conditions.

¾ Kept set-1 in frozen condition to use for second freeze and thaw cycle when analytical

results of third freeze and thaw cycle were not within the acceptance criteria.

¾ The second freeze - thaw cycle was repeated for set-2 and set-3.

¾ The frozen set-2 and set-3 were thawed for the third freeze and thaw cycle. Set-3 was

thawed.

¾ Calibration standards and six replicates each LQC and HQC comparison samples were

prepared by spiking with freshly prepared stock solutions or stock solution with proven

stability as per the procedure. Those samples were processed and analyzed.

¾ Set-2 stability samples after third freeze and thaw cycle along with freshly prepared low

and high quality control comparison samples were processed and analyzed.

¾ Fourth freeze and thaw cycle for set-3 was repeated.

¾ The mean back-calculated concentration of stability samples with those of freshly

prepared comparison samples was calculated.

¾ % mean change was calculated as per formula.

Acceptance criteria:

¾ The back-calculated concentrations of all LQC and HQC samples must be within 85- 115

% of their nominal concentration.

¾ At least 67 % of QC samples must fall within above-mentioned criteria at each LQC and

HQC levels.

¾ % Mean change must be within ± 15 %.

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Samsung RT34M Bedienungsanleitung Seite 62