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Dushyant Patel LC-MS/MS Method

S.K.P.C.P.E.R., Kherva 48 M .Pharm. Thesis

¾ After relevant long-term stability period at 2-8°C, fresh stock comparison solution of

analyte and an internal standard were prepared as per the procedure.

¾ Above steps were repeated for long-term solution stability.

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

prepared comparison solutions.

¾ % mean change for analyte and internal standard was calculated.

Acceptance criteria:

¾ % mean change between freshly prepared stock solution (comparison samples) area

results and stability samples area results must be within ± 10%.

¾ If %CV of area of analyte and internal standard for both stability and comparison sample

is greater than 5 % than out of six only one inappropriate sample should be rejected.

¾ If above acceptance criteria are not met, then experiment should be repeated if on

investigation any processing error is found or should be repeated for relevant shorter

storage period or storage temperature.

Main stock solution stability of GBP and LEV (IS) at room temperature for 93 hrs:

¾ Main stock solution of GBP and LEV (IS) were freshly prepared and aliquots of stocks

were kept at room temperature for 93 hrs (stability sample). Aqueous equivalent highest

calibration standards of GBP and LEV (IS) were prepared from the stability samples and

analyzed. Areas of stability samples and freshly prepared samples were compared to

determine % mean change during stability period.

Main stock solution stability of GBP and LEV (IS) at 2-8°C for 93 hrs:

¾ Main stock solution of GBP and LEV (IS) were freshly prepared and aliquots of stocks

were kept at 2-8°C for 93 hrs (stability sample). Aqueous equivalent highest calibration

standards of GBP and LEV (IS) were freshly prepared from the stability samples and

analyzed. Areas of stability samples and freshly prepared samples were compared to

determine % mean change during stability period.

2. Bench top stability of GBP (at room temperature for 20 hrs):

Procedure:

¾ Six aliquots each of LQC and HQC samples were spiked for bench top stability. These

samples were kept at room temperature for 20 hrs.

¾ In case of spiking and keeping the bench top stability samples at room temperature, the

bench top stability period was considered between the time of keeping at room temp.

and the time of start of processing those samples.

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

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

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Samsung RT34M Bedienungsanleitung Seite 60