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Dushyant Patel LC-MS/MS Method

S.K.P.C.P.E.R., Kherva 42 M .Pharm. Thesis

anticoagulant to be used for study), 0l lipemic plasma and 01 haemolysed plasma lot

were included.

¾ One sample each of the above mentioned 10 plasma lots at blank and LLOQ level was

processed and analyzed as per the procedure described in sample preparation section.

Acceptance criteria:

¾ No interfering peaks from endogenous matrix components, decomposition product etc.,

should be present at the retention time of an analyte and an internal standard in blank

matrix.

¾ If any peak is present at the retention time of analyte in blank matrix, its area response

should be ≤20 % of response of an extracted lowest plasma calibration standard i.e.

LLOQ standard of the same lot.

¾ If any peak is present at the retention time of an internal standard in blank matrix, its area

response should be ≤5 % of the response of an extracted internal standard concentration

of the same lot.

¾ At least 75 % of the buffered plasma and heparinised plasma should meet the acceptance

criteria.

¾ Both lipemic and haemolysed plasma should meet the above three criteria for the

interference at the respective retention time of analyte and internal standard. If the

experiment fails, repeat the experiment and then change the methodology if required.

C. Sensitivity:

Procedure:

¾ Calibration standards, zero standard (matrix spiked only with internal standard) and six

sets of matrix sample spiked at LLOQ concentration were processed and analyzed using

blank matrix lot, as per the procedure described in sample preparation section.

Acceptance criteria:

¾ The analyte area response at the LLOQ should be at least 5 times the response compared

to blank response.

¾ Analyte calculated concentration should be identifiable and reproducible with a precision

of 20% and accuracy of 80- 120%

D. Linearity:

¾ A calibration curve (standard curve) is the relationship between the response of the

instrument and known concentrations of the analyte.

¾ A calibration curve should be prepared for each analyte in the sample.

¾ A sufficient number of standards should be used in order to properly define the

relationship between concentration and response.

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Samsung RT34M Bedienungsanleitung Seite 54