Samsung RT34M Uživatelský manuál stáhnout pdf (Strana 57)

Dushyant Patel LC-MS/MS Method

S.K.P.C.P.E.R., Kherva 45 M .Pharm. Thesis

F. Precision:

1. Within-batch or intra-batch precision:

¾ Calibration standards and six replicates each of LLOQ, LQC, MQC and HQC samples

were processed and analyzed as per the procedure described in sample preparation

section.

¾ Mean, standard deviation and % coefficient of variation for LLOQ, LQC, MQC and HQC

samples, analyzed in single analytical batch were calculated.

2. Between -batch or inter-batch precision:

¾ Calibration standards and six replicates of LLOQ, LQC, MQC and HQC samples were

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

¾ Five different batches on different days were performed.

¾ Mean, standard deviation and % coefficient of variation for LLOQ, LQC, MQC and HQC

samples analyzed on five different batches on different days were calculated.

Acceptance criteria:

¾ The %CV of the back-calculated concentrations of all QC samples (LQC, MQC, and

HQC) must be within 15%, except for LLOQ, which should be within 20%.

¾ At least 67% quality control samples must fall within above-mentioned criteria at each

LLOQ, LQC, MQC and HQC levels.

G. Recovery:

¾ Recovery for analyte and internal standard was performed by comparing the area of

extracted samples at three different concentrations (LQC, MQC and HQC) with un-

extracted standards area that represents 100% recovery.

Procedure:

¾ Recovery of an analyte was determined at LQC, MQC, HQC levels and recovery of an

internal standard was determined at concentration to be used during method validation.

¾ Six replicates each of LQC, MQC, and HQC samples were processed and analyzed as per

the procedure described in sample preparation section. These were considered as

extracted samples for recovery.

¾ To prepare comparison samples for recovery, extracted solutions of blank matrix were

used, for the preparation of equivalent unextracted samples, to nullify the matrix effect

while calculating the recovery.

¾ For the recovery comparison samples, the spiking stock of standard solution of an analyte

and internal standard were spiked in the extracted blank matrix solution to achieve

concentration equivalent to extracted samples nominal concentration.

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