Samsung RT34M Uživatelský manuál stáhnout pdf (Strana 58)

Dushyant Patel LC-MS/MS Method

S.K.P.C.P.E.R., Kherva 46 M .Pharm. Thesis

¾ Unextracted standard solution of an analyte (at LQC, MQC and HQC level) and internal

standard of concentrations equivalent to concentration of extracted samples were

processed and analyzed.

¾ The area for extracted LQC, MQC, HQC samples and internal standard were compared

with areas of unextracted standards and internal standard that represent 100 % recovery.

¾ % recovery of an analyte at LQC, MQC and HQC samples and an internal standard were

calculated.

¾ % recovery for extracted HQC, MQC and LQC samples should not exceed 115%, if it

exceeds then reporting should be justified.

Acceptance criteria:

¾ Recovery of analyte and internal standard should be consistent, precise and reproducible.

¾ Variability within areas at each QC level for analyte should be within CV of 15%.

¾ Variability of the analyte recoveries across all the three QC levels should be within C.V

of 20%.

¾ Variability within areas of IS found with each extracted QC level should be within CV of

15%, while the variability of internal standard area found between all the QC levels

should be within CV of 20%.

H. Dilution integrity:

Procedure:

¾ The stock solutions of analyte and internal standard were prepared as per the procedure

described in sample preparation section.

¾ Analyte spiking stock solution was spiked in blank plasma to get concentration

equivalent to 2 times of ULOQ.

¾ Above spiked samples (2xULOQ) was diluted with blank plasma to get 1/2 and 1/4

concentrations of the spiked sample or as per requirement.

¾ Calibration standards and six aliquots each of diluted samples (1/2 and 1/4 dilutions)

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

section.

¾ %CV for the back calculated concentration was calculated.

¾ % accuracy for the back calculated concentration was calculated.

Acceptance criteria:

¾ Back calculated concentration accuracy should be within 85-115% of theoretical

concentration.

¾ Precision (% CV) for the back calculated concentration should be within 15%.

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Samsung RT34M Uživatelský manuál Strana 58