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Dushyant Patel LC-MS/MS Method

S.K.P.C.P.E.R., Kherva 35 M .Pharm. Thesis

c) Preparation of calibration standards and quality control samples in biological

matrix with respect to 5 % spiking:

TABLE NO: 4.7

d) System suitability:

¾ Prepared MQC level sample was used in system suitability and followed the sample

treatment procedure as per section 4.2.12.

4.2.7 TUNING OF GBP AND LEV IN MS:

a) Preparation of tuning GBP solution ( 50 ng/ml):

¾ GBP (5 mg) was taken in 10 ml vol. flask and made up the volume up to mark with

methanol. Above solution (0.01 ml) was taken in 100 ml volumetric flask and diluted

with methanol to 100 ml.

b) Preparation of tuning LEV solution ( 50 ng/ml):

¾ LEV (5 mg) was taken in 10 ml vol. flask and made up the volume up to mark with

methanol. Above solution (0.01 ml) was taken in 100 ml volumetric flask and diluted

with methanol to 100 ml.

Details of spiking stock solution used

Plasma

volume

(µl)

GBP Conc. (µg/ml) Sample Name

GBP Conc. (µg/ml) Volume (µl)

1.00 5 95 0.05

CS-1

2.00 5 95 0.10

CS-2

6.00 5 95 0.30

CS-3

12.00 5 95 0.60

CS-4

24.00 5 95 1.20

CS-5

48.00 5 95 2.40

CS-6

72.00 5 95 3.60

CS-7

96.00 5 95 4.80

CS-8

120.00 5 95 6.00

CS-9

3.00 5 95 0.15

LQC

40.00 5 95 2.00

MQC

90.00 5 95 4.50

HQC

240.00 5 95 12.00

2ULOQ

1 2 ... 42 43 44 45 46 47 48 49 50 51 52 ... 92 93

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Samsung RT34M Manuale Utente Pagina 47

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