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Dushyant Patel LC-MS/MS Method

S.K.P.C.P.E.R., Kherva 33 M .Pharm. Thesis

4.2.3 PREPARATION OF ANALYTE SOLUTIONS:

a) Preparation of GBP main stock solution (5.00 mg/ml):

¾ GBP working/reference standard (equivalent to 50 mg) was weighed accurately.

Transferred it in 10 ml volumetric flask. Diluent (50 ml) was added and sonicated to

dissolve. Diluted up to mark with diluent.

b) Preparation of GBP intermediate stock solutions:

1. GBP intermediate stock solution (2.50 mg/ml )

¾ Calculated volume of GBP main stock solution (5 ml) was transferred to 10 ml

volumetric flask and diluted up to mark with diluent.

2. GBP intermediate stock solution (0.50 mg/ml)

¾ Calculated volume of above GBP intermediate stock solution (5 ml) was transferred to

make conc. 0.50 mg/ml of GBP in 25 ml volumetric flask and diluted up to mark with

diluent.

Note: a) Percentage purity/ assay of standard were considered while weighing.

b) Salt equivalency was considered while weighing.

c) Weight and volume of solution might be changed as per the requirement

without altering the concentration for analysis.

4.2.4 PREPARATION OF INTERNAL STANDARD SOLUTION:

a) Preparation of LEV main stock solution (1.00 mg/ml):

¾ LEV working/reference standard (equivalent to 10 mg) was weighed accurately.

Transferred it in 10 ml volumetric flask. Diluent (about 5.0 ml) was added and sonicated

to dissolve. Diluted up to mark with diluent.

b) Preparation of LEV intermediate stock solution (0.20 mg/ml):

¾ The calculated volume of LEV main stock solution (2 ml) was transferred to make conc.

0.20 mg/ml in 10 ml volumetric flask and diluted up to mark with diluent.

c) Preparation of LEV spiking stock solution (1.50 µg/ml):

¾ The calculated volume of LEV intermediate stock solution (0.188 ml) was transferred to

make conc. 1.50 µg/ml of LEV in 25 ml volumetric flask and diluted up to mark with

diluent.

Note: a) Percentage purity/ assay of standard were considered while weighing.

b) Salt equivalency was considered while weighing.

c) Weight and volume of solution might be changed as per the requirement

without altering the concentration for analysis.

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Samsung RT34M Manuale Utente Pagina 45