Chan, Miranda, Tapel PhCh 135 PH2

EXPERIMENT 4: Determination of
Quinine Sulfate in Tablets Using 0.5 mL 1 M H2SO4
Fluorescence Spectroscopy
Dilute with H2O
PREPARATION OF STANDARD QUININE STOCK
SOLUTION, 1000 ppm Filter if necessary
[1000 ppm] until clear

25 mL H2O in
Sample
100-mL beaker
5 mL 1 M H2SO4
0.1207 g quinine 2.5 µL sample solution in
Transfer to 100-mL 100-mL volumetric flask
volumetric flask
Dilute with 0.05 M H2SO4
Dilute with H2O
Measure fluorescence
SS1 intensities in triplicates

MEASUREMENT OF FLUORESCENCE INTENSITY

[10.0 ppm]
Determination of Excitation (lex) and Emission (lem) Wavelengths
5.00 mL of SS1 in
Standard (5) and sample solutions in
500-mL vol. flask
plastic 96-well microplates
25.0 mL 1 M H2SO4

Dilute with H2O Place inside machine chamber

SS2
Scan for optimum lex and lem

Preparation of Standard Quinine Solutions

Repeat twice
1 mL SS2 3 mL SS2 5 mL SS2 7.5 mL SS2 10 mL SS2
DATA ANALYSIS
Transfer to separate 100-mL volumetric flasks
Determine emission of each
Fill to volume with 0.05 M H2SO4 solution using lex and lem

0.1 ppm 0.3 ppm 0.5 ppm 0.75 ppm 1.0 ppm Plot emission against concentration
Use linear regression
Sample Preparation
Compute for amount of quinine
Weigh & finely
sulfate (ppm) in the sample tablets
powder ≥ 20 tablets

Compute for relative standard

Transfer 200 mg to 10-mL vol.
deviation and % recovery
flask using H2O as aide