Report Of Laboratory Exercises

Report of laboratory exercises

Atomic absorption specroscopy is analytical method characterized with high selectivity,sensitivity and fast speed.

Application of flame atomic absorption spectrometric techniques to pharmaceuticals and waters

 Three different brands of multivitamins (effervescent tablets) were taken from the market and the levels of some elements (total amount) were determined (Ca, Mg, Zn, Cr, Mn)  One tablet from each of the three pharmaceutical products was dissolved in 100ml (mother solution) water and one milliliter of each solution was diluted 25 times. So were prepared the working sample solutions and were marked as follows: Sample 1 (samp1) - ABO Pharma A-Z ®; Sample 2 (samp2) - Supradyn ®; Sample 3 (samp3) - Supravit Active ®;  A brand of mineral water - Gorna Banja ® was tested for any Mg and the concentration of the metal was under the detection limit of the instrument  For each different element was made a standard calibration curve, using freshly prepared standard solutions from 0,5; 1; 3; 5; 10; 20ppm containing all the mentioned elements in water (deionized)  For the last sample results were obtained both after automated calibration and a manually made calibration curve.  Differences in the absorption using reducing and oxidizing flames were observed

Measured Given values # Sample values [mg/tablet] Measured [mg/tablet] Given values # Sample values Measured [mg/tablet] Given values [mg/tablet] # Measured 1 Sample 102 ± values 10% 160 [mg/tablet] Given values [mg/tablet] # Sample values 1 150±10% 100 [mg/tablet] Measured [mg/tablet] Given values # Sample values 2 1 167 ± 10% 120 5[ug/tablet] 5,25±10% [mg/tablet] 100±10% 2 80 1 0.9±10% 2 3 2 - 7±10% 8 1 25

Ca calibration curve

Mgycalibration curve = 4,8951x + 22,446

300

absorbance

absorbance

absorbance

absorance absorbtion

250 1200 200 1000 150 900 800 800 100 700600 600 50 600 500 500 160 400 0 400400 140 0 300 10 200 300120 200 0 100200100 80 00 100 0 60 0 40

20 0 0

2

R = 0,9939 curve Zn calibration y = 190,51x + 76,783 2

= 0,984 + 65,358 yR = 73,959x Mn calibration curve

Cr

20

1 2

2 = 0,9706+ 11,941 yR= 25,781x calibrationRcurve(reductive 2 = 0,9971

flame) λ =422,7 nm y = 6.4178x + 5.7374

λ =285,2 nm 50 60 λ =213.9 nm concentration [ppm] 2 3 5 6 λ4 8=279.5 nm 4 6 [ppm] 10 12 concentration λ =213.9 nm R2 = 0.9935 30 40

concentration [ppm] 10 15

5

0

5

20

concentration [ppm]

10

15

3

25

20

3 25

concentration [ppm]

Cr calibration curve (oxidation flame) 20 18 16 14 12 10 8 6 4 2 0

y = 0.8219x + 1.6256 R2 = 0.9996

λ =213.9 nm 0

5

10

15

20

2

3

25

2 3

1.6±10% 12,5±10% 1,75±10% 1.0±10% -

1.8

20 3

1

25 -

# Sample

Measured values [ug/tablet]

1

1.9±10%

2

2.4±10%

Pb calibration curve (ET AAS) 350

y = 3,775x + 8,3333 R2 = 0,9909

absorption

300 250 200 150 100

λ =283.3 nm

50 0 0

20

40

60

80

100

Et AA S

concentration [ppb]

3

2.1±10%

# Sample

Measured values [ug/tablet]

1

8.9±10%

2

1.6±10%

3

1.9±10%

Cd calibration curve (ETAAS) 300

y = 144,38x + 8,8333 R2 = 0,9828

absoption

250 200 150 100

λ =228.8 nm

50 0 0

0,5

1 concentration [ppb]

1,5

2

Sample 1 (samp1) - ABO Pharma A-Z ®; Manufacturer: ABO Pharma AG

Sample 2 (samp2) - Supradyn ®; Manufacturer: Bayer AG

Sample 3 (samp3) - Supravit Active ®; Manufacturer: Kendy Ltd Bulgaria Patented by Swisse AG

IR spectra of benzocaine

C-H str. vibr

CH3, CH2 def. vibr.

CH3 (end) def. vibr.

KBr Spectra benzocaine

-CH2

C-C

-NH2 -C=O

-Ar -NH2

Thank You for Your attention Lora Georgieva Denitsa Atanasova Krum Bardarov