Rapid Analysis of adulterated

dexamethasone in traditional herbal medicine

for joint-pain killer using infrared spectroscopy

Ardi Nugroho
Department of Pharmacy
Faculty of Mathematic and Natural Sciences
Univesitas Islam Indonesia
Background

Green Chemistry

Rapid, reliable, low cost, low waste

FTIR
Why???
Chemometric
is the science of extracting
information from chemical
systems by data-driven means.
Background

THM Analytical method

• Common illness • Profit
• Elder • Relatively safe • Dangerous • HPLC

• Chronic • Longterm • TLC

Joint-pain Adulteration
Background

toxic
expensive

destructive

Infrared + Chemometric
Material and Method
Material
• Eight different herbal products from local pharmacies in special region of
Yogyakarta.
• Dexamethasone standard (purchased from Indonesia National Agency of
Drug and Food Control).
• KBr from Sigma (Aldrich, St. Louis, USA).
• Spectrophotometer Spectrum-Two (Perkin-Elmer, Ohio, US), with deuterate
d triglycine sulphate (DTGS) detector and Dynascan™ interferometer
Method

• TLC
Qualitative
Analyis
• TLC-densitometry

• Dexamethasone
Self-made
sample
• Various concentration (5%-85%)

• Minitab 17
Chemometric • PLS
Result

Qualitative analysis
FTIR
Standard dexamethasone
Overlay standard and 2 samples
PLS without cross-validation

wavenumbers
3646, 3642, 2461, 2453,
2432, 2406, 2229, 2209,
2197, 2097, 2092, 2064,
2059, 2047, 2026, 2009,
1969, 1513 cm-1
PLS result with leave-one-out

internal validation
by issuing of one data
from the calibration set,
then from the remaining
data created an equation
and used to calculate the
predicted levels of data
released earlier.
Model selection and validation
Fits and Residuals
Summary

equation:
ĉ = 0,999382c + 0,000149
R 0,9988
RMSEC 0,009455549

equation:
ĉ = 0,990419c + 0,003545
R 0,989
PRESS 0,02272
RMSECV 0,029015481
Conclusion

These results indicated that infrared spectroscopy combined with PLS is

an alternative technique for determination of adulterated dexamethasone
in traditional herbal medicine for joint-pain killer.
Thank You