Purity Identificaion of Crack-Coccaine

1
Purity Identificaion of Crack-Coccaine
Through the use of HPLC
We selected 47 samples of crack seized by police
and they were weighed by difference and diluted
in 100 acetonitrile in the first two races and
80 acetonitrile in water in the third race. The
method used a high-efficiency liquid
chromatography with diode array detector (Thermo
Scentific, USA). The mobile phase was an aqueous
solution of 0.01 triethylamine (solvent A) and
acetonitrile (solvent B). The mobile phase (pH
7.8) was eluted in isocratic mode at 55 B (v/v)
1mL/min. The separation was achieved using a
chromatographic column C-18 (15cm x 4.6 mm id x
5mm, 5 Ace, catalog the ACE-121-1546).
Calibration curves were constructed with 6 points
between 3.45 µg/ml and 103.65 µg/ml. The
detection was performed using a diode array
detector and quantification of cocaine was made
to 224nm. The column was maintained at 30 degrees
celsius during every race. The samples were
diluted in 2 ml tubes eppendorffs with a solution
of 40 acetonitrile in water and filtered through
polyvinylidene fluoride membrane (0.45 µm) for
HPLC vials. Aliquots (10ul) samples at a
concentration of the 75 µg/ml were directly
injected into the liquid chromatography by
autosampler.
Rony Anderson1, Eduardo de Jesus
Oliveira1, Kyle Wojciechowski2 1- Laboratorio
de Tecnologia Farmaceutica, Federal University of
Paraiba 2- State University of New York at
Oswego, NY, USA
Introduction
Methods
Objectives
Crack-Cocaine is an illicit drug throughout the
world today. It is highly addictive and can be
used in a variety of ways which may include
injection into veins and smoking of the crack.
With Brazil now being the second largest consumer
of Crack-Cocaine in the world, certain techniques
have to be done to combat this drug invasion.
To do this, an efficient and accurate method of
drug analysis has to be done in order to have a
chance of combating the sale of the drug and also
to see how the drug is evolving.
We selected 47 samples of crack seized by police
and they were weighed by difference and diluted
in 100 acetonitrile in the first two races and
80 acetonitrile in water in the third race. The
method used a high-efficiency liquid
chromatography with diode array detector (Thermo
Scentific, USA). The mobile phase was an aqueous
solution of 0.01 triethylamine (solvent A) and
acetonitrile (solvent B). The mobile phase (pH
7.8) was eluted in isocratic mode at 55 B (v/v)
1mL/min. The separation was achieved using a
chromatographic column C-18 (15cm x 4.6 mm id x
5mm, 5 Ace, catalog the ACE-121-1546).
Calibration curves were constructed with 6 points
between 3.45 µg/ml and 103.65 µg/ml. The
detection was performed using a diode array
detector and quantification of cocaine was made
to 224nm. The column was maintained at 30 degrees
celsius during every race. The samples were
diluted in 2 ml tubes eppendorffs with a solution
of 40 acetonitrile in water and filtered through
polyvinylidene fluoride membrane (0.45 µm) for
HPLC vials. Aliquots (10ul) samples at a
concentration of the 75 µg/ml were directly
injected into the liquid chromatography by
autosampler.
The method was to develop a High Pressure Liquid
Chromatography (HPLC) method to quantify cocaine
in Crack-Cocaine samples that were seized by the
State Police force of Paraiba
Results
Figure 1. These are the correlation curves of the
standard sample of Crack-Cocaine for three
different runs in which the area of the unknown
samples where based off of.
Figure 2. This is an example of an HPLC Crack
sample readout with the Cocaine peaking at around
6.3 minutes
Figure 4. This is a spreadsheet for the average
purity, 6 for each, with the standard deviation
for all 47 samples of Crack-Cocaine.
Figure 3. This is a comparison of the purity
between Runs 1-2 and Run 3 for all of the samples.
Conclusion
References
Acknowledgements
Hays, PA, Thompson, RA (2009) The processing
method enabling the use of peak heightneed for
accurate and proton NMR quantitation. Magnetic
Resonance in Chemistry 47819-824.
Overall, the results from the third run were
more accurate than that of the first and second
runs. This is due to the increased accuracy of
weighing techniques and pipeting techniques over
the time of first two runs. The next step would
be to do NMR tests on all of the samples then
compare the results with the HPLC results to see
the data agrees with each other.