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Experimental
Chemicals, Material, and Reagents
Standards were obtained from the reference collection of
this laboratory. Sodium hydroxide 0.1N, CElixir A (pH 2.5),
CElixir B (pH 2.5), CElixir B (pH 2.5) with hydroxypropyl-cyclodextrin (HPCD)1 (Custom Chiral2 Buffer), and injection
solvent concentrate (75 mM sodium phosphate, pH 2.5) were
all acquired from MicroSolv Technology (Long Branch, NJ).
Deionized and high purity water (HPLC-grade water) were
obtained from a Millipore Synergy 185 water system
(Bedford, MA).
Instrumentation and Procedures
An Agilent Model HP3D CE Capillary Electrophoresis
System fitted with a diode array detector (Waldbronn,
Germany) was used for CE separations. New, bare silica
capillaries were conditioned following the same procedure used
for regular analysis. Capillaries were first flushed with 0.1 N
sodium hydroxide for 1 minute, followed by water for 1 minute,
then CElixir Reagent A for 1 minute, and finally the run buffer
for 2 minutes. 1.0 mL polypropylene vials were used as
reservoirs for 0.1N sodium hydroxide solution and for the run
buffer; while 2.0 mL glass vials were used as reservoirs for the
remaining flush solutions, waste vials, and samples. 0.1N
sodium hydroxide and run buffer vials were fill with 500 L of
liquid, while samples and flush vials containing CElixir
Reagent A and water, respectively, were filled with 1000 L of
liquid. Waste vials were filled with 500 L of water.
Standard and Sample Preparation
An injection solvent concentrate was diluted with 1:20
HPLC-grade water. For standard solutions, an appropriate
amount of standard dextro and levo isomers of
methamphetamine HCl, amphetamine sulfate, ephedrine HCl,
1
Figure 1 - Dynamically coated CE separation of standard mixture of (a) l-pseudoephedrine, (b) d-ephedrine,
(c) l-amphetamine, (d) l-ephedrine, (e) d-amphetamine, (f) l-methamphetamine, (g) d-methamphetamine,
(h) d-pseudoephedrine, (i) n-butylamphetamine (1), and (j) n-butylamphetamine (2). CE conditions are described in the
experimental section.
Microgram Journal, Volume 8, Number 1
25
l-methamphetamine,
Abundance
TIC: d_methTPC.D
17.81
130000
120000
110000
100000
90000
80000
70000
60000
50000
40000
30000
20000
10000
17.05
5.57
4.00
6.00
8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00 24.00 26.00
Time-->
Figure 4 - GC TPC separation of d-methamphetamine. Capillary 30 m x 0.25um x 0.25mm DB-17, temperature programming
120
13.704 - l-methamphetamine
100
80
60
40
20
0
140
160
13.902 - d-methamphetamine
-20
10
11
12
13
14
15
min
RMt
0.587
0.607
0.649
0.671
0.683
0.729
0.733
0.743
0.783
0.791
0.824
0.831
0.841
0.848
0.852
0.857
0.857
0.860
0.862
0.866
0.867
0.868
0.869
0.874
0.879
0.883
0.897
0.902
0.907
0.909
0.948
0.987
1.000
1.019
1.030
1.031
1.037
1.051
1.074
1.085
1.092
1.101
1.104
1.157
1.160
1.162
1.169
1.180
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