Journal of Chromatography B, 1038 (2016) 19–25
Contents lists available at ScienceDirect
Journal of Chromatography B
jou rn al hom ep age: www.elsevier.com/locate/chromb
Amphetamine and derivatives in natural weight loss pills and dietary
supplements by capillary electrophoresis-tandem mass spectrometry
Vagner Bezerra dos Santos
a
, Daniela Daniel
b
, Melina Singh
c
,
Prof. Dr. Claudimir Lucio do Lago
a,∗
a
Department of Fundamental Chemistry, Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes, 748, CEP 05508-000 São Paulo, SP, Brazil
b
Agilent Technologies, Alameda Araguaia, 1142, CEP 06455-000 Barueri, SP, Brazil
c
Bishop’s University, Sherbrooke, Canada
a r t i c l e i n f o
Article history:
Received 5 July 2016
Received in revised form 14 October 2016
Accepted 16 October 2016
Available online 17 October 2016
Chemical compounds studied in this article:
Amphetamine (PubChem CID 3007)
-methylphenylethylamine (PubChem CID
11398)
Phentermine (PubChem CID 4771)
Methamphetamine (PubChem CID 10836)
Methylenedioxyamphetamine (PubChem
CID 297310)
Methylenedioxymethamphetamine
(PubChem CID 1615)
Methylenedioxyethylamphetamine
(PubChem CID 3057998)
Keywords:
Capillary electrophoresis
Tandem mass spectrometry
Amphetamines
Amphetamine derivatives
Natural weight loss pills
Illegal drugs
a b s t r a c t
A capillary electrophoresis-tandem mass spectrometry (CE-MS/MS) method for amphetamine (AM),
phentermine (PTM), methamphetamine (MAM), methylenedioxyamphetamine (MDA), methylene-
dioxymethamphetamine (MDMA), and methylenedioxyethylamphetamine (MDEA) in commercial
samples of homeopathic and phytotherapic medicines and dietary supplements is presented. The sam-
ples were submitted to a modified QuEChERS extraction procedure (at apparent pH 13) followed by
electrophoretic separation in 0.1 mol L
−1
formic acid electrolyte (pH 2.4) and detection by ESI–MS/MS. A
polyvinyl alcohol coated capillary was employed to prevent the adsorption of the analytes to the capillary
wall. The limits of detection and quantitation were from 0.02 to 0.06 g L
−1
and from 0.06 to 0.21 g L
−1
,
respectively, with recovery ranging from 85 to 123% and the standard deviations were not greater than
6.1%. In addition, the separation occurs in less than six minutes.
© 2016 Elsevier B.V. All rights reserved.
1. Introduction
The characterization and quantification of chemical substances
in a wide variety of matrices is a challenge faced by forensic
scientists. Many forensic samples are complex mixtures, such as
biological extracts or debris associated with the crime scene, and
analysis generally requires separation prior to identification of
chemical species [1,2]. This task has traditionally been carried out
∗
Corresponding author at: Instituto de Química – Universidade de São Paulo, Av.
Prof. Lineu Prestes 748, CEP 05508-000, São Paulo, SP, Brazil.
E-mail addresses: vagnerbs@ufpa.br (V.B. dos Santos), daniel@agilent.com
(D. Daniel), MSINGH13@ubishops.ca (M. Singh), claudemi@iq.usp.br (C.L. do Lago).
using gas chromatography (GC) [3–7] and high-performance liq-
uid chromatography (HPLC) [8–19]. Capillary electrophoresis has
proven to be a good alternative to classical techniques for forensic
analysis. CE has the potential to provide more rapid separations and
higher number of plates than are generally achieved by HPLC, and it
can be applied to separation of thermally unstable analytes, in con-
trast to GC [2,20]. In this sense, the use of capillary electrophoresis
(CE) [1,21–23], as analytical separation technique, coupled to mass
spectrometry (MS), as the detection method, can provide signifi-
cant advantages by combining the high separation efficiency of CE
with the identification power of MS [20,24–29].
Amphetamine and its derivatives are powerful stimulants
of the central nervous system, and the abuse of amphetamine
(AM), methamphetamine (MAM), phentermine (PTM), and
http://dx.doi.org/10.1016/j.jchromb.2016.10.019
1570-0232/© 2016 Elsevier B.V. All rights reserved.