Analysis of MDMA in Plasma Samples with LCMS – AppNote

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September 27, 2013
Bill Ciccone

AppNotes Cogent Phenyl Hydride / AppNotes Library / AppNotes Pharmaceuticals / AppNotes Reversed Phase Methods / ARTICLES, APPNOTES, FAQ

Methylenedioxymethamphetamine Analyzed with MS
Click HERE for Column Ordering Information.

Under the described conditions, MDMA was retained and eluted as a Symmetrical Peak. The Sensitivity of the Method is very good and comparable to that reported with GCMS Detection [1]. Matrix effects were of minor extent and reproducible and hence should not compromise Quantification. The Method can be used for Forensic Research and Clinical Analysis.

Chromatogram for MDMA
MDMA Chemical Structure

Peak:
(±)-3,4-Methylenedioxymethamphetamine, m/z 194.1176 [M+H]+

Method Conditions
Column: Cogent Phenyl Hydride™, 4μm, 100Å
Catalog No.: 69020-05P-2
Dimensions: 2.1 x 50mm
Mobile Phase:
—A: DI Water / 0.1% Formic Acid (v/v)
—B: Acetonitrile / 0.1% Formic Acid (v/v)
Gradient:

Time (minutes)	%B
0	10
1	10
6	90
7	10

Post Time: 3 minutes
Flow rate: 0.4mL / minute
Injection vol.: 1μL
Sample Preparation: 50 μl of Acetonitrile was mixed with 50μl of plasma for protein precipitation. The samples were centrifuged (16000×g for 15 minutes), and the supernatant was filtered through a 0.45μm Nylon Syringe Filter (MicroSolv Tech Corp.) and transferred to autosampler vials for injection.
Detection: ESI – POS – Agilent 6210 MSD TOF Mass Spectrometer
t0: 0.9 minutes

Note: The Amphetamine derivative 3,4-methylenedioxymethamphetamine (MDMA), known also as Molly or Ecstasy, is often used or abused as a recreational drug. Because of a reported high inter-individual difference of its toxicity, sensitive analytical methods are needed. A urine test is a standard method to investigate drug abuse but the method has a very low diagnostic sensitivity and makes testing in plasma much more suitable.

Reference:
[1]. R. Kikura, Y. Nakahara, T. Mieczkowski, F. Tagliaro, Forensic Sci. Int. 84 (1997) 165–177.

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