Enantiomeric determination and evaluation of the racemization process of atropine in Solanaceae seeds and contaminated samples by high performance liquid chromatography-tandem mass spectrometry
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URI: http://hdl.handle.net/10835/4969
DOI: https://doi.org/10.1016/j.chroma.2016.10.047
DOI: https://doi.org/10.1016/j.chroma.2016.10.047
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2016Resumen
A new method has been developed for the enantioselective separation of (−) and (+) hyoscyamine in
Solanaceaes seeds and contaminated buckwheat. Chromatographic separation was optimized, evaluating
two chiral columns, Chirobiotic V and Chiralpal-AY3. Better resolution was obtained using a ChiralpakAY3
column, utilizing as mobile phase ethanol (0.1% diethanolamine). An extraction procedure based
on a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) was applied, using water and
acetonitrile containing 1% of acetic acid, and a clean-up step utilizing primary secondary amine (PSA) and
graphitized carbon black (GCB) as sorbents. The extract was diluted with ethanol (50/:50, v/v) prior to
chromatographic analysis, and the separation was carried out avoiding the racemization during this stage.
Enantiomerization process of atropine was studied in samples at different conditions such as temperature
(30, 50 and 80 ◦C) and pH (3, 5, 7 and 9), observing that racemization ...
Palabra/s clave
Atropine
(−)-Hyoscyamine
Solanaceaes seeds
Buckwheat
Chiral separation
Racemization process