Analysis of paspalic acid, lysergic acid, and iso-lysergic acid by capillary zone electrophoresis with UV- and quadrupole time-of-flight mass spectrometric detection

CZE was investigated for separation of lysergic, iso‐lysergic, and paspalic acid. BGEs were optimized regarding separation selectivity and analysis time as well as MS compatibility. BGEs using asparagine, Na‐tetraborate, or ammonium acetate yielded satisfactory resolution when 40% of methanol was ad...

Full description

Saved in:
Bibliographic Details
Published in:Electrophoresis 2014-05, Vol.35 (9), p.1329-1333
Main Authors: Himmelsbach, Markus, Ferdig, Matthias, Rohrer, Thomas
Format: Article
Language:English
Subjects:
Capillary electrophoresis
Claviceps
Electrophoresis
Electrophoresis, Capillary - methods
Fermentation
Limit of Detection
Linear Models
Lysergic acid
Lysergic Acid - analogs & derivatives
Lysergic Acid - analysis
Lysergic Acid - chemistry
Lysergic Acid - metabolism
Mass Spectrometry - methods
Methyl alcohol
Paspalic acid
Quadrupole time-of-flight mass spectrometry
Quadrupoles
Recovery
Repeatability
Reproducibility
Reproducibility of Results
Separation
Spectrophotometry, Ultraviolet
Citations: Items that this one cites
Items that cite this one
Online Access:Get full text
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary:CZE was investigated for separation of lysergic, iso‐lysergic, and paspalic acid. BGEs were optimized regarding separation selectivity and analysis time as well as MS compatibility. BGEs using asparagine, Na‐tetraborate, or ammonium acetate yielded satisfactory resolution when 40% of methanol was added and the pH adjusted to 8.3. Applying acidic BGEs also allowed fast separations but the poor stability under acidic conditions of the selected analytes prevented further use. With ultraviolet (UV) detection, LODs were 0.45 and 0.40 mg/L for paspalic acid and lysergic acid, respectively. Run‐to‐run precision of peak areas was 1.8% for lysergic acid and 1.9% for paspalic acid and day‐to‐day precision was 2.4 and 4.0%, respectively. When MS detection was used LODs improved to 0.09 mg/L for paspalic acid and 0.07 mg/L for lysergic acid. Repeatability results were excellent for a CZE‐MS method without internal standard ranging from 3.4% for the highest standard concentration to 5.8% for the lowest concentration. Recovery and matrix effects were studied with samples taken from different stages of the manufacturing process and yielded an average recovery of 100.8% and a RSD of 5.7%.
ISSN:0173-0835
1522-2683
DOI:10.1002/elps.201300224