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

Abstract

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%.

Analysis of Ergot Alkaloids

“…UV and fluorescence detection methods were used. CZE has been used to determine lysergic acid, iso -lysergic acid and the related paspalic acid in reaction mixtures [ 43 ]. The method was made compatible with mass spectrometric Time of Flight (TOF) detection as well as UV by optimising the running background electrolytes (BGEs) which comprised methanol with asparagine, sodium tetraborate, or ammonium acetate at alkaline pH.…”

Construction of an efficient Claviceps paspali cell factory for lysergic acid production

“…Supplementary Table S3 indicated the attribution of 1 H and 13 C NMR data for LA and ILA. Due to its instability, LA could be partially converted to its isomer ILA ( Stoll et al, 1949 ; Himmelsbach et al, 2014 ; Yao et al, 2022 ). The percentages of LA were stabilized at around 45%, while the percentages of ILA were stabilized at around 55%.…”

Capillary electrophoresis in phytochemical analysis (2014–2017)

“…Although UV had been the most frequently used detection method in CE, MS was also widely used due to the high sensitivity and selectivity. Few examples are determination of mushroom toxins ibotenic acid, muscimol and muscarine in human urine , fingerprinting analysis of flavonoids in Ginkgo biloba herbal supplements , and fast determination of harmala alkaloids in edible algae by CE‐MS; Differential detection of Rhizoma coptidis by CE‐MS with a nanospray interface ; Characterization of hydrothermally isolated xylan from beech wood by CE‐laser‐induced fluorescence (LIF) and MS detection ; Analysis of paspalic acid, lysergic acid, and iso‐lysergic acid with UV and Q‐TOF/MS detection ; Dereplication of known nucleobase and nucleoside compounds in natural product extracts by CE‐high resolution mass spectrometry (HR‐MS) ; Separating and determining physcion, chrysophanol and aloe‐emodin in rhubarb and quantifying palmatin, columbin, cepharanthine, menisperine, magnoflorine and 20‐hydroxyecdysone in Radix tinosporae by NACE‐MS.…”