Development and Validation of a Rapid and Sensitive Lc-Ms/Ms Approach for Alkaloids Testing in Different Lupin Species

The Fate of Quinolizidine Alkaloids During the Processing of Lupins (Lupinus Spp.) for Human Consumption

“…In contrary to what was reported by Khedr et al (2023), the extraction method (70/30 methanol/water) resulted in little adverse matrix effects and satisfactory matrix recoveries, with average recoveries within the range of 70% and 120%. An overview of average recoveries at three concentration levels is given in S13.…”

A New Fluorescence Detection Method for Tryptophan- and Tyrosine-Derived Allelopathic Compounds in Barley and Lupin

“…The UPLC HSS T3 column resulted in being the suitable choice for this application as it is a low ligand density C18 column that shows enhanced retention of polar compounds and metabolites by reversed phase liquid chromatography, and displays a balanced retention of polar and hydrophobic molecules [51,52]. Moreover, it contributed to a time of analysis of 10.5 min, which is relatively short compared to previously described runs lasting more than 30 min, and it is comparable to the shorter times of 6 min runs performed by Khedr et al on LC-MS/MS [53][54][55]. The precision of the method for the measurement of gramine was assessed on pooled seeds of lupin.…”

“…The most recent studies suggest water/acetonitrile extraction followed by an LC-MS/MS analysis. This method reports linearity in the range of 0.55–55 mg/kg, an estimated accuracy of 93% and a relative standard deviation ((RSD) < 3.6%) [ 55 ]. Concerning the methods’ sensitivities, Ganzera et al presented LOD values ranging from 24.575 to 129.93 pmol/μL [ 63 ] for gramine and other alkaloids present in lupin (such as 13α-Hydroxylupanine and sparteine).…”

“…Gramine and other alkaloids (such as piperidine derivatives) present in lupin and barley also raise major concerns for human health and nutrition [ 80 ]. High alkaloid concentrations (200 mg/kg for animals and 100 mg/kg for humans) can cause acute anticholinergic toxicity and poisoning [ 55 ]. In fact, it is worth noting that gramine, in lupin plants, is equal in concentration to the total amount of quinolizidine alkaloids such as lupanine, sparteine, 13-hydroxylupanine and multiflorine found in the plants [ 17 ].…”

“…The limit of detection (LOD) and the limit of quantification (LOQ) were assessed to have an indicator of the sensitivity of the method. LOD and LOQ were defined as the smallest concentration at which an analyte can be confidently determined as being present in a sample and the smallest concentration that can be reported as a quantitative value with acceptable precision and accuracy, respectively, and calculated [ 55 ]. LOD and LOQ were defined as follows: LOD = 3.3σ/S’, LOQ = 10σ/S’, are the calibration curves and S’ is the slope constituted by the peak area unit response per pmol/µL of concentration.…”