Quantitative determination of trigonelline in mouse serum by means of hydrophilic interaction liquid chromatography–MS/MS analysis: Application to a pharmacokinetic study

Abstract

Trigonelline is a pyridine alkaloid found in fenugreek seeds and coffee beans. Most of the previous studies are concerned with the quantification of trigonelline along with other constituents in coffee herbs or beverages. Only a few have focused on its determination in animal or human tissues by applying different modes of HPLC with UV or MS detection. The aim of the study was to develop and validate a fast and simple method for trigonelline determination in serum by the use of hydrophilic interaction liquid chromatography (HILIC) with ESI-MS/MS detection. Separation of trigonelline was achieved on a Kinetex HILIC column operated at 35°C with acetonitrile-ammonium formate (10 mm, pH = 3) buffer mixture (55:45, v/v) as the mobile phase. The developed method was successfully applied to determine trigonelline concentration in mouse serum after intravenous administration of 10 mg/kg. The developed assay is sensitive (limit of detection = 1.5 ng/mL, limit of quantification = 5.0 ng/mL) and linear in a concentration range from 5.0 to 250.0 ng/mL. Sample preparation is limited to deproteinization, centrifugation and filtration. The application of the HILIC mode of chromatography with MS detection and selection of deuterated trigonelline as internal standard allowed a rapid and precise method of trigonelline quantification to be to developed.

Trigonelline recovers memory function in Alzheimer’s disease model mice: evidence of brain penetration and target molecule

“…Therefore, we supposed TGN had a potency of neural network repairing and aimed to clarify whether TGN improved memory dysfunction and axonal damage in 5XFAD mice, which overexpress mutated APP and PS1 genes. In addition, we investigated the brain penetration of TGN, which has not been previously reported, although absorption in the blood has been indicated in several pharmacokinetic studies 16 – 18 . Furthermore, the mechanism of action of TGN, other than antioxidative stress, was examined.…”

TLC–MS identification of alkaloids in Leonuri Herba and Leonuri Fructus aided by a newly developed universal derivatisation reagent optimised by the response surface method

“…Spot c showed two intensive peaks at m/z 138 [M + H] + and m/z 160 [M + Na] + . Its MS 2 spectrum showed an abundant ion at m/z 94 (Figure S7), corresponding to the loss of CO 2 , which was consistent with that of trigonelline 16 . Spot d exhibited an intensive molecular ion at m/z 104 [M] + , and a MS 2 fragment ion at m/z 60 (the trimethylammonium ion) (Figure S7), which are consistent with those of choline 17 .…”

A novel UPLC–MS/MS method for simultaneous quantification of trigonelline, 4‐hydroxyisoleucine, and diosgenin from Trigonella foenum‐graecum extract: Application to pharmacokinetic study in healthy and type 2 diabetic rats

“…In the present work, a novel, sensitive, reliable, and reproducible simultaneous assay has been developed and validated to quantify the bioactives using a sophisticated ultra‐performance liquid chromatography tandem mass spectroscopy (UPLC–MS/MS) method. To the best of our knowledge, there is no simultaneous UPLC–MS/MS method established to estimate TR, 4‐HI, and DG (Cheng et al, 2013; Szczesny et al, 2018; Xue et al, 2011). The validated method was applied for the estimation of pharmacokinetic parameters in normal and type 2 diabetic rats.…”