Determination of Calystegines in Several Tomato Varieties Based on GC-Q-Orbitrap Analysis and Their Classification by ANOVA.

In this study, several calystegines (A3, A5, B1, B2, B3, B4, and C1) were determined in tomato. A simple extraction followed by a derivatization step with silylating agents was performed prior to their analysis by gas chromatography coupled to high resolution mass spectrometry (GC-HRMS-Q-Orbitrap), which allowed the monitoring of several ions at accurate mass. The validation of the method has provided suitable values of linearity, trueness (73.7-120.0%), and precision (≤20.0%, except for calystegines B3 and B4 at 0.5 mg/kg). The limit of quantitation was set at 0.5 mg/kg for all analytes. The validated method was successfully applied to the analysis of nine different tomato varieties, and calystegines A3, A5, B2, and C1 were found at concentrations ranging between 0.65 mg/kg (C1) and 12.47 mg/kg (B2). Tomato varieties were classified according to their calystegines content by applying an analysis of variance (ANOVA).

Analytical methods, occurrence and trends of tropane alkaloids and calystegines: An update.

In the last years, the interest in secondary metabolites from plants has been growing, and even more if they have or would have medical applications, as it happens with tropane alkaloids and calystegines. Therefore, the number of analytical methods for the analysis of these compounds has been increasing. In this review, the extraction methods as well as the chromatographic separation and detection techniques based on mass spectrometry to determine tropane alkaloids and calystegines in plant raw material and food have been described. Finally, a summary of the natural occurrence of tropane alkaloids and calystegines in the studied matrices, as well as their accidental presence in food, is presented, highlighting current and future determination trends.

Simultaneous analysis of tropane alkaloids in teas and herbal teas by liquid chromatography coupled to high-resolution mass spectrometry (Orbitrap).

A new method has been developed for the simultaneous determination of 13 tropane alkaloids in tea and herbal teas using high-performance liquid chromatography coupled to an Exactive-Orbitrap analyzer. A mixture of methanol, water, and formic acid was used for the extraction of the target compounds followed by a solid-phase extraction step. The validated method provided recoveries from 75 to 128% with intra- and interday precision lower than or equal to 24% (except for apoatropine). Limits of quantification ranged from 5 to 20 µg/kg. Eleven tea and herbal tea samples and two contaminated samples with Datura stramonium seeds were analyzed. Tropane alkaloids were detected in six samples with concentrations from 5 (apoatropine) to 4340 µg/kg (sum of physoperuvine, pseudotropine, and tropine), whereas concentrations from 5 (apoatropine) to 1725 µg/kg (sum of physoperuvine, pseudotropine, and tropine) were found in the contaminated samples.