High‐throughput assay of rotenone in olive oil using atmospheric pressure chemical ionization tandem mass spectrometry

Abstract

A high-throughput method is presented for the determination of rotenone in contaminated matrices. The procedure involves atmospheric pressure chemical ionization tandem mass spectrometry with a triple-quadrupole instrument and the use as internal standard of a cycloadduct derivative of rotenone itself. The method was applied to the evaluation of the decay of rotenone in olives and olive oil at various times after exposure to the contaminant.

Identification and assay of carbohydrates in olive drupes by cesium attachment electrospray tandem mass spectrometry (ESI‐MS/MS)

“…Higher sensitivity is obtained following the fragmentation of [M + NH 4 ] + adducts of saccharides and glucosides. [3][4][5][6][7][8][9] Other approaches to monosaccharide analysis are based on (1) chloride anion, or (2) sodium cation, attachment. The assay of chlorinated species suffers, among others, by the drawback of dealing with multi-isotopic species, whereas the disadvantage of sampling sodiated derivatives is represented by the insufficient sensitivity due, in part, to undesirable multicharged adduct ion formation.…”

“…[1,2] Tandem mass spectrometry has been widely applied in the characterization and authenticity of Mediterranean olive oils. [3][4][5][6][7][8][9] The established methods for evaluating the proper degree of ripeness are mainly based on the assessment of some physical parameters such as the darkening and ripening index, [10,11] which are not applicable to all cultivars and suffer by the lack of objectivity.…”

Assay of rotenone in river water by high‐throughput tandem mass spectrometry and multiple‐reaction monitoring methodology

“…By analogy with the method previously applied to foodstuff analysis,10 the transitions m/z 395 → 192 for rotenone and m/z 514 → 192 for the internal standard were chosen for the quantitative analysis. The calibration curve was built using standard solutions of rotenone and internal standard in rotenone‐free water taken from the River Emoli in the city of Rende.…”

“…There have been very few reports of its quantitative determination by mass spectrometry7–9 and none of these papers refers to the use of an internal standard and of tandem mass spectrometry (MS/MS) methods to improve the accuracy of the analysis. Recently, the presence of rotenone in olive oil has been quantified by mass spectrometry using the cycloadduct 2 as an internal standard 10. It should be noted that compounds 1 and 2 (Scheme ) experience significantly different physicochemical environments, when sampled in olive oil or in water.…”

Isotope dilution method for the assay of rotenone in olive oil and river waters by liquid chromatography/multiple reaction monitoring tandem mass spectrometry

“…The methods most frequently used to analyze rotenone in foods are based on liquid chromatography (LC) coupled to UV detection,10, 11 or hyphenated with mass spectrometers, as for the quantitation of this phytodrug in olive oil or in river water 12, 13. Assays of this analyte have been performed, until now, by means of external standards or by rotenone derivatives used as internal standards.…”