Rapid method for determination of chlormequat residues in tomato products by ion‐exchange liquid chromatography/electrospray tandem mass spectrometry

Abstract

A rapid method has been devised for the direct determination of chlormequat in tomato samples. No clean-up is required, and analysis uses ion-exchange liquid chromatography/tandem mass spectrometry interfaced with electrospray ionization (LC/ESI-MS/MS). A cation-exchange column was used with an aqueous ammonium acetate/acetonitrile mixture as the mobile phase under isocratic conditions. The method was validated in terms of detection limits (LOD), quantitation limits (LOQ), linearity, recovery, precision and accuracy. Good results in the low micro g kg(-1) level were obtained for the LOD and LOQ of chlormequat in tomato samples. Comparison of solvent and matrix-matched calibration curves demonstrated the absence of significant matrix effects and the feasibility of using external calibration. Linearity was established over two orders of magnitude by performing homoscedasticity and Mandel fitting statistical tests. The absence of both constant and proportional systematic errors was verified by evaluating the recovery function, demonstrating good method accuracy. Excellent precision in terms of intra-day repeatability was calculated (RSD% <3.4). Extraction recoveries from tomato products were calculated, by using a labelled internal standard (d(4)-chlormequat), to be in the 93 +/- 5-99 +/- 7% range. The applicability of the method to the determination of chlormequat residues in tomato products was demonstrated.

Fast LC/MS in the analysis of small molecules

“…Careri et al [133] report a rapid isocratic analysis for the determination of chlormequat residues in tomato prod- ucts using methanol extraction with filtration in conjunction with ion-exchange chromatography. Liu et al [134] use a small imbedded membrane (IAM) column (10 mm×3 mm) with sample pooling by ionization mode to reduce analysis time for membrane interaction studies.…”

Umweltanalytik mit Ionenchromatografie: Status quo und Zukunftsperspektiven

“…Als Nachweisgrenze wird 0,5 mg·kg -1 angegeben (Peeters et al 2001). Eine deutlich höhere Empfindlichkeit (0,88 µg·kg -1 ) offeriert die ESI-MS/MS-Detektion, wobei hier ein flüchtiger Eluent (0,2 M Ammoniumacetat mit 40 Vol.-% ACN) und eine IonPac CS 15-Trennsäule gewählt werden (Careri et al 2002).…”

Detection of Target Peptides in Foods and Feeds by Mass Spectrometry

“…Proteomics has become a potent approach for the study of proteins in complex biological systems, and it appears particularly attractive to detect target components in food and feed products such as GM, animal-derived, and allergenic proteins [58][59][60]. Mass spectrometric investigations for the detection of proteins and peptides present in diverse foods have been reviewed [58].…”