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J AOAC Int. 2017 May 1;100(3):640-646. doi: 10.5740/jaoacint.17-0047. Epub 2017 Mar 18.

Determination of Triazines and Triazoles in Grapes Using Atmospheric Pressure Matrix-Assisted Laser Desorption/Ionization High-Resolution Mass Spectrometry.

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Council of Scientific and Industrial Research-National Chemical Laboratory, Chemical Engineering Division, Dr. Homi Bhabha Rd, Pune 411 008, India.
Indian Council of Agricultural Research, National Research Centre for Grapes, National Referral Laboratory, PO Manjri Farm, Solapur Rd, Pune 412 307, Maharashtra, India.


A chromatography-free atmospheric pressure matrix-assisted laser desorption/ionization high-resolution mass spectrometry (AP-MALDI HRMS) method is described for the simultaneous and quantitative detection of triazines and triazoles in grapes. The analytes were detected reproducibly with high mass accuracy (mass error within 5 ppm) and further confirmed by collision-induced dissociation fragmentation in tandem MS. The LODs and LOQs for all the analytes were found to be in the nanogram per gram level (15-20 ng/g LOQ). Internal standard-normalized high-resolution accurate mass-extracted (HR-AM) peak intensities of the detected ions were used to generate the concentration response curves. Linearity (with R2 values around 0.99) was obtained for these curves within a concentration range of 20-200 ng/g of the individual analytes. The accuracy and precision of the method were further established using QC samples. Validation and performance comparison of the AP-MALDI HRMS method with an existing standard method using LC with triple quadrupole MS was carried out (evaluating sensitivity, accuracy, precision, and analysis time) using 20 table-grape field samples after QuEChERS extraction.

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