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Inclusion of 1-naphthylacetic acid and 2-(1-naphthyl)acetamide into three typical multiresidue methods for LC/MS/MS analysis of tomatoes and zucchini.

A. Lozano, A. Pérez-Parada, H. Heinzen and Amadeo R. Fernandez-Alba.

2012, Journal of AOAC International, 95 (5) , 1520-1527


In spite of high plant growth regulator application rates, little has been reported in the literature on determination of their residues in fruits and vegetables. This would be useful in monitoring good manufacturing practices and overall safety through the enforcement of maximum residue levels (MRLs).
The present work describes method validation for the determination of 1-naphthylacetic acid (NAA) and 2(1-naphthyl)acetamide (NAAm) in tomato and zucchini using the mini-Luke, ethyl acetate (EtOAc) and acetate-buffered quick, easy, cheap, effective, rugged, and safe (QuEChERS) methods.
Samples were spiked at two different levels: 50 and 100 μg/kg for NAA and 20 and 100 μg/kg for NAAm. These compounds were analyzed within the same chromatographic run with LC coupled to triple quadrupole MS (LC/(QqQ)MS/MS) in positive and negative electrospray ionization [ESI(+) and ESI(-)] modes for NAAm and NAA, respectively. For analyte confirmation, LC/ESI(-)QTOF-MS was also investigated given that NAA has only one multiple reaction monitoring transition (185.1→140.9 m/z). These three common methods were used to determine linearity, recoveries, precision (RSD), matrix effects, repeatability, and reproducibility (n = 5) for the selected matrixes.
In terms of the Directorate-General for Health and Consumers (DG-SANCO) guidelines, only insignificant differences were found for the multiresidue methods tested, regardless of the commodity. Matrix-matched calibration was used, and LODs were below 10.1 μg/kg for NAA and 6.0 μg/kg for NAAm, which were lower than the MRLs established in current European Union legislation for these compounds.
Obtained recoveries for NAA ranged from 87 to 107% with RSD values below 10% for mini-Luke, 83 to 107% with RSD <11% for EtOAc, and 76 to 85% with RSD ≤7% for QuEChERS. NAAm recoveries ranged from 74 to 102% with RSD ≤ 15% for mini- Luke, 76 to 97% with RSD <4% for EtOAc, and 76 to 93% with RSD ≤ 5% for QuEChERS. The linearity of the response over two orders of magnitude was demonstrated (r2 > 0.996) for all methods used. Good repeatability and reproducibility in terms of RSD were obtained (11.3-17.8%) for these analytical methods. The results were acceptable within the studied ranges for both analytes in all methods. As these multiresidue methods are used at the present time in many laboratories, this survey indicates that these analytes should be included in their monitoring scope.


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Published 01-04-2013, 09:45:18

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