14th European Pesticide Residue Workshop, Bologna, İtalya, 19 - 23 Eylül 2022, cilt.1, ss.173-174
The residues of
high polar chemicals used as plant growth regulators, fertilizer, pesticide or
their metabolites are questionable issue in terms of food safety. To detect these
toxic chemicals for humans, a rapid and reliable chromatographic method should
be developed. In this study, a multi-residue analysis method was validated for
the detection of 11 different high polar
chemicals such as aminomethylphosphonic acid, chlorate, ethephon, fosetly-al,
glyphosate, glufosinate, maleic-hydrazine, phosphonic acid, perchlorate and
propylene-thiourea, in 4 different matrixes (tomato, chestnut, raisin and
lentil) using LC MS/MS. In this method, there are some modifications in
extraction of samples, buffer formulation and colon specifications compared with
common used QuPPe method. With this test method, the detection time for these
compounds was very short (from 1.1 min. to 8.7 min). Also, interference and
retention time shift were not observed. Results of calibration study showed
good linearity (R2 values are between 0.993 and 0.998). LOQ values
for analysed compounds were between 2.93 and 6.78 μg kg−1 in tomato;
6.36 and 9.37 μg kg−1 in chestnut, 3.89 and 8.65 μg kg−1
in raisin and 3.27 and 7.83 μg kg−1 in lentil, respectively. Although
LOQ value of oil crop matrix (chestnut) was found higher than other matrixes, all
LOQ values were under the lowest Maximum Residue Limits of the compounds (50 to
3000 µg kg-1). Average recovery rates were also detected for 10 and
50 µg kg-1 concentrations of each compound. Their recovery rates were
between 77.44 and 115.75% in tomato; 78.63 and 105.35% in chestnut, 81.24 and
116.79% in raisin and 82.54 and 111.0% in lentil, respectively, in line with lowest
(70%) and highest (120%) limits of the SANTE/12682/2019 Guideline. Recovery
rates of oil crop matrix such as chestnut, was found less than other matrixes. The
RSD values of repeatability were in the range of 0.45-7.96% in tomato; 1.11-13.13%
in chestnut, 0.93-12.74% in raisin and 0.86-10.15% in lentil, separately. Additionally,
the RSD values of reproducibility were in the range of 1.46-14.77% in tomato; 1.79-13.03%
in chestnut, 2.20-16.68% in raisin and 2.33-15.43% in lentil, separately. The
validation data of all high polar compounds obtained in LC-MS/MS analysis was
quite reliable and were in line with the SANTE/12682/2019 Guideline. This
chromatographic method was patented with the number of 2020/22810. This study
was funded with as a research project (grant number ULUTEK STB079417) by Perla
Fruit Company.