2. Gıda Kimyası Kongresi, Antalya, Türkiye, 15 - 19 Mart 2023, ss.7
The high
polar chemicals, such as aminomethylphosphonic acid, bromate, bromide, chlorate,
chlormequat, cyromazine, diquat, ethephon, fosetly-al, mepiquat, N-acetyl-glufosinate,
perchlorate, phosphonic acid, propylene-thiourea and trimethyl sulfonium, are plant
growth regulators, fertilizers, pesticides or pesticide metabolites. Their
residual level in fresh foods is
regulated in European Union and Türkiye. But, direct analysis of these
compounds have always been challenging since they cannot be extracted easily
using Quick Polar Pesticides Extraction (QuPPe) method1. Unstable
retention times and chromatographically very long detection periods are the other
major problems of the analysis2. It is necessary to develop a more rapid
and robust chromatographic analysis method. In this study, a multi-residue
analysis method was developed and verified for the detection of polar compounds
in tomato matrix using LC MS/MS. The compounds were extracted using a methanol-based
very short
sample preparation method. All 15 compounds were analysed simultaneously in a single run with a
total analysis period of less than 4 minutes though changing column
specification and buffer formulation. The validation data of all
compounds obtained in LC-MS/MS analysis was quite reliable and were in line
with the SANTE 11312/2021 Guideline3. Calibration results for 6 concentrations from 10 to 400 μg kg−1, showed good linearity (R2 = 0.990
– 0.999). In addition, interference and retention time shift
were not detected. Average
recovery rates were between 84.03 and 119.65% for all compounds, when tested
with 10 and 50 µg kg-1 concentrations, respectively. The maximum RSD
values of repeatability (RSDr) varied between 0.74
and 18.31% for same concentrations
of the compounds. The maximum RSD values of reproducibility (RSDwR) for
same concentrations were between 2.94 and 18.62%. Low LOQ values (6.00 to 8.09
μg kg−1) were achieved for all compounds.
The validated LOQ values were under the lowest Maximum Residue Limits of European
Union of the compounds for tomato sample. This
study was funded by Perla Fruit Company with the grant number ULUTEK STB079417.