Optimizing of a LC-MS/MS method for the detection of high polar compounds in different matrixes

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Hazarhun G., Kumral N. A., Gümül B., Aşcı R., Kolcu A., Kumral A.

14th European Pesticide Residue Workshop, Bologna, Italy, 19 - 23 September 2022, vol.1, pp.173-174

  • Publication Type: Conference Paper / Summary Text
  • Volume: 1
  • City: Bologna
  • Country: Italy
  • Page Numbers: pp.173-174
  • Bursa Uludag University Affiliated: Yes


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.