Development of a method Sin-QuEChERS for the determination of multiple pesticide residues in oilseed samples

Main Article Content

J. Hua
A. Fayyaz
H. Song
M.R. Tufail
Y. Gai


Sin-QuEChERS, oilseeds, multiple pesticide residues, monitor


The determination of pesticide residues in oilseeds is a formidable challenge because compound pesticides are widely used in farming oilseeds. In this work, a novel method named Sin-QuEChERS (single-step, cheap, effective, rugged, safe) was established for the analysis of multiple pesticide residues in oil-bearing crop samples (rapeseed, peanut, sesame and melon seeds), based on the improvement of QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach. In the Sin-QuEChERS method, acetonitrile was used for sample extraction and primary-secondary amine (PSA) using C18 cartridge as purification media. By using Sin-QuEChERS, 38 pesticide residues in 4 oilseeds were detected by high performance liquid chromatography mass spectrometry (HPLC-MS/MS) within 5 min. and the correlation coefficient was more than 0.99. The average recoveries were 80.2 to 99.8%, and the relative standard deviation was less than 15%. Application of Sin-QuEChERS to monitor the pesticide residues of 100 batches of oilseeds showed that the established method was high throughput, accurate, sensitive, and reliable, and the limited detection ranged from 0.006 to 0.054 mg/kg.

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Abbas, M.S., Soliman, A.S., El-Gammal, H.A., Amer, M.E. and Attallah, E.R., 2017. Development and validation of a multiresidue method for the determination of 323 pesticide residues in dry herbs using QuEChERS method and LC-ESI-MS/MS. International Journal of Environmental Analytical Chemistry 97(11): 1003-1023.
Ambrus, Á., Buczkó, J., Hamow, K.Á., Juhász, V., Solymosné Majzik, E., Szemánné Dobrik, H. and Szitás, R., 2016. Contribution of sample processing to variability and accuracy of the results of pesticide residue analysis in plant commodities. Journal of Agricultural and Food Chemistry 64(31): 6071-6081.
Andrade, G.C.R.M., Monteiro, S.H., Francisco, J.G., Figueiredo, L.A., Botelho, R.G. and Tornisielo, V.L., 2015. Liquid chromatography-electrospray ionization tandem mass spectrometry and dynamic multiple reaction monitoring method for determining multiple pesticide residues in tomato. Food Chemistry 175: 57-65.
Delcour, I., Rademaker, M., Jacxsens, L., De Win, J., De Baets, B. and Spanoghe, P., 2015. A risk-based pesticide residue monitoring tool to prioritize the sampling of fresh. Food Control 10: 1016.
Fang, Y., Tian, W., Pei, F., Li, P., Shao, X., Fan, Y. and Hu, Q., 2017. Simultaneous determination of pesticide residues and antioxidants in blended oil using a liquid-liquid extraction combined with dispersive solid phase extraction method. Food Chemistry 229: 347-353.
Golge, O. and Kabak, B., 2015. Evaluation of QuEChERS sample preparation and liquid chromatography-triple-quadrupole mass spectrometry method for the determination of 109 pesticide residues in tomatoes. Food Chemistry 176: 319-332.
Golge, O. and Kabak, B., 2018. Pesticide residues in table grapes and exposure assessment. Journal of Agricultural and Food Chemistry 66(7): 1701-1713.
Han, Y., Song, L., Liu, S., Zou, N., Li, Y., Qin, Y., Li, X. and Pan, C., 2017. Simultaneous determination of 124 pesticide residues in Chinese liquor and liquor-making. Food Chemistry 241: 258-267.
Khan, Z., Kamble, N., Bhongale, A., Girme, M., Chauhan, B.V. and Banerjee, K., 2018. Analysis of pesticide residues in tuber crops using pressurised liquid extraction. Food Chemistry 241: 250-257.
Li, J., Sun, M., Chang, Q., Hu, X., Kang, J. and Fan, C., 2017. Determination of Pesticide residues in teas via QuEChERS combined with dispersive liquid-liquid microextraction followed by gas chromatography-tandem mass spectrometry. Chromatographia 80(9): 1447-1458.
Liu, H., Yao, G., Liu, X., Liu, C., Zhan, J., Liu, D., Wang, P. and Zhou, Z., 2017. Approach for pesticide residue analysis for metabolite prothioconazole-desthio in animal origin food. Journal of Agricultural and Food Chemistry 65(11): 2481-2487.
Machado, I., Gérez, N., Pistón, M., Heinzen, H. and Cesio, M.V., 2017. Determination of pesticide residues in globe artichoke leaves and fruits by GC-MS and LC-MS/MS using the same QuEChERS procedure. Food Chemistry 227: 227-236.
Malhat, F., Boulangé, J., Abdelraheem, E., Abd Allah, O., Abd El-Hamid, R. and Abd El-Salam, S., 2017. Validation of QuEChERS based method for determination of fenitrothion residues in tomatoes by gas chromatography-flame photometric detector: decline pattern and risk assessment. Food Chemistry 229: 814-819.
Ozkan, A., 2015. Determination of pesticide residues in some oilseeds and nuts using LC-MS/MS analysis. Fresenius Environmental Bulletin 24(2A): 615-620.
Pirsaheb, M., Fattahi, N., Rahimi, R., Sharafi, K. and Ghaffari, H.R., 2017. Evaluation of abamectin, diazinon and chlorpyrifos pesticide residues in apple. Food Chemistry 15: 148-155.
Psoma, A.K., Pasias, I.N., Bletsou, A.A. and Thomaidis, N.S., 2015. Development and validation of a multi-residue method for the determination of pesticides in chios mastic gum by QuEChERS and liquid chromatography-tandem mass spectrometry. Food Analytical Methods 8(3): 624-634.
Santarelli, G.A., Migliorati, G., Pomilio, F., Marfoglia, C., Centorame, P., D’Agostino, A., D’Aurelio, R., Scarpone, R., Battistelli, N., Di Simone, F., Aprea, G. and Iannetti, L., 2018. Assessment of pesticide residues and microbial contamination in raw leafy green vegetables marketed in Italy. Food Control 85: 350-358.
Sivaperumal, P., Anand, P. and Riddhi, L., 2015. Rapid determination of pesticide residues in fruits and vegetables, using ultra-high-performance liquid chromatography/time-of-flight mass spectrometry. Food Chemistry 168: 356-365.
Song, L., Han, Y., Yang, J., Qin, Y., Zeng, W., Xu, S. and Pan, C., 2019. Rapid single-step cleanup method for analyzing 47 pesticide residues in pepper, chili peppers and its sauce product by high performance liquid and gas chromatography-tandem mass spectrometry. Food Chemistry 279: 237-245.
Wang, J., Tao, J., Yang, C., Chu, M. and Lam, H., 2017. A general framework incorporating knowledge, risk perception and practices to eliminate pesticide residues in food: a structural equation modelling analysis based on survey data of 986 Chinese farmers. Food Control 80: 143-150.
Xu, M.L., Gao, Y., Han, X.X. and Zhao, B., 2017. Detection of pesticide residues in food using surface-enhanced Raman spectroscopy: a review. Journal of Agricultural and Food Chemistry 65(32): 6719-6726.
Yang, X., Luo, J., Duan, Y., Li, S. and Liu, C., 2018. Simultaneous analysis of multiple pesticide residues in minor fruits by ultrahigh-performance liquid chromatography/hybrid quadrupole time-of-fight mass spectrometry. Food Chemistry 241: 188-198.