QuEChERS Method Combined with Gas- and Liquid-Chromatography High Resolution Mass Spectrometry to Screen and Confirm 237 Pesticides and Metabolites in Cottonseed Hull

Abstract

Cottonseed hull is a livestock feed with large daily consumption. If pesticide residues exceed the standard, it is easy for them to be introduced into the human body through the food chain, with potential harm to consumer health. A method for multi-residue analysis of 237 pesticides and their metabolites in cottonseed hull was developed by gas-chromatography and liquid-chromatography time-of-flight mass spectrometry (GC-QTOF/MS and LC-QTOF/MS). After being hydrated, a sample was extracted with 1% acetic acid in acetonitrile, then purified in a clean-up tube containing 400 mg MgSO4, 100 mg PSA, and 100 mg C18. The results showed that this method has a significant effect in removing co-extracts from the oily matrix. The screening detection limit (SDL) was in the range of 0.2–20 μg/kg, and the limit of quantification (LOQ) was in the range of 0.2–20 μg/kg. The recovery was verified at the spiked levels of 1-, 2-, and 10-times LOQ (n = 6), and the 237 pesticides were successfully verified. The percentages of pesticides with recovery in the range of 70–120% were 91.6%, 92.8%, and 94.5%, respectively, and the relative standard deviations (RSDs) of all pesticides were less than 20%. This method was successfully applied to the detection of real samples. Finally, this study effectively reduced the matrix effect of cottonseed hull, which provided necessary data support for the analysis of pesticide residues in oil crops.

Assessing the Quality of Burkina Faso Soybeans Based on Fatty Acid Composition and Pesticide Residue Contamination

“…Contrary to previous data, our study did not unambiguously detect some FAs (oleic acid, stearic acid and α-linolenic acid) usually found in soybeans. These results confirm the influence of the germplasm on the fatty acid content of the seeds, which has been explained by the duration of seed filling, including the time to maturity [ 10 , 11 , 12 , 13 , 14 , 15 , 16 , 17 , 18 , 19 , 20 , 21 , 22 , 23 , 24 ]. In 2019, Seym et al found the highest concentrations of linoleic acid (C18:2) in industrially processed soybean oils, compared to myristic acid (C14:0), palmitic acid (C16:0), palmitoleic acid (C16:1), stearic acid (C18:0), oleic acid (C18:1), and linolenic acid (C18:3) [ 25 ].…”

“…Nowadays, the “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) method is an accepted analysis and extraction of pesticides in plant materials [ 16 ], especially in different plant extracts, such as vegetables containing high amounts of oils [ 15 ]. In 2022, Tong et al combined the advantages of QuEChERS and gas and liquid chromatography high-resolution mass spectrometry to analyze fatty acid compositions and levels of pesticide residues [ 17 ]. It was confirmed that such a combination of analysis methods is suitable for the pesticide multiresidue determination of soybean-based beverages in routine laboratory analyses.…”

Advances in Accurate Quantification Methods in Food Analysis

“…The other three manuscripts focus on multi-pesticide analysis via HRMS. Chen and coworkers coupled the QuEChERS method with time-of-flight mass spectrometry for hundreds of pesticides in cottonseed hull [12] and raw milk samples [13]. For the oily samples, acetonitrile with 1% acetic acid was selected as an extraction solvent, followed by purification with MgSO 4 , C 18 , or primary secondary amine sorbents.…”