Simultaneous Analysis of 272 Pesticides in Agricultural Products by the QuEChERS Method and Gas Chromatography with Tandem Mass Spectrometry.

The aim of this study is to develop a rapid and accurate method for simultaneous analysis of multi-residue pesticides and conduct pesticide monitoring in agricultural products produced by the production and distribution stage in Korea. The representative agricultural products were selected as brown rice, soybean, potato, mandarin, and green pepper and developed using gas chromatography with tandem mass (GC-MS/MS) for the analysis of 272 pesticide residues. The experimental samples were extracted by the QuEChERS-EN method and then cleaned up by using d-SPE, including MgSO4 and primary secondary amine (PSA) sorbents. The established method was validated in accordance with Codex CAC-GL/40, and the limit of quantitation (LOQ) was determined to be 0.01 mg/kg. A total of 243 pesticides satisfied the guidelines in five samples at three levels with values of 60 to 120% (recovery) and ≤45% (coefficient of variation, CV). The remaining 29 pesticides did not satisfy the guidelines, and these pesticides are expected to be used as a screening method for the routine inspection of agricultural products. As a result of analyzing 223 agricultural products in South Korea by applying the simultaneous analysis method, none of the detected levels in the samples exceeded the standard values based on maximum residue limits (MRLs). The developed method in this study will be used to inspect residual pesticides in agricultural products, and it is anticipated to contribute to the distribution of safe agricultural products to consumers.

Determination of Modified QuEChERS Method for Chlorothalonil Analysis in Agricultural Products Using Gas Chromatography-Mass Spectrometry (GC-MS/MS).

Chlorothalonil is an organochlorine fungicide that blocks the respiratory process of cells and persists in agricultural products because it is used extensively to prevent fungal diseases. An analytical method of chlorothalonil using the modified QuEChERS method and gas chromatography- mass spectrometry (GC-MS/MS) was developed to analyze the residue in agricultural commodities distributed in Republic of Korea. Acetonitrile, including acetic acid and formic acid, was used to compare the extraction efficiency. The extraction and purification processes were established by comparing three versions of the QuEChERS method and various dispersive solid-phase extraction (d-SPE) combinations. Ultimately, 1% formic acid in acetonitrile with QuEChERS original salts and d-SPE (PSA, C18) were selected for the extraction and clean-up procedures for method validation and establishment. Five agricultural commodities, viz., brown rice, mandarin, soybean, pepper, and potato, were examined to validate the established method, which displayed excellent linearity, with a coefficient of determination of R2 = 0.9939-0.997 in the calibration curve range of 0.002-0.1 mg/kg. The limits of detection (LOD) and quantification (LOQ) were calculated to be 0.003 mg/kg and 0.01, respectively, for the method. The LOQ value satisfied the suitable level for the Positive List System (PLS). The mean recovery of chlorothalonil was 79.3-104.1%, and the coefficient of variation was <17.9% for intra- and inter-day precision at 0.01, 0.1, and 0.5 mg/kg. The matrix effects in the five commodities were confirmed by the ion suppression effects, except for brown rice, in which a medium enhancement effect was observed at 21.4%. Chlorothalonil was detected in eight apples, one watermelon, and one cucumber. Ultimately, chlorothalonil was detected in ten agricultural products. Thus, this analytical method could be used for the routine detection of chlorothalonil in agricultural products, and the data may be used to inform and improve current food policies.

Simultaneous Screening of 322 Residual Pesticides in Fruits and Vegetables Using GC-MS/MS and Deterministic Health Risk Assessments.

The development of efficient methods for evaluating pesticide residues is essential in order to ensure the safety and quality of agricultural products since the Republic of Korea implemented the Positive List System (PLS). The objective of this research was to establish a method for the simultaneous analysis of 322 pesticide residues in fruits and vegetables (such as coffee, potato, corn, and chili pepper), using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach in combination with gas chromatography-tandem mass spectrometry (GC-MS/MS). This study introduces a robust, high-throughput GC-MS/MS method for screening the target pesticide residues in agricultural products, achieving the PLS criterion of 0.01 mg/kg LOQ. Despite some compounds not aligning with the CODEX recovery guideline, sufficient reproducibility was confirmed, attesting to the method's applicability in qualitative analyses. A health risk assessment conducted using estimated daily intake/acceptable daily intake ratios indicated low risks associated with product consumption (<0.035391%), thereby confirming their safety. This efficient method holds significant implications for the safe distribution of agricultural products, including during import inspections.

Determination of 66 pesticide residues in livestock products using QuEChERS and GC-MS/MS.

Determinations of 66 pesticide residues in different matrices including beef, pork, chicken, eggs, and milk were conducted using GC-MS/MS combined with the quick easy cheap effective rugged safe (QuEChERS) method for sample extraction. A high linearity was achieved in the concentration range from 2.5 to 1000 µg/L (R 2 ≥ 0.99), and the limit of quantification for multi-class pesticides ranged from 0.74 to 23.1 µg/kg. The recovery ranged from 70.0 to 120%, while the reproducibility of the measurements was between 0.23 and 19.9%. Monitoring was conducted for livestock products purchased from local markets. Chlorpyrifos and fenitrothion in beef and chlorpyrifos in pork were detected below the maximum residue limits for the respective samples. No detectable residues were found in the other samples. Due to its high efficiency, reproducibility, and simple analytical operation, the proposed method can be applied to the regular monitoring of multi-residue pesticides in livestock products.