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The significance of sample grinding is frequently disregarded during the development of analytical methods, which are often validated with spiked samples that may not accurately reflect incurred residues. This study investigated the particle size of ground beans as a key factor in optimizing extraction efficiency in order to develop a simple quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based modified method for identifying 380 pesticides in beans using liquid chromatography–tandem mass spectrometry. The efficacy of pesticide extraction was found to be significantly affected by particle size. With small particle sizes (>40 mesh), no supernatant was recovered after QuEChERS partitioning. Therefore, a simple modification was performed before partitioning. The modified method was validated for selective extraction of pesticides, limits of quantification, linearity, accuracy, and precision. This method is simple to implement and, therefore, useful for the analysis of pesticide residues in beans. [ABSTRACT FROM AUTHOR]

This study investigated the effect of milling on the yields of incurred residues extracted from cereals. Rice, wheat, barley, and oat were soaked in nine pesticides (acetamiprid, azoxystrobin, imidacloprid, ferimzone, etofenprox, tebufenozide, clothianidin, hexaconazole, and indoxacarb), dried, milled, and passed through sieves of various sizes. The quick, easy, cheap, effective, rugged, and safe method and liquid chromatography–tandem mass spectrometry extracted and quantified the incurred pesticides, respectively. For rice and oat, the yields were higher for vortexed samples than for soaked samples. For rice, the yields improved as the extraction time increased from 1 to 5 min. The optimized method was validated based on the selectivity, limit of quantitation, linearity, accuracy, precision, and the matrix effect. For rice and barley, the average yields improved as the particle size decreased from <10 mesh to >60 mesh. For 40–60-mesh wheat and oat, all pesticides (except tebufenozide in oat) had the highest yields. For cereals, 0.5 min vortexing, 5 min extraction, and >40-mesh particle size should be used to optimize incurred pesticide extraction. [ABSTRACT FROM AUTHOR]

This study aimed to investigate the residual characteristics of pesticides drifted by unmanned aerial spray according to buffer strip, windbreak, and morphological characteristics of non-target crops, suggest prevention for drift reduction, and finally conduct a risk analysis on pesticides exceeding the maximum residue limit (MRL) or uniform level (0.01 mg/kg) of the positive list system (PLS). Non-target crops were collected around the aerial sprayed area (paddy rice) in Boryeong, Seocheon, and Pyeongtaek after UAV spray. When pesticides were detected in more than three samples, Duncan's multiple range test was performed. In cases where pesticides were detected in only two samples, an independent sample t-test was conducted (p < 0.05). The drift rate of pesticides tends to decrease by up to 100% as the buffer distance from aerial sprayed area increases or when a windbreak, such as maize, is present between two locations. Thus, the reduction of drifted pesticides could be effective if both factors were applied near the UAV spray area. Moreover, the residue of drifted pesticides was found to be the highest in leafy vegetables such as perilla leaves or leaf and stem vegetables such as Welsh onion, followed by fruit vegetables and cucurbits, owing to the morphological characteristics of crops. Therefore, selecting pulse or cereal such as soybean or maize as a farm product near the UAV spray area can be considered to minimize the drift. For pesticides that exceed the MRL or PLS uniform level, %acceptable dietary intake is 0–0.81% with no risk. Additionally, employing pesticides approved for both paddy rice and farm products in UAV spraying can effectively minimize instances where MRL or PLS are exceeded. Therefore, this study aims to provide farmers with effective guidelines for mitigating drift. Furthermore, we strive to promote stable and uninterrupted food production while facilitating the utilization of agricultural technologies such as UAV spraying to address labor shortages and ensure sustainable food security. [ABSTRACT FROM AUTHOR]

Since the introduction of the positive list system (PLS) for agricultural products in the Republic of Korea, the demand for a quick, easy multi-residue analysis method increased continuously. Herein, the quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique combined with liquid chromatography–tandem mass spectrometry was employed to optimize a method for the multi-residue analysis of 287 pesticide residues in mandarin orange and grapefruit. Method validation was conducted in terms of selectivity, limit of quantitation (LOQ), linearity, accuracy, precision, and matrix effect. All the compounds at low spiking levels (1, 2.5, 5, or 10 mg/kg) could be quantified at LOQs lower than 0.01 mg/kg (PLS level). The linearity of the matrix-matched calibration curve for each compound is in the range 0.5–50 μg/L, and its coefficient of determination (R2) is >0.990. Satisfactory recovery values of 70–120% with a relative standard deviation of ≤20% are obtained for all compounds in the mandarin orange and grapefruit samples. A negligible matrix effect (−20–20%) is observed for more than 94.8% and 85.4% of the pesticides in mandarin orange and grapefruit, respectively. Therefore, this analytical method can contribute to pesticide residue analyses of citrus fruits for routine laboratory testing. [ABSTRACT FROM AUTHOR]

Since broflanilide is a newly developed pesticide, analytical methods are required to determine the corresponding pesticide residues in diverse crops and foods. In this study, a pesticide residue analysis method was optimized for the detection and quantification of broflanilide and its two metabolites, DM-8007 and S(PFH-OH)-8007, in brown rice, soybean, apple, green pepper, mandarin, and kimchi cabbage. Residue samples were extracted from the produce using QuEChERS acetate and citrate buffering methods and were purified by dispersive solid-phase extraction (d-SPE) using six different adsorbent compositions with varying amounts of primary secondary amine (PSA), C18, and graphitized carbon black. All the sample preparation methods gave low-to-medium matrix effects, as confirmed by liquid chromatography–tandem mass spectrometry using standard solutions and matrix-matched standards. In particular, the use of the citrate buffering method, in combination with purification by d-SPE using 25 mg of PSA and a mixture of other adsorbents, consistently gave low matrix effects that in the range from −18.3 to 18.8%. Pesticide recoveries within the valid recovery range 70–120% were obtained both with and without d-SPE purification using 25 mg of PSA and other adsorbents. Thus, the developed residue analysis method is viable for the determination of broflanilide and its metabolites in various crops. [ABSTRACT FROM AUTHOR]

Pesticides which are diluted and sprayed according to the pre-harvest interval (PHI) are generally decomposed and lost through various factors and pathways, and the leftover pesticides are known as residual pesticides. This study aims to determine the dissipation of residual amounts of dinotefuran, fluazinam, indoxacarb, and thiacloprid in persimmon and the changes in the concentration of various processing products. Pesticide spraying is performed in accordance with the GAP (good agricultue practice) of Korea, and the processed products are manufactured using a conventional method after removing the skin of persimmons. The modified QuEchERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method and an optimized method using LC-MS/MS (liquid chromatography mass spectrometry) is implemented to analyze the residual pesticides. The linearity, recovery, and LOQ (limit of quantitation) are presented to verify the analysis method. The amount of residual pesticides tested decreases significantly in a time-dependent manner, regardless of the minimal dilution effect present due to growth. The residual concentration does not vary significantly during the processing stage despite the removal of the systemic pesticides, dinotefuran and thiacloprid. The residues of non-systemic pesticides, fluazinam and indoxacarb, are typically removed by the peeling removal and processing methods. The reduction factor of dinotefuran, whose residual concentration is increased, is less than 1, and the absolute amount of pesticides is decreased through processing. The results of this study can be used as the scientific basis data to ensure the safety of residual pesticides in processed products in the future. [ABSTRACT FROM AUTHOR]

• QuEChERS CEN version was modified for determine 12 acidic pesticides in cabbage and spinach. • Carbopack Z, a high surface area graphitized carbon black, was used as sorbent material. • Carbopack Z and C18 mixture showed excellent matrix component removal ability in clean-up. • The extract was 10-fold diluted before LC-MS/MS injection, which reduced matrix effect efficiently. • The method was validated following SANTE/12682/2019 directions. A quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was developed and combined with liquid chromatography–tandem mass spectrometry to analyze 12 acidic pesticides in cabbage and spinach. The extraction solvents, phase partition salts and sorbents effect was studied to optimize the method followed by dilution before sample injection. The extraction involved 5% formic acid in acetonitrile, and the liquid-liquid partition was salt-induced. Carbopack Z, a high surface area graphitized carbon black, was a new sorbent used in the clean-up. The results show that Carbopack Z effectively removes interferences with little loss of acidic pesticides. All tested pesticide recoveries were satisfactory when Carbopack Z was combined with C18 in the clean-up at optimized condition. After clean-up, the extract was subjected to 10-fold dilution to sufficiently reduce the matrix effect (<20%). The limit of quantification (LOQ) was 1–5 ng/g, and the mean recovery was between 95 and 110% with a relative standard deviation <20% (between 2% and 10%) for the spiking of three concentrations: 5, 50, and 500 ng/g. The extract was less pigmented in the modified QuEChERS method than its original version. Thus, the modified method is a useful alternative for investigating the acidic pesticide residues in cabbage and spinach. [ABSTRACT FROM AUTHOR]

An effective analytical method was optimized for residues including chlorpyrifos–methyl, deltamethrin, fenoxanil, thiobencarb and fludioxonil in mealworms, the larval form of Tenebrio molitor. They are listed for pest control during wheat cultivation and can be found in wheat-bran feed for growing mealworms in South Korea. Analytes were extracted using acetonitrile and salt packet. Four clean-up methods ((1) MgSO4 + 25 mg PSA + 25 mg C18; (2) MgSO4 + 50 mg PSA + 50 mg C18; (3) EMR-lipidTM tube; and (4) 10 mL n-hexane) were investigated and the method (1) was selected due to its robustness. Low-temperature precipitation of fat and proteins improved the recoveries. Recoveries from the Method (1) were satisfying with 70–120% with <20% relative SD at a spiking level of 0.01 mg/kg. With the simultaneous sample preparation, fenoxanil, thiobencarb and fludioxonil were analyzed by liquid chromatography tandem mass spectrometry (LC–MS/MS) and chlorpyrifos–methyl and deltamethrin by gas chromatography tandem mass spectrometry (GC–MS/MS). Quantification limits for LC–MS/MS and GC–MS/MS were 0.5 and 2.5 μg/L, respectively. No pesticides of interest were detected in 30 real samples collected across the nation. However, the data can be provided for establishing maximum residue limits for the pesticides in mealworms in response to the positive list system. [ABSTRACT FROM AUTHOR]