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Article

Effects of Activated Carbon on Reduction in Pesticide Residues in Lettuce Grown in Soil Treated with Cyantraniliprole and Fluopyram

by
Seon Hwa Kim
1,
Da Jung Lim
2,
Jihyun Yoon
3 and
In Seon Kim
1,*
1
Department of Agricultural Chemistry, Institute of Environmentally Friendly Agriculture, College of Agriculture and Life Sciences, Chonnam National University, Gwangju 61186, Republic of Korea
2
Department of Research and Development, Center for Industrialization of Agricultural and Livestock Microorganisms, Jeongeup-si 56212, Republic of Korea
3
Doping Control Center, Korea Institute of Science and Technology, Seoul 02792, Republic of Korea
*
Author to whom correspondence should be addressed.
Agronomy 2025, 15(10), 2340; https://doi.org/10.3390/agronomy15102340 (registering DOI)
Submission received: 15 September 2025 / Revised: 29 September 2025 / Accepted: 2 October 2025 / Published: 5 October 2025
(This article belongs to the Special Issue Soil Pollution and Remediation in Sustainable Agriculture)
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Abstract

Reducing pesticide residues in crops is essential to ensure food safety, protect human health, and promote environmental sustainability. In this study, activated carbon (AC) was applied as a soil amendment to investigate its effect on reducing residues of the pesticides cyantraniliprole and fluopyram in greenhouse-grown lettuce. The effectiveness of AC in reducing pesticide residues varies significantly based on pesticides and crops. Pesticide dissipation patterns in the soil and a set of pesticide residues of lettuce leaf and root tissues, as well as the soil surrounding the roots for each of the tested pesticides, were analyzed using liquid chromatography with tandem mass spectrometry (LC-MS/MS) during the test periods. The results showed different pesticide dissipation patterns for cyantraniliprole, fitting the first-order kinetics, and fluopyram. Nevertheless, both AC treatments exhibited a similar decreasing tendency in which cyantraniliprole residues ranged from 0.050 to 0.064 mg/kg in leaf and 0.019 to 0.034 mg/kg in root samples, while fluopyram residues ranged from 0.168 to 0.509 mg/kg in leaf and 0.315 to 0.787 mg/kg in root samples. The highest percentage reductions were 71.3% and 77.3% for cyantraniliprole in leaf and root samples, respectively, and 79.7% and 87.5% for fluopyram in leaf and root samples. In addition, the soil samples showed a more dynamic pattern of pesticide residues compared to those of the lettuce samples. The overall findings suggest that applying AC as a soil amendment in pesticide-treated soils has a positive effect on reducing residues of cyantraniliprole and fluopyram in lettuce. Therefore, this AC-treated soil amendment could be considered a safer agricultural practice with great potential for producing safer food resources from pesticide-contaminated soils. Thus, it is expected that proper utilization of AC plays an important role in the production of safe agri-food products to manage and generate a sustainable agricultural environment.

1. Introduction

The use of pesticides in agriculture has become a foundation of modern farming, corroborating high crop yields and protecting plants from pests. However, there has been increasing public concern about environmental impact (e.g., reducing soil fertility, water and air contamination), negative effect on biodiversity (e.g., declining pollination and damaging non-target organisms), and escalating human health risk (e.g., acute and chronic poisoning, as well as residues in food) [1,2]. Therefore, it is crucial to monitor pesticide residues in plants or crops to minimize their potential risks. These pesticide residues pose significant risks to human health and food safety, especially when they exceed established maximum residue limits (MRLs). In the Republic of Korea, the positive list system (PLS), as a strict and comprehensive policy, has been implemented since 2019 to promote the safe use of pesticides for all agricultural products [3].
Importantly, fresh leafy vegetables such as lettuce, spinach, kale, and cabbage are vulnerable to pesticide contamination or residues due to the direct consumption of the vegetables without any processing or cooking [4,5]. Lettuce is one of the most widely consumed vegetables worldwide, mainly used in salads and sandwiches, and in the Republic of Korea, leaf lettuce is the second most common leaf vegetable and is primarily cultivated in greenhouses and open fields where frequent continuous cultivation methods occur [6]. The particular cropping system operated with rotational cultivation methods within short growing periods is highly responsible for the pesticide residues since the pesticides used for primary crops remain in the soil, contaminating secondary crops.
Cyantraniliprole is an anthranilic diamide insecticide belonging to the group 28 in the mode of action classification by the Insecticide Resistance Action Committee [7,8,9,10]. A wide range of target pests and its high efficacy facilitate its broad-spectrum use in various crops including vegetables, fruits, and ornamentals, as well as, rice, corn, soybeans, and cotton [7,8,11,12]. More importantly, cyantraniliprole demonstrates upward movement in plants such as tomato, cotton, bell pepper, zucchini, and cabbage via the xylem, significant acropetal movement within leaves, and translaminar movement through leaf cuticles and uptake by the corn and rice plants, followed by translocation and accumulation in the upper parts [13,14,15].
Fluopyram was initially discovered as a broad-spectrum fungicide, and later its nematicidal activity effective against Meloidogyne incognita enhanced the utilization of the pesticide [16,17]. The compound belongs to the pyridinyl ethylbenzamides class group at position 5. This specific arrangement of substituents contributes to its biological activity as a succinate dehydrogenase inhibitor (SDHI) [EC 1.3.5.1], targeting the mitochondrial respiratory chain, thus blocking electron transport in fungi, resulting in inhibition of spore germination, germ tube elongation, mycelium growth, and sporulation for controlling a broad spectrum of phytopathogens on various crops [18,19]. Within plants, fluopyram shows translaminar activity and some movement within the xylem [20].
The systemic properties with moderate solubility (between 10 and 1000 mgL−1) of cyantraniliprole and fluopyram, related to their mobility and effectiveness, imply their uptake and translocation in plants, resulting in their accumulation primarily in leafy tissues. As shown in Figure 1, two different pesticides, cyantraniliprole and fluopyram, were selected based on their possibility of persistence in the soil and mobility or uptake into crops, which may cause non-conforming agricultural products. Particularly, we considered the groundwater ubiquity score (GUS), an experimentally calculated value with pesticide persistence (half-life) and sorption potential Koc (binding affinity) for selection of the pesticides since GUS index is one of the most widely used indicators for predicting the pesticides’ potential of leaching in groundwater implying their persistence and movement in the environment [21,22,23,24]. The respective GUS values for cyantraniliprole and fluopyram are 2.59 and 3.87, interpreted as an intermediate (GUS 1.8–2.8) and a high (GUS above 2.8) potential for leachability to the environment [22] (Table 1).
Activated carbon, a highly porous material of carbon produced through physical or chemical activation processes, is derived from raw materials or biomass such as wood and agricultural residues (e.g., coconut shells) to have a vast internal surface area and a network of pores including macropores, mesopores, and micropores [25,26,27]. This structure enables it to adsorb a wide range of organic compounds, including harmful substances or contaminants [28]. Adsorption is a superficial process in which atoms, ions, or molecules adhere to the surface of an adsorbent [29,30]. Activated carbon as an adsorbent is mainly used in the field of water and air purification, medical applications, and industrial processes to remove impurities [31,32,33]. Notwithstanding that the activated carbon is a versatile adsorbent with exceptional adsorption capacity, possessing high surface area, porosity, and stability, used in various applications, research on the application of activated carbon as a soil amendment to reduce pesticide residues in plants or crops for securing food safety is rarely reported.
To fulfill a gap in the research, we hypothesized that activated carbon applied as a soil amendment diminishes the selected pesticide residues in lettuce. Hence, this study aims to evaluate the efficacy of commercially available activated carbon in reducing pesticide residues in lettuce, focusing on two systemically mobile pesticides with known environmental persistence. The trials were performed in 2021 for cyantraniliprole and in 2022 for fluopyram.

2. Materials and Methods

2.1. Chemicals and Reagents

Analytical standards, including Cyantraniliprole (98% purity) from Toronto Research Chemicals (Toronto, ON, Canada) and Fluopyram (purity ≥ 98%) from Kemidas (Gunpo, Republic of Korea), as well as other chemicals and reagents used for the LC-MS/MS analyses, were purchased from Sigma-Aldrich Corp. (St. Louis, MO, USA), unless specified otherwise. HPLC-grade organic solvents (methanol, acetonitrile) and water were obtained from J. T. Baker (Phillipsburg, NJ, USA). QuEChERS kits for sample preparation and extraction were acquired from Agilent (San Francisco, CA, USA).

2.2. Application of Pesticides and Activated Carbon

Pesticide formulation for each active ingredient (a.i.) was selected based on the most widely used products in Republic of Korea, including Benevia oil dispersion (OD) (10.26% a.i. cyantraniliprole) and Velum granule (GR) (0.5% a.i. fluopyram) purchased from Farmhannong and Bayer Crop Science Korea (Seoul, Republic of Korea), respectively. The applied rate was determined to be five times the recommended doses to maximize the pesticide uptake of the plants; A granular formulation, Velum (60 kg/10a) was mixed thoroughly with the dried soil (particle size: 4 mm or less) equivalent to 50–100 times (g/g) in a stainless serum bottle and applied evenly onto each plot of soil, while OD formulation, Benevia (1949 kg/10a) was diluted in water and then evenly sprayed on the soil. The soils for each plot were mixed by using a land management machine (Dongyang Tech., Daegu, Republic of Korea), as previously described [34]. The size of each plot for each treatment was 5 m2 (2 m × 2.5 m) with triplicate and the distance between each plot was 1 m. The plots without pesticide and AC were considered as control plots. Between the control and treatment plots, buffer zones (2 m distance) were maintained. After 7 days of the pesticide treatment, the granular activated carbon purchased from Selvas Co. (Gwangju-si, Gyeonggi-do, Republic of Korea) was applied at 5% (w/w) onto the soil for each treatment and then carefully mixed by using an agricultural farm management machine (Model KM WG420 of Dongyang Techtool, Daegu, Republic of Korea). The physicochemical properties of the activated carbon used for this study are described in Table 2. Those values had a lower surface area and pore volume, but larger pore diameter when compared with coconut-based activated carbon reported by McGinley et al. (2024) [surface area (10.52 m2g−1); pore volume (0.028 cm3g−1); pore diameter (14.5 nm)] [35].

2.3. Greenhouse Experiments

Two-year field trials for each pesticide were performed at a greenhouse (Damyang, Joennam, Republic of Korea) to investigate whether the activated carbon influences the residues of cyantraniliprole (in 2021) and fluopyram (in 2022) in lettuce plants and in soil or not. The tested soil had a loam texture containing sand 50.4%, silt 37.6%, and clay 12.0%, and basic physicochemical properties are shown in Table 3.
The lettuce (Lactuca sativa L.) seeds were purchased from Kwonnong Seed Co., Ltd. (Cheongju, Chungcheongbuk-do, Republic of Korea) and the seedlings (21 days old) were transplanted at a distance of 20 cm between plants after treating the activated carbon where the pesticides were applied 7 days before treating AC and transplanting the plants. The plants were cultivated in a conventional way under greenhouse conditions. The lettuce plants were harvested depending on their growth stages at 18, 21, 24, 27, and 31 days after the treatment (DAT) of the pesticide, Benevia (a.i. cyantraniliprole) and 23, 26, 29, 32, and 35 DAT of the pesticide, Velum (a.i. fluopyram), respectively. The control groups for sole lettuce, lettuce-applied AC without the treatment of the pesticides, and lettuce treated with the pesticides were also collected at the same time as the treatments. The plant and soil samples (1 kg per plot) were collected into polyethylene bags, stored in the ice box (at 4 °C), transported to the laboratory, and then kept in the freezer at −20 °C after removing debris. Then the frozen samples were crushed into small pieces using a high-speed homogenizer and stored at −20 °C until the extraction process.

2.4. Sample Preparation

Sample preparation for pesticide (cyantraniliprole and fluopyram) analyses in plant and soil samples was performed through the quick, easy, cheap, effective, rugged, safe (QuEChERS) method with a slight modification, optimized to meet the requirements of the organization for economic cooperation and development (OECD) that has guided pesticide residue analysis [36,37]. For the initial extraction step, a 10 g sample was added with 10 mL of acetonitrile to a 50 mL centrifuge tube. The sample was vortexed vigorously for 2 min at 2500 rpm and mixed with 4.0 g of anhydrous MgSO4 and 1.0 g of MgCl2 followed by vortexing again for 2 min at 2500 rpm. The mixture was centrifuged at 3500 rpm for 5 min to obtain the supernatant. A 1 mL aliquot of supernatant (organic solvent layer) was transferred into a 2 mL microcentrifuge tube containing anhydrous MgSO4 (150 mg), primary secondary amine (PSA, 25 mg) and graphitized carbon black (GCB, 2.5 mg), mixed for 2 min and centrifuged at 8000 rpm for 3 min; in case of soil and root samples C18 (2.5 mg) was used instead of the GCB. The resultant supernatant was used for liquid chromatography/tandem mass spectroscopy (LC-MS/MS) analyses after being passed through a 0.2 μm syringe membrane filter (PTFE-H).
The chemical stability of the pesticides in the samples during storage at −20 °C was examined by calculating the recovery data of the standard solutions spiked in the control samples at a level of 0.1 mg/L. The spiked samples were stored at −20 °C during the same period as the field sample storage period until analyzed.

2.5. LC-MS/MS Analyses and Method Validation

The prepared samples were subjected to the following analytical procedure to investigate the tested pesticide residues in lettuce and soil using a Waters model Xevo TQD and TQ MS triple stage quadrupole mass spectrometer equipped with a Waters model ACQUITYTM UPLC system. The used analytical column was a C18 stainless column (Osaka Soda CAPCELL CORE, 150 × 2.1 mm length, 2.7 μm particle size, 90 Å pore size). The mobile phase consisted of a mixture of water (A) and acetonitrile (ACN, B) with 0.1% (v/v) formic acid for both cyantraniliprole and fluopyram. The other analytical conditions including flow rates with the gradient tables for each pesticide were described in Supplementary Table S1.
The electron spray ionization (ESI) method at positive ion mode was used for acquiring LC/MS/MS spectra for the pesticides with optimized conditions as follows: capillary voltage 3.5 KV, de-solvation N2 flow 650 Lh−1, ion source temperature 150 °C, cone gas flow 50 Lh−1, de-solvation temperature 350 °C. MS/MS ions were selected based on their abundance while reflecting the compound structure, where cyantraniliprole had m/z 286.0 for quantification and m/z 177.1 for qualification [38]. The quantitative and the qualitative ions for fluopyram were m/z 208.0 and m/z 173.0, respectively [39]. Ionization conditions for each pesticide were optimized for the most abundant ion transition, summarized in Table 4. For optimizing LC-MS/MS, instrumental validation was conducted as guided by the European Commission (SANTE/11312/2021), which requires that ion ratios from sample extracts should be within ±30% (relative) of the average of calibration standards from the same sequence [40].
Six-point calibration curves for respective pesticides were constructed using standard solutions for both solvent calibration and matrix-matched calibration (MMC). MMC was used for the tested pesticides to minimize the matrix (lettuce leaves, roots, and soils) effect. For the generation of the MMC curves, the control (blank) extracts were spiked with respective standard solutions (500 mg L−1 of cyantraniliprole and 1000 mg L−1 of fluopyram) at the final concentrations of 5 to 200 μg L−1 for both cyantraniliprole and fluopyram. The limit of quantification (LOQ) at the signal-to-noise (S/N) ratio of 10:1 was calculated. The recovery tests at levels of LOQ and 10× the LOQ were conducted in triplicate.
Data are the mean of three replicates with standard deviation. One-way analysis of variance (ANOVA) Tukey’s Honestly Significant Difference (HSD) using IBM SPSS Statistics (version 20 for Windows, Chicago, IL, USA) was used to test whether the plant height and weight in pesticide treatments and pesticide with AC treatments were significantly different at p-value 0.05. Each pesticide was analyzed separately.

3. Results

3.1. Validation and Establishment of Methods

The plant and soil samples were prepared through the QuEChERS method adjusted for the extraction and clean-up of the samples. Analytical methods using liquid chromatography/tandem mass spectrometry (LC-MS/MS) for the tested pesticides were established and validated based on the OECD guidelines. The linearity of the matrix matched calibration curves for cyantraniliprole (0.005 to 0.20 mgL−1) and fluopyram (0.005 to 0.20 mgL−1) was good, with a correlation coefficient (R2) greater than 0.995 (Table 5). The matrix effects for the lettuce leaf and soil samples for each analyte ranged from −6.359 to 9.802. In case of the root samples, values of the matrix effects were 37.903 and −44.335, implying a considerable interference of the matrices on the analytes. Thus, the matrix-matched standard calibration was applied to improve accuracy since the sample matrix generally affects quantitative measurements of pesticides when the matrix effect is >±10%. The ion ratio tolerances measured were from −6.32 to 3.62, with ratios within ±30% of the guidelines for pesticide analysis set by the European Commission (SANTE/11312/2021) being considered acceptable [40]. The limit of detection (LOD) and the limit of quantification (LOQ) for the respective analytes were 0.005 mgkg−1 and 0.01 mgkg−1.
The recovery values for cyantraniliprole and fluopyram at LOQ (0.01 mgkg−1) and 10 × LOQ (0.1 mgkg−1) ranged from 73.6% to 113.0% and 81.6% and 113.7%, respectively, as shown on Table 6. The reproducibility of the analytical method (n = 3) was less than 11%. These results conformed to the guidelines of SANTE/11312/2021, which validated the determination of the pesticides or analytes in lettuce and soil samples. In connection with storage stability (at −20 °C), recovery ranges for cyantraniliprole were from 102.6% to 106.2% in plant and from 92.2% to 100.8% in soil for 56 days, and for fluopyram were from 100.2% to 101.7% in plant and from 102.9% to 109.6% in soil for 61 days, meaning that chemical instability would not be significant during the storage periods.

3.2. Pesticide Dissipation Patterns in Soil

Soil samples were obtained on each sampling day after treatment (DAT) of respective pesticides, cyantraniliprole and fluopyram, and subjected to the LC-MS/MS analyses to investigate the pesticide residues in the soils. As shown in Figure 2, cyantraniliprole residues decreased considerably from the initial concentration to approximately 25% at 14 DAT, 50% at 21 DAT, but remained about 14.4% at minimum concentration during the tested period. The regression equation (C = 141.07e−0.052t; R2 = 0.8183) of the cyantraniliprole described the first-order cyantraniliprole dissipation kinetics, where a half-life (DT50) of cyantraniliprole was approximately 13 days. However, the regression equation (C = 80.268e−0.017t; R2 = 0.2299) of fluopyram did not fit on the first-order dissipation kinetics during the tested period, where a theoretical DT50 of fluopyram was approximately 41 days. Fluopyram was considered to be a non-linear model due to the poor R2. Based on this investigation during the period, cyantraniliprole tended to dissipate more rapidly than fluopyram implying more residues of fluopyram. Furthermore, the fluctuation of fluopyram residues might be derived from adsorption or binding capacity.

3.3. Dynamics of Pesticide Residues in Lettuce Tissues and Soil

The respective residues of cyantraniliprole and fluopyram were quantified in lettuce leaf and root tissues, as well as in soil samples at each sampling DAT. As shown in Figure 3, cyantraniliprole residues of the sole pesticide treatment ranged from 0.125 to 0.193 mgkg−1 in leaf samples and 0.077 to 0.126 mgkg−1 in root samples, while cyantraniliprole residues of AC treatment tended to be decreased ranging from 0.050 to 0.064 mgkg−1 in leaf samples and 0.019 to 0.034 mgkg−1 in root samples when compared with the pesticide treatment at each sampling DAT. In soil samples, the decreasing pattern of cyantraniliprole was observed on the AC treatment at 18, 24, and 31 DAT. Fluopyram residues of the sole pesticide treatment ranged from 0.715 to 1.573 mgkg−1 in leaf samples and 2.222 to 6.291 mgkg−1 in root samples, while fluopyram residues of the AC treatment tended to be decreased, ranging from 0.168 to 0.509 mgkg−1 in leaf samples and 0.315 to 0.787 mgkg−1 in root samples when compared with the pesticide treatment at each sampling DAT. In soil samples, the decreasing pattern of fluopyram was observed on the AC treatment at all the sampling DATs.

3.4. Effects of the Activated Carbon on Pesticide Reduction in Lettuce

To evaluate the effect of AC treatment on pesticide reduction in lettuce leaf and root parts, AC treatments at each sampling time were compared with pesticide treatments and calculated for the percentage of pesticide reduction (Table 7). Values of pesticide reduction (%) showed more than 59.6% and 65.1% in leaf and root samples of cyantraniliprole with AC treatments, while in the case of fluopyram, AC treatments exhibited more than 66.4% and 73.8% reduction values in leaf and root samples, respectively. The highest reduction reached 71.3%, 79.7%, 77.3%, and 87.5% in leaf and root samples of cyantraniliprole and fluopyram treatments, respectively. The results suggest that the AC application had a positive effect on the reduction in cyantraniliprole and fluopyram (residues) in lettuce samples at all the sampling times.
Application of AC treatment as a soil amendment in cyantraniliprole or fluopyram-treated soils did not reveal statistically significant differences in plant height and weight at all the sampling days after treatment when compared with the pesticide treatments (Figure 4). This suggested that the 5% AC application rate (v/v) in soil and the application timing during the planting after 1 week of pesticide treatment is appropriate for lettuce growth without its growth inhibition.

4. Discussion

Research on activated carbon with its effectiveness in reducing pesticide residues exhibits a considerable variability depending on pesticides and crops [41,42,43]. Specific case studies on the activated carbon reducing cyantraniliprole and fluopyram in lettuce have not been reported yet. In this study, we investigated the effect of the activated carbon as a soil amendment in lettuce-grown greenhouses where the soils were treated with the respective pesticides (cyantraniliprole and fluopyram). Cyantraniliprole dissipated in soil after treatment, showing a half-life of 13 days, while the dissipation of fluopyram fluctuated, exhibiting a DT50 (41 days). Those values are shorter than the literature (32.4 and 118.8 days for cyantraniliprole and fluopyram in field soils), which may differ mainly due to the complex interactions between soil, pesticides, and activated carbon mechanistically influenced by organic matter, pH, and microbial activity [22,44]. The recovery of cyantraniliprole in root samples at LOQ and 10LOQ showed the lowest value (73.6% and 81.6%), whereas the recovery of fluopyram exhibited the highest value (113.0% and 104.7%). The difference between them may be mainly derived from matrix interference variation due to higher plant growth, inferring more root development with various root secondary compounds or metabolome profiles [45].
Residues of the tested pesticides with/without AC treatments in lettuce leaf and root tissues, as well as in the soil surrounding the roots, showed dynamic changes. The soil samples of cyantraniliprole residues showed the high residues followed by leaf and root samples, whereas the root samples of fluopyram residues showed the high residues followed by the soil and leaf samples, which insinuate that cyantraniliprole was absorbed into root tissues from soil environment and finally transported into the leaf tissues, while fluopyram was moved to the root tissues from the soil but was lowered the movement to the leaf tissues. These different residual patterns of cyantraniliprole and fluopyram may be derived from the physicochemical properties of the pesticides, particularly hydrophobicity (measured by log Kow), which significantly influence on plant uptake; more hydrophobic compounds generally show lower shoot concentrations in lettuce, following expected patterns of poor in planta transport [46]. Furthermore, the organic adsorption coefficient values reported for cyantraniliprole (155–266 mLg−1) and fluopyram (233–400 mLg−1) and electrostatic interactions were supportive to the different residual patterns, explaining that fluopyram having a higher Koc value had a stronger affinity for organic carbon, potentially in the soil, and could tend to bind to the soil with less mobility than cyantraniliprole [47].
When comparing the pesticide with/without AC treatments, the results showed a significant reduction (%) of the pesticide residues. In the AC treatments, cyantraniliprole and fluopyram residues were reduced by up to 71.3%, 79.7%, 77.3%, and 87.5% in leaf and root samples for each pesticide. These results highlight the effectiveness of AC as a soil amendment directly incorporated into the pesticide-treated soils to minimize pesticide uptake in lettuce during the continuous growing season of the lettuce, contributing to safer agricultural practices and reduced health risks related to pesticide residues to produce safe agri-food products and manage a sustainable agricultural environment. Further, this AC soil amendment is expected to help farmers comply with the PLS while preventing detection of unapproved pesticides or unintentional pesticide contamination, thus consumers are less likely to be exposed to pesticide-contaminated food.

5. Conclusions

The use of activated carbon in agricultural practices has shown promise or potential in reducing pesticide residues in lettuce tissues and soil. The tested activated carbon, derived from agricultural waste (coconut shells), showed adsorption capacity to the tested pesticides (cyantraniliprole and fluopyram), mitigating their presence in soil and reducing their uptake by lettuce. This approach not only minimizes pesticide residues in soil and plants but also helps in managing the agricultural environment sustainably. However, the effectiveness and efficiency of the activated carbon can vary based on the type of pesticide and environmental conditions, as well as the type of plants, which facilitates future work on testing the activated carbon on diverse subjects or conditions.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/agronomy15102340/s1, Table S1: Chromatographic conditions for cyantraniliprole and fluopyram.

Author Contributions

Conceptualization: I.S.K.; methodology: D.J.L. and J.Y.; validation: D.J.L., J.Y., I.S.K. and S.H.K.; formal analysis: D.J.L., J.Y., I.S.K. and S.H.K.; investigation: D.J.L. and J.Y.; resources: I.S.K.; data curation: D.J.L., J.Y. and S.H.K.; writing—original draft preparation: S.H.K.; writing—review and editing: S.H.K. and I.S.K.; visualization: S.H.K.; supervision: I.S.K.; project administration: I.S.K.; funding acquisition: I.S.K. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the Rural Development Administration, Republic of Korea (grant numbers RS-2024-00396930 and RS-PJ015956).

Data Availability Statement

All the data are represented in this paper. Further inquiries should be addressed to the corresponding author.

Acknowledgments

The authors would like to thank the anonymous reviewers of this paper.

Conflicts of Interest

The authors declare no conflicts of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript; or in the decision to publish the results.

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Agronomy 15 02340 g001
Figure 1. Chemical structure of the tested pesticides: (a) cyantraniliprole; (b) fluopyram.
Figure 1. Chemical structure of the tested pesticides: (a) cyantraniliprole; (b) fluopyram.
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Figure 2. The residual patterns of cyantraniliprole (a) and fluopyram (b) indicating the pesticide dissipation kinetics in soil during the tested period (1, 7, 14, 21, 25, 28, 31, 34, and 38 days after treatment). Data are means ± standard deviation of triplicate.
Figure 2. The residual patterns of cyantraniliprole (a) and fluopyram (b) indicating the pesticide dissipation kinetics in soil during the tested period (1, 7, 14, 21, 25, 28, 31, 34, and 38 days after treatment). Data are means ± standard deviation of triplicate.
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Figure 3. Dynamic patterns of pesticide residues in lettuce leaf and root tissues and soil. The soils were treated with cyantraniliprole (a) and fluopyram (b) with/without the activated carbon as a soil amendment, and then, seedlings of the lettuce were transplanted in the soils. The grown lettuces containing leaf and root tissues and soils were taken at sampling days after treatments. Data are means ± standard deviation of three replicates.
Figure 3. Dynamic patterns of pesticide residues in lettuce leaf and root tissues and soil. The soils were treated with cyantraniliprole (a) and fluopyram (b) with/without the activated carbon as a soil amendment, and then, seedlings of the lettuce were transplanted in the soils. The grown lettuces containing leaf and root tissues and soils were taken at sampling days after treatments. Data are means ± standard deviation of three replicates.
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Figure 4. Plant growth indicated by plant height and weight of lettuce in the soil treated with respective pesticide, cyantraniliprole (a) and fluopyram (b), where each pesticide-treated soil contained AC as a soil amendment at the harvesting time (days after treatment): Pesticide treatments on black bars; pesticide and AC treatments on gray bars. Data are the mean of three replicates with error bars representing standard deviation, analyzed by ANOVA Tukey’s HSD (p < 0.05). The same letters above the error bars are not significantly different at p < 0.05.
Figure 4. Plant growth indicated by plant height and weight of lettuce in the soil treated with respective pesticide, cyantraniliprole (a) and fluopyram (b), where each pesticide-treated soil contained AC as a soil amendment at the harvesting time (days after treatment): Pesticide treatments on black bars; pesticide and AC treatments on gray bars. Data are the mean of three replicates with error bars representing standard deviation, analyzed by ANOVA Tukey’s HSD (p < 0.05). The same letters above the error bars are not significantly different at p < 0.05.
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Table 1. Physicochemical properties of cyantraniliprole and fluopyram.
Table 1. Physicochemical properties of cyantraniliprole and fluopyram.
CyantraniliproleFluopyram
Molecular formulaC19H14BrClN6O2 C16H11ClF6N2O
Molecular weight (g/mol)473.71396.71
Water solubility (20 °C)12.33 mg/L 16 mg/L
Log Kow (1) (Hydrophobicity)1.94 at 22 °C3.3 at pH 6.5
Dissociation constant (pKa)8.8 (at 20 °C at pH 2–11)0.5 at 23 °C at pH 1
DT50 (2) (days) in Soil32.4118.8
Koc (3) (binding affinity)155–266 mLg−1233–400 mLg−1
GUS (4)2.593.87
(1) Log Kow or P, n-octanol/water coefficient; (2) DT50, half-life; (3) Koc (binding affinity), organic adsorption coefficient; (4) GUS, Groundwater ubiquity score.
Table 2. Physicochemical properties of the tested activated carbon.
Table 2. Physicochemical properties of the tested activated carbon.
C (%)H (%)O (%)N (%)S (%)O/CH/CSBET
(m2g−1) (1)		Vtotal
(cm3g−1) (2)		MPD
(nm) (3)
81.300.913.980.480.740.050.011.56810.013735.044
(1) Surface area measured by the Brunauer–Emmett–Teller (BET) Method; (2) Total pore volume; (3) Mean pore diameter.
Table 3. Physicochemical properties of the soil for greenhouse experiments.
Table 3. Physicochemical properties of the soil for greenhouse experiments.
Soil
Texture		Particle Size Distribution (%)pHOrganic Matter (gkg−1)Exchangeable Cation (cmolkg−1)
SandSiltClay
Loam50.437.612.06.895.0831.62
Table 4. Ionization conditions for cyantraniliprole and fluopyram.
Table 4. Ionization conditions for cyantraniliprole and fluopyram.
PesticideRetention Time (min)Precursor Ion (m/z)Fragment Ion (m/z)Declustering
Potential (eV)		Collision
Energy (eV)
Cyantraniliprole1.81475.1286.02314
177.141
Fluopyram3.10397.2208.01525
173.030
Table 5. Calibration equations, coefficient values of determinations, matrix effects, ion ratios, and LOQ values of the tested pesticides.
Table 5. Calibration equations, coefficient values of determinations, matrix effects, ion ratios, and LOQ values of the tested pesticides.
PesticideMatrixMatrix-Matched
Calibration Equation		R2Matrix
Effect (%) (1)		Ion Ratio
Tolerance (%) (2)		LOQ
(mgkg−1) (3)
CyantraniliproleLeafy = 6335x + 25.4321.0009.8022.030.01
Rooty = 10,099x + 87.6991.00037.903−2.800.01
Soily = 8837x + 17.7081.000−4.6923.620.01
FluopyramLeafy = 36,235x + 39.450.997−6.3592.690.01
Rooty = 21,540x + 14.5740.996−44.3351.420.01
Soily = 14,021x + 334.8260.999−5.618−6.320.01
(1) [(Slope of the line for the matrix-matched standard solution—slope of the line for the solvent standard solution)/(Slope of the line for the solvent standard solution)] × 100; (2) [(Ion ratio obtained from the sample—ion ratio obtained from the solvent standard solution)/(Ion ratio obtained from the solvent standard solution)] × 100; (3) Limit of quantification.
Table 6. Recovery of the tested pesticides fortified in the samples.
Table 6. Recovery of the tested pesticides fortified in the samples.
PesticideSampleRecovery (%) (1)
LOQ (2)10 × LOQ
CyantraniliproleLeaf84.3 ± 3.6105.5 ± 2.3
Root73.6 ± 9.781.6 ± 1.5
Soil101.4 ± 10.4113.7 ± 2.1
FluopyramLeaf94.6 ± 6.494.9 ± 4.5
Root113.0 ± 2.1104.7 ± 1.2
Soil77.7 ± 7.3102.1 ± 2.9
(1) Data are means ± SD of triplicate; (2) Limit of quantification.
Table 7. Pesticide reduction (%) in lettuce leaf and root samples.
Table 7. Pesticide reduction (%) in lettuce leaf and root samples.
PesticideDATPesticide Reduction (%) (1)
LeafRoot
Cyantraniliprole1859.6 ± 2.97 78.7 ± 2.13
2171.3 ± 0.6065.1 ± 1.62
2467.0 ± 1.0279.7 ± 1.74
2759.7 ± 2.3571.8 ± 0.53
3166.7 ± 0.7879.3 ± 1.30
Fluopyram2367.6 ± 1.5987.5 ± 0.38
2666.4 ± 1.6273.8 ± 3.81
2977.3 ± 2.1882.5 ± 2.24
3267.5 ± 1.1982.6 ± 0.86
3576.4 ± 2.3185.8 ± 0.27
(1) (Residue of pesticide treatment − Residue of AC treatment)/Average Residue of Pesticide treatment × 100. Data are means ± SD of triplicate.
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Kim, S.H.; Lim, D.J.; Yoon, J.; Kim, I.S. Effects of Activated Carbon on Reduction in Pesticide Residues in Lettuce Grown in Soil Treated with Cyantraniliprole and Fluopyram. Agronomy 2025, 15, 2340. https://doi.org/10.3390/agronomy15102340

AMA Style

Kim SH, Lim DJ, Yoon J, Kim IS. Effects of Activated Carbon on Reduction in Pesticide Residues in Lettuce Grown in Soil Treated with Cyantraniliprole and Fluopyram. Agronomy. 2025; 15(10):2340. https://doi.org/10.3390/agronomy15102340

Chicago/Turabian Style

Kim, Seon Hwa, Da Jung Lim, Jihyun Yoon, and In Seon Kim. 2025. "Effects of Activated Carbon on Reduction in Pesticide Residues in Lettuce Grown in Soil Treated with Cyantraniliprole and Fluopyram" Agronomy 15, no. 10: 2340. https://doi.org/10.3390/agronomy15102340

APA Style

Kim, S. H., Lim, D. J., Yoon, J., & Kim, I. S. (2025). Effects of Activated Carbon on Reduction in Pesticide Residues in Lettuce Grown in Soil Treated with Cyantraniliprole and Fluopyram. Agronomy, 15(10), 2340. https://doi.org/10.3390/agronomy15102340

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