Simultaneous Determination of Pyrethroid Insecticides in Foods of Animal Origins Using the Modified QuEChERS Method and Gas Chromatography-Mass Spectrometry

Kim, Byung Joon; Shu, Yang; Choi, Hoon

doi:10.3390/foods11223634

Cited by 4 publications

(8 citation statements)

References 33 publications

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“…The addition of buffer components to the partitioning salts can improve the recovery of certain polar pesticides, but it could result in a negative impact on the matrix effect. The original method is still widely used because it is more rugged and less costly compared to buffer methods [ 41 ]. Based on the results of recovery and matrix effect, the M1 and M3 were selected as the optimal extraction-partitioning procedures.…”

Section: Resultsmentioning

confidence: 99%

LC-MS/MS Method Minimizing Matrix Effect for the Analysis of Bifenthrin and Butachlor in Chinese Chives and Its Application for Residual Study

Kim

Lee

Jeong

et al. 2023

Foods

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The matrix effect refers to the change in the analytical signal caused by the matrix in which the sample is contained, as well as the impurities that are co-eluted with the target analyte. In crop sample analysis using LC–MS/MS, the matrix effect can affect the quantification results. Chinese chives are likely to exhibit a strong matrix effect when co-extracted with bifenthrin and butachlor due to the presence of phytochemicals and chlorophyll. A novel analytical method was developed to reduce the matrix effects of bifenthrin and butachlor to a negligible level in Chinese chives. The established method had a limit of quantitation of 0.005 mg/kg and correlation coefficients greater than 0.999 within the range of 0.005–0.5 mg/kg. Matrix effects were found to be negligible, with values ranging from −18.8% to 7.2% in four different sources of chives and two leafy vegetables. Compared to conventional analytical methods for the LOQ and matrix effect, the established method demonstrated improved performances. The analytical method was further applied in a residual study in chive fields. The active ingredient of butachlor 5 granule (GR) was not detected after soil admixture application, while that of bifenthrin 1 emulsifiable concentrate (EC) showed a range from 1.002 to 0.087 mg/kg after foliar spraying. The dissipation rate constant (k) of bifenthrin was determined to be 0.115, thus its half-life was calculated to be 6.0 days. From the results, PHI and safety use standards of both pesticides were suggested. The developed analytical method can be applied to accurately determine bifenthrin and butachlor residues in Chinese chives and provides a foundation for further research on the fate and behavior of these pesticides in the environment.

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Section: Resultsmentioning

confidence: 99%

LC-MS/MS Method Minimizing Matrix Effect for the Analysis of Bifenthrin and Butachlor in Chinese Chives and Its Application for Residual Study

Kim

Lee

Jeong

et al. 2023

Foods

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“…For a better understanding of the co-extractives effect, ME was estimated using both slope data (Equation ( 1)) as authors such as Kim et al [25] or Shendy et al [26], and area data (Equation ( 2)) as suggested by SANTE guidance document [20] or Rutkowska et al [24]. In the latter area equation, the response of the targeted limit of quantification (LOQ) was chosen as a method threshold at which the interferences are considered to be the strongest.…”

Section: Resultsmentioning

confidence: 99%

“…Kim et al investigated 11 pyrethroid insecticides in animal-derived foods using GC-MSMS and modified the QuEChERS method, dealing with the matrix effect using matrix-matched calibration. Matrix effects, calculated by the slope approach, were in the range from −35.8% to 56.0% under the optimized clean-up conditions [25]. QuEChERS extraction followed by GC-MS/MS determination for 216 pesticide and metabolites determination in soil was explored by Łozowicka et al Matrix effect values were obtained using a slope equation, and for most pesticides, signal enhancement was recorded, with a soft matrix effect observed for 87.0% of pesticides, moderate for 10.6%, and strong only for 2.4% of pesticides [31].…”

Section: Resultsmentioning

confidence: 99%

Matrix Effect Evaluation in GC/MS-MS Analysis of Multiple Pesticide Residues in Selected Food Matrices

Bulaić Nevistić,

Kovač Tomas

2023

Foods

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Multi-analyte methods based on QuEChERS sample preparation and chromatography/mass spectrometry determination are indispensable in monitoring pesticide residues in the feed and food chain. QuEChERS method, even though perceived as convenient and generic, can contribute to sample matrix constituents’ introduction to the measuring system and possibly affect analytical results. In this study, matrix effects (ME) were investigated in four food matrices of plant origin (apples, grapes, spelt kernels, and sunflower seeds) during GC-MS/MS analysis of >200 pesticide residues using QuEChERS sample preparation. Data analysis revealed considerable analyte signal enhancement and suppression: strong enhancement was observed for the majority of analytes in two matrices within the commodity groups with high water content—apples, and high acid and water content—grapes (73.9% MES and 72.5% MEA, and 77.7% MES and 74.9% MEA, respectively), while strong suppression was observed for matrices within the commodity groups with high starch/protein content and low water and fat content—spelt kernels, and high oil content and very low water content—sunflower seeds (82.1% MES and 82.6% MEA, and 65.2% MES and 70.0% MEA, respectively). Although strong matrix effects were the most common for all investigated matrices, the use of matrix-matched calibration for each sample type enabled satisfactory method performance, i.e., recoveries for the majority of analytes (up to roughly 90%, depending on the fortification level and matrix type), which was also externally confirmed through participation in proficiency testing schemes for relevant food commodity groups with the achieved z-scores within acceptable range ≤ |2|.

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“…Finally, selected larval samples from Experiment 3 were analyzed by a gas chromatography-mass spectrometry (GC-MS/MS) based analytical procedure after a QuEChERS extraction to determine the concentrations of these substances in the larvae. The GC-MS/MS method was used for the larval samples because it is generally more sensitive for analysis of (low-polarity) pyrethroids than LC-MS/MS (Murcia-Morales et al, 2019;Kim et al, 2022), especially in case of the comparatively high fat content of BSFL (Barragan-Fonseca et al, 2017). Based on the analyzed concentrations, carryover, defined as the concentration in the larvae as a percentage of the concentration in the feed, was calculated.…”

Section: Chemical Analysesmentioning

confidence: 99%

Effects of pyrethroid and organophosphate insecticides on reared black soldier fly larvae (Hermetia illucens)

Meijer,

Zoet,

de Rijk

et al. 2023

Insect Science

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Black soldier fly larvae (Hermetia illucens) receive growing interest as a potential alternative animal feed source. These insects may be exposed to insecticide residues in the rearing substrate. This study aimed to investigate the effects of six different pyrethroid and organophosphate insecticides on this insect species’ performance. The toxicity of two “model” substances for each of these classes (cypermethrin; pirimiphos‐methyl) was quantified, with and without the synergist piperonyl butoxide (PBO). Critical effect doses corresponding to 10% yield (CED10) for cypermethrin (0.4 mg/kg) and pirimiphos‐methyl (4.8 mg/kg) were determined. The addition of PBO to cypermethrin enhanced its relative potency with a factor 2.6. These data were compared against the relative toxicity of two analogue substances in each class (permethrin, deltamethrin; chlorpyrifos‐methyl, malathion). Results suggest that exposure to concentrations complying with legal limits can cause significant reductions in yield. Exposure to multiple substances at lower concentrations resulted in negative additive and synergistic effects. Of the tested substances, deltamethrin was most toxic, causing 94% yield at 0.5 mg/kg. Analytical results suggested that transfer of tested substances to the larval biomass was substance‐ and concentration‐specific, but appeared to be correlated to reduced yields and the presence of PBO. Transfer of organophosphates was overall low (<2%), but ranged from 8% to 75% for pyrethroids. Due to very low limits in insect biomass (∼0.01 mg/kg), high transfer may result in noncompliance. It is recommended that rearing companies implement lower contractual thresholds, and that policymakers consider adjusting legally allowed maximum residue levels in insect feed.

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Simultaneous Determination of Pyrethroid Insecticides in Foods of Animal Origins Using the Modified QuEChERS Method and Gas Chromatography-Mass Spectrometry

Cited by 4 publications

References 33 publications

LC-MS/MS Method Minimizing Matrix Effect for the Analysis of Bifenthrin and Butachlor in Chinese Chives and Its Application for Residual Study

LC-MS/MS Method Minimizing Matrix Effect for the Analysis of Bifenthrin and Butachlor in Chinese Chives and Its Application for Residual Study

Matrix Effect Evaluation in GC/MS-MS Analysis of Multiple Pesticide Residues in Selected Food Matrices

Effects of pyrethroid and organophosphate insecticides on reared black soldier fly larvae (Hermetia illucens)

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