Multi-residue Analysis of Pesticides using GC-TOF/MS, ECD, NPD with QuEChERS Sample Preparation

Park, Jungwook; Kim, Ae-Kyung; Kim, Jong-Pil; Lee, Hyanghee; Park, Duckwoong; Moon, Su‐Jin; Ha, Dongryong; Kim, Eunsun; Seo, Kyewon

doi:10.7585/kjps.2014.18.4.278

Cited by 5 publications

(2 citation statements)

References 7 publications

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“…Spinosad와 spinetoram은 토양 방선균 Saccharopolyspora spinosa의 배양액으로부터 추출 된 천연 살충성분 spinosyn을 화학적으로 변형시켜 만들어진 살충제로 Lepidoptera larvae, Leafminers, Thrips 등의 해충 방제에 널리 사용 (Kim et al, 2011;Malhat, 2013)되지만 대부분 익충에게는 영향력이 적은 것으로 알려져 있다 (Duffield et al, 2000;Sparks et al, 2007; Residue analysis of spinetoram and spinosad on paprika leaf using the modified QuEChERS pre-treatment methods (Park et al, 2012;Liu et al, 2011 (Kwon et al, 2011;Lee et al, 2011;Kim et al, 2012;Park et al, 2014). 최근에는 ECD, NPD, UVD에도 적용 가능한 QuEChERS법 개발도 이루어지고 있으나 (Lee et al, 2012;Yang et al, 2013;Park et al, 2015)…”

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Residue analysis of spinetoram and spinosad on paprika leaf using the modified QuEChERS pre-treatment methods

2017

Korean Journal of Agricultural Science

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Spinosad and spinetoram are widely used insecticides for the control of lepidopteran larvae, leaf miners, and thrips; however, they might also have low toxicity toward beneficial insects like bees. Because these pesticides are easily photolyzed by ultraviolet radiation, the QuEChERS method, with its simple pretreatment procedure, is often used for analyzing residues of spinosad and spinetoram. The present study performed a residue analysis using a modified QuEChERS method by pretreating with ammonium salt. The limit of detection (LOD) of the modified method was 0.05 mg/kg and the limit of quantification (LOQ) was 0.25 mg/kg. The coefficient of determination (R 2 ) for the calibration curve was 0.999. Also, we examined any change in the adhesion of spinosad and spinetoram on the plants depending on a spray volume. The adhesion was approximately 70% when the spray volume was increased from 60 L to 120 L per 10 a whereas the adhesion was approximately 37% when the spray volume was increased from 125 L to 250 L. This showed that the amount of adhesion decreased with the higher spray volume. The efficacy result of spinetoram was that over 90% of Frankliniella occidentalis was controlled with the application volume of 125 L per 10 a. Therefore, the result of this study indicates that control of insects is effective and sufficient with a spray volume of 125 L per 10 a in paprika cultivation facilities.

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Section: Introductionunclassified

Residue analysis of spinetoram and spinosad on paprika leaf using the modified QuEChERS pre-treatment methods

2017

Korean Journal of Agricultural Science

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“…. 최근 QuEChERS (Quick, Easy, Cheap, effective, rugged and safe)법 도입 에 따라 GC-MS (mass spectrometry)를 이용한 사례가 다수 보고되고 있으며, 상추 [3,4], 토마토, 사과, 바나나 [3,5], 포도, 브로콜리 [3], 소 지방 [6], 차 [7], 계란 [8,9], 파, 배추, 완두콩 a) Pre-washed with 50 mL of n-hexane, followed by elution with ethyl acetate/n-hexane(1/5, v/v) 50 mL (I), followed by second elution with the same solvent (50 mL) (II), and followed by thrid elution with the same solvent (50 mL) (III).…”

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Development of Analytical methods for Chinomethionat in Livestock Products

Shu¹,

Kim²,

Choi³

2021

Korean Journal of Environmental Agriculture

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BACKGROUND:The analytical method was established for determination of fungicide chinomethionat in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining chinomethonat in various livestock products including beef, pork, chicken, milk and egg. Chinomethionat residual was extracted using acetone/dichloromethane(9/1, v/v) with magnesium sulfate and sodium chloride (salting outassociated liquid-liquid extraction). The extract was diluted by direct partitioning into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was finally purified with optimized silica gel 10 g. CONCLUSION:The method limit of quantitation (MLOQ) was 0.02 mg/kg, which was in accordance with the maximum residue level (MRL) of chinomathionate as 0.05 mg/kg in livestock product. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (84.8~103.0%). Reproducibilities were obtained (Coefficient of variation <5.2%), and the linearity of calibration curves were reasonable (r 2 >0.995) in the range of 0.01-0.2 μg/mL. This established analytical method was fully validated and could be useful for quantification of chinomathionat in animal commodities as official analytical method.

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Residual Multi Pesticides Screening of Dead Birds by Orbitrap High Resolution Mass Spectrometry

Lee¹,

Kim²,

Wang³

et al. 2017

Korean Journal of Environmental Agriculture

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BACKGROUND:The objective of this study was to evaluate screening method of residual multi pesticides in dead birds by Orbitrap high resolution mass spectrometry (HRMS) to identify the cause of death for birds . METHODS AND RESULTS: Extraction and clean-up method of residual pesticides in liver of dead birds was used QuEChERS (Quick Easy Cheap Effective Rugged and Safe) and method validations was conducted using liquid chromatography and gas chroamtography with triplequadrupole mass spectrometer (LC/MS/MS and GC/MS/ MS) Also, we were evaluated screening method for the determination of residual pesticides in liver of dead birds by LC and GC Orbitrap Mass Spectrometry. Results of method validations, Correlation coefficients of the matrix matched calibration curves were >0.978, and the method detection limits (MDLs) and limits of quantitation (LOQ) were 2.87 2.1 ng/g (18.4 ng/g on average) and 9.0~230 ng/g (58.5 ng/g on average). The accuracy ranged from 69.1% to 130% (103% on average), and the precision values were less than 14.8%(3.8%on average). The screening of residual pesticides in liver of dead birds by LC and GC Orbitrap HRMS was detected monocrotophos, carbofuran, carbosulfan, deltametrin, benfuracarb, carbofuran, phosphamidon, prochloraz in investigated samples. CONCLUSION: This results showed that accurate mass were extraction of residual pesticides in dead birds by Orbitrap HRMS. It suggested that this screening method is applicable to the residual pesticide analysis for the cause of death as a main tool.

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Multi-residue Analysis of Pesticides using GC-TOF/MS, ECD, NPD with QuEChERS Sample Preparation

Cited by 5 publications

References 7 publications

Residue analysis of spinetoram and spinosad on paprika leaf using the modified QuEChERS pre-treatment methods

Residue analysis of spinetoram and spinosad on paprika leaf using the modified QuEChERS pre-treatment methods

Development of Analytical methods for Chinomethionat in Livestock Products

Residual Multi Pesticides Screening of Dead Birds by Orbitrap High Resolution Mass Spectrometry

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