Optimization of a Simplified and Effective Analytical Method of Pesticide Residues in Mealworms (<i>Tenebrio molitor</i> Larvae) Combined with GC–MS/MS and LC–MS/MS

An effective analytical method was optimized for residues including chlorpyrifos–methyl, deltamethrin, fenoxanil, thiobencarb and fludioxonil in mealworms, the larval form of <i>Tenebrio molitor</i>. They are listed for pest control during wheat cultivation and can be found in wheat-bran...

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Main Authors: Leesun Kim, Sujin Baek, Kyungae Son, Eunsun Kim, Hyun Ho Noh, Danbi Kim, Min-seok Oh, Byeong-chul Moon, Jin-Ho Ro
Format: Article
Language:English
Published: MDPI AG 2020-07-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/25/15/3518
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spelling doaj-c0b0e5d5945c4721b08a988d2e22d8a62020-11-25T03:30:31ZengMDPI AGMolecules1420-30492020-07-01253518351810.3390/molecules25153518Optimization of a Simplified and Effective Analytical Method of Pesticide Residues in Mealworms (<i>Tenebrio molitor</i> Larvae) Combined with GC–MS/MS and LC–MS/MSLeesun Kim0Sujin Baek1Kyungae Son2Eunsun Kim3Hyun Ho Noh4Danbi Kim5Min-seok Oh6Byeong-chul Moon7Jin-Ho Ro8Chemical Safety Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaChemical Safety Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaAgromaterial Assessment Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaIndustrial Insect Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaChemical Safety Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaChemical Safety Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaChemical Safety Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaChemical Safety Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaChemical Safety Division, National Institute of Agricultural Sciences, RDA, Iseo-myeon, Wanju-gun, Jeollabuk-do 55365, KoreaAn effective analytical method was optimized for residues including chlorpyrifos–methyl, deltamethrin, fenoxanil, thiobencarb and fludioxonil in mealworms, the larval form of <i>Tenebrio molitor</i>. 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) MgSO<sub>4</sub> + 25 mg PSA + 25 mg C18; (2) MgSO<sub>4</sub> + 50 mg PSA + 50 mg C18; (3) EMR-lipid<sup>TM</sup> tube; and (4) 10 mL <i>n</i>-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.https://www.mdpi.com/1420-3049/25/15/3518mealwormspesticide residueQuEChERSGC–MS/MSLC–MS/MS
collection DOAJ
language English
format Article
sources DOAJ
author Leesun Kim
Sujin Baek
Kyungae Son
Eunsun Kim
Hyun Ho Noh
Danbi Kim
Min-seok Oh
Byeong-chul Moon
Jin-Ho Ro
spellingShingle Leesun Kim
Sujin Baek
Kyungae Son
Eunsun Kim
Hyun Ho Noh
Danbi Kim
Min-seok Oh
Byeong-chul Moon
Jin-Ho Ro
Optimization of a Simplified and Effective Analytical Method of Pesticide Residues in Mealworms (<i>Tenebrio molitor</i> Larvae) Combined with GC–MS/MS and LC–MS/MS
Molecules
mealworms
pesticide residue
QuEChERS
GC–MS/MS
LC–MS/MS
author_facet Leesun Kim
Sujin Baek
Kyungae Son
Eunsun Kim
Hyun Ho Noh
Danbi Kim
Min-seok Oh
Byeong-chul Moon
Jin-Ho Ro
author_sort Leesun Kim
title Optimization of a Simplified and Effective Analytical Method of Pesticide Residues in Mealworms (<i>Tenebrio molitor</i> Larvae) Combined with GC–MS/MS and LC–MS/MS
title_short Optimization of a Simplified and Effective Analytical Method of Pesticide Residues in Mealworms (<i>Tenebrio molitor</i> Larvae) Combined with GC–MS/MS and LC–MS/MS
title_full Optimization of a Simplified and Effective Analytical Method of Pesticide Residues in Mealworms (<i>Tenebrio molitor</i> Larvae) Combined with GC–MS/MS and LC–MS/MS
title_fullStr Optimization of a Simplified and Effective Analytical Method of Pesticide Residues in Mealworms (<i>Tenebrio molitor</i> Larvae) Combined with GC–MS/MS and LC–MS/MS
title_full_unstemmed Optimization of a Simplified and Effective Analytical Method of Pesticide Residues in Mealworms (<i>Tenebrio molitor</i> Larvae) Combined with GC–MS/MS and LC–MS/MS
title_sort optimization of a simplified and effective analytical method of pesticide residues in mealworms (<i>tenebrio molitor</i> larvae) combined with gc–ms/ms and lc–ms/ms
publisher MDPI AG
series Molecules
issn 1420-3049
publishDate 2020-07-01
description An effective analytical method was optimized for residues including chlorpyrifos–methyl, deltamethrin, fenoxanil, thiobencarb and fludioxonil in mealworms, the larval form of <i>Tenebrio molitor</i>. 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) MgSO<sub>4</sub> + 25 mg PSA + 25 mg C18; (2) MgSO<sub>4</sub> + 50 mg PSA + 50 mg C18; (3) EMR-lipid<sup>TM</sup> tube; and (4) 10 mL <i>n</i>-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.
topic mealworms
pesticide residue
QuEChERS
GC–MS/MS
LC–MS/MS
url https://www.mdpi.com/1420-3049/25/15/3518
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