Determination of 73 multi-class pesticides in okra (Abelmoschus esculentus L.) fruits using LC–MS/MS and GC–MS/MS and estimation of analytical uncertainty of measurement

This study developed a method to simultaneously determine 73 multi-class pesticides in okra fruit using LC-MS/MS and GC–MS/MS. The sample was extracted with acetonitrile and subsequent clean-up through dispersive-SPE method. The quantification level of the technique was 0.01 µg g−1 and compliance to...

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Main Authors: M.S. Pallavi, R. Harischandra Naik, K. Pavankumar, Ratnamma, Nandini, A. Shwetha, P. Naveenkumar, M. Paramasivam, R. Udaykumar Nidoni, A. Prabhuraj, M. Bheemanna
Format: Article
Language:English
Published: Elsevier 2023-10-01
Series:Food Chemistry: X
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S2590157523002572
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author M.S. Pallavi
R. Harischandra Naik
K. Pavankumar
Ratnamma
Nandini
A. Shwetha
P. Naveenkumar
M. Paramasivam
R. Udaykumar Nidoni
A. Prabhuraj
M. Bheemanna
author_facet M.S. Pallavi
R. Harischandra Naik
K. Pavankumar
Ratnamma
Nandini
A. Shwetha
P. Naveenkumar
M. Paramasivam
R. Udaykumar Nidoni
A. Prabhuraj
M. Bheemanna
author_sort M.S. Pallavi
collection DOAJ
description This study developed a method to simultaneously determine 73 multi-class pesticides in okra fruit using LC-MS/MS and GC–MS/MS. The sample was extracted with acetonitrile and subsequent clean-up through dispersive-SPE method. The quantification level of the technique was 0.01 µg g−1 and compliance to the MRLs fixed by the regulatory bodies like EU and FSSAI. The recovery at 10, 50, and 100 µg kg−1 spiked levels; intra and inter-day precision at 50 µg kg−1 were found within 70–120% with RSD less than 15% with LC-MS/MS and GC–MS/MS. Measurement uncertainty was in the range of 1.81 to 12.91 µg kg−1 estimated at 50 µg kg−1. The matrix effects were slightly higher for LC than GC-compatible pesticides. Risk assessment for pesticides detected in the field and market samples found no hazardous to the consumers except profenofos. The proposed method is highly sensitive, reproducible for the complex matrix like okra, and meets the regulatory standards.
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spelling doaj.art-1d8023994dc14208a7b4e3e9b8cdd5762023-09-23T05:12:22ZengElsevierFood Chemistry: X2590-15752023-10-0119100814Determination of 73 multi-class pesticides in okra (Abelmoschus esculentus L.) fruits using LC–MS/MS and GC–MS/MS and estimation of analytical uncertainty of measurementM.S. Pallavi0R. Harischandra Naik1K. Pavankumar2 Ratnamma3 Nandini4A. Shwetha5P. Naveenkumar6M. Paramasivam7R. Udaykumar Nidoni8A. Prabhuraj9M. Bheemanna10University of Agricultural Sciences, Raichur 584 104, India; KSN University of Agricultural and Horticultural Sciences, Shivamogga 577 412, IndiaUniversity of Agricultural Sciences, Raichur 584 104, India; University of Horticultural Sciences, Bagalkot, College of Horticulture, Bangalore 560 065, Karnataka, India; Corresponding author at: University of Horticultural Sciences, Bagalkot, India; University of Agricultural Sciences Raichur, India.University of Agricultural Sciences, Raichur 584 104, IndiaUniversity of Agricultural Sciences, Raichur 584 104, IndiaUniversity of Agricultural Sciences, Raichur 584 104, IndiaUniversity of Agricultural Sciences, Raichur 584 104, IndiaUniversity of Agricultural Sciences, Raichur 584 104, IndiaTamil Nadu Agricultural University, Coimbatore 641 003, IndiaUniversity of Agricultural Sciences, Raichur 584 104, IndiaUniversity of Agricultural Sciences, Raichur 584 104, IndiaUniversity of Agricultural Sciences, Raichur 584 104, IndiaThis study developed a method to simultaneously determine 73 multi-class pesticides in okra fruit using LC-MS/MS and GC–MS/MS. The sample was extracted with acetonitrile and subsequent clean-up through dispersive-SPE method. The quantification level of the technique was 0.01 µg g−1 and compliance to the MRLs fixed by the regulatory bodies like EU and FSSAI. The recovery at 10, 50, and 100 µg kg−1 spiked levels; intra and inter-day precision at 50 µg kg−1 were found within 70–120% with RSD less than 15% with LC-MS/MS and GC–MS/MS. Measurement uncertainty was in the range of 1.81 to 12.91 µg kg−1 estimated at 50 µg kg−1. The matrix effects were slightly higher for LC than GC-compatible pesticides. Risk assessment for pesticides detected in the field and market samples found no hazardous to the consumers except profenofos. The proposed method is highly sensitive, reproducible for the complex matrix like okra, and meets the regulatory standards.http://www.sciencedirect.com/science/article/pii/S2590157523002572Okra fruitsPesticidesQuEChERSLC-MS/MSGC–MS/MSRisk assessment
spellingShingle M.S. Pallavi
R. Harischandra Naik
K. Pavankumar
Ratnamma
Nandini
A. Shwetha
P. Naveenkumar
M. Paramasivam
R. Udaykumar Nidoni
A. Prabhuraj
M. Bheemanna
Determination of 73 multi-class pesticides in okra (Abelmoschus esculentus L.) fruits using LC–MS/MS and GC–MS/MS and estimation of analytical uncertainty of measurement
Food Chemistry: X
Okra fruits
Pesticides
QuEChERS
LC-MS/MS
GC–MS/MS
Risk assessment
title Determination of 73 multi-class pesticides in okra (Abelmoschus esculentus L.) fruits using LC–MS/MS and GC–MS/MS and estimation of analytical uncertainty of measurement
title_full Determination of 73 multi-class pesticides in okra (Abelmoschus esculentus L.) fruits using LC–MS/MS and GC–MS/MS and estimation of analytical uncertainty of measurement
title_fullStr Determination of 73 multi-class pesticides in okra (Abelmoschus esculentus L.) fruits using LC–MS/MS and GC–MS/MS and estimation of analytical uncertainty of measurement
title_full_unstemmed Determination of 73 multi-class pesticides in okra (Abelmoschus esculentus L.) fruits using LC–MS/MS and GC–MS/MS and estimation of analytical uncertainty of measurement
title_short Determination of 73 multi-class pesticides in okra (Abelmoschus esculentus L.) fruits using LC–MS/MS and GC–MS/MS and estimation of analytical uncertainty of measurement
title_sort determination of 73 multi class pesticides in okra abelmoschus esculentus l fruits using lc ms ms and gc ms ms and estimation of analytical uncertainty of measurement
topic Okra fruits
Pesticides
QuEChERS
LC-MS/MS
GC–MS/MS
Risk assessment
url http://www.sciencedirect.com/science/article/pii/S2590157523002572
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